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STP 1165
Metallography:
Past, Present, and Future
(75th Anniversary Volume)
George F. Vander Voort, Francis J. Warmuth,
Samuel M. Purdy, and Albert Szirmae, editors
ASTM Pubhcation Code No. (PCN)

04-011650-23
AsTM
1916 Race Street
Philadelphia, PA 19103
Library of Congress Cataloging-in-Publication Data
Metallography--past, present, and future 75th anniversary volume/
George F Vander Voort [et al ], editors
(STP 1165)
"ASTM publication code no (PCN) 04-011650-23 "
Includes bibliograph=cal references and indexes
ISBN 0-8031-1484-2
1 Metallography--Congresses I Vander Voort, George F
II Amencan Soc=ety for Testing and Materials III Senes ASTM
speo=altechnical pubhcation 1165
TN689 2 M445 1993
669' 95--dc20 93-14998
CIP
Copyright 9 1993 AMERICAN SOCIETY FOR TESTING AND MATERIALS, Philadelphia, PA All
nghts reserved This material may not be reproduced or cop=ed,=nwhole or in part, in any pnnted,
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Peer Review Policy
Each paper pubhshed in th=s volume was evaluated by three peer reviewers The authors addressed
all of the reviewers' comments to the satisfaction of both the technical ed0tor(s)and the ASTM
Committee on Pubhcatlons
The quality of the papers m this pubhcatlon reflects not only the obvious efforts of the authors and the
technical editor(s), but also the work of these peer rev=ewers The ASTM Committee on Publications
acknowledges w=th appreciation their ded~cat=onand contribution to t~meand effort on behalf of ASTM
Pnnted In Baltimore,MD
June 1993
Foreword
The papers m this pubhcatlon, Metallography Past, Present, and Future, were presented at
the symposmm on Metallography" 75 Years Later held 8-10 May 1991 m Atlantic C~ty, New
Jersey The symposmm was sponsored by ASTM Committee E4 on Metallography. George
F Vander Voort, Carpenter Technology Corporation, Franc~s J. Warmuth, Cameron Forge
Company, Samuel M Purdy, National Steel Company, and Albert Szlrmae, U S Steel Cor-
poration, served as symposmm cochmrmen and are coe&tors of th~s pubhcatlon
Contents
Overview
The History of ASTM Committee E4 on Metallography--

GEORGE F VANDER VOORT
LIGHT MICROSCOPY
Some Incidental History of Metallography and ASTM Committee E 4 - -

THEODORE G. ROCHOW 83
Research Under the Microscope--WILLIAM G. FRICKE,JR 88
METALLOGRAPHIC PREPARATION TECHNIQUES
Automotive Materials and Their Characterization: 1916 to 1 9 9 1 -

GERALD S COLE, LESLIE BARTOSIEWICZ, AND FLOYD E ALBERTS 109
New Diamond Grinding Disks for Specimen Surface l>reparation--

ROBERT L. BENNER 139
Advancements in Ultrathin Section Techniques for the Characterization of Brittle

m a t e r i a l s - - N A T A L I O T SAENZ 155
The Early Metallographic Studies of Chih-Hung Chon on the Formation and

Morphology of Widmanstatten Structure and Martensite--
MICHAEL R. NOTIS, ARNOLD R. MARDER, AND YE T. CHOU 167
X - R A Y AND ELECTRON METALLOGRAPHY
Those Magnificent Men on Their Scanning Machines--KURT F. J HEINRICH 177
Seventy-Five Years of Activity in X-Ray Methods by ASTM Committee E4.06--

SAMUEL M. PURDY AND LEO ZWELL 184
Microstrnetural Studies of an Oxide-Dispersion-Stabilized Niobium Composite

Using Transmission Electron Microscopy--ATUL S RAMANI
AND PAUL R HOWELL 189
The Application of Transmission Electron Microscopy to the Study of a Low-
Carbon Steel: H S L A - 1 0 0 - - R A J A N VARUGHESE AND PAUL R HOWELL 199
Transmission Electron Microscopy of the lnterdiffusion Regions of Iron-Zinc

C o u p I e s - - L U C I L L E A. GIANNUZZI, PAUL R HOWELL,
HOWARD W PICKERING, AND WILLIAM R. BITLER 212
Some Reflections on the Early Development of Electron Microscopy and

Microanalysis--JAMES HILLIER 224
QUANTITATIVE METALLOGRAPHY
Quantitative Metallography in Test Method Standards and Product

SpecificationS--DANIEL B FOWLER 235
Artificial Intelligence for Twin Identification--JOHN J. FRIEL

AND EDDIE B PRESTRIDGE 243
The Use of Quantitative Image Analysis for the Characterization of Corrosion-

Resistant Coatings--SCOTT T. BLUNI, KATHERINE M. GOGGINS,
BRIAN J. SMITH, AND ARNOLD R MARDER 254
Examination of Some Grain Size Measurement Problems--

G E O R G E F. VANDER VOORT 266
Measurement and Interpretation of Fracture Surface Fractal Dimension--

WILLIAM DRURY AND ARUN M GOKHALE 295
APPLICATIONS I
In Search of Mierostructure--JAMES A NELSON 313
The Microstructure of Laser-Welded Aluminum BronzeS--DAVID E BELL,

TERRI A. MARSICO, KATHLEEN PETROLONIS, PAUL E DENNEY,
AND PAUL R HOWELL 327
Metallography of Mechanically Alloyed Aluminum--WILLIAM J. D SHAW 344
Microstructural Investigations of Rapidly Solidified Copper-Niobium (Cu-Nb)

Alloy Powders Produced by Inert Gas Atomization--gEVXN L ZEIK,
IVER E ANDERSON, DONALD A KOOS, AND PAUL R. HOWELL 363
Metallography Applied to the Structure of Electrorheoiogical (ER) Fluids--

M A R K D. FISHER, ARNOLD F. SPRECHER, AND HANS CONRAD 372
APPLICATIONS II
Interpreting Solidification Phenomena and Microstructural Evolution in Metals

Through the Use of Transparent Model Alloy Systems--
R I C H A R D N. GRUGEL AND ROHIT TRIVEDI 393
Some Failure Analysis Case Histories in Galvanized Steel Products--

E D W A R D LARKIN AND MEHROOZ ZAMANZADEH 414
Characterization of Reaction Between Cast Titanium and Silica-Containing

Investment M o l d - - H E R B E R T J. MUELLER 429
Author Index 447
Subject Index 449
VII
STP1165-EB/Jun. 1993
Overview
The ongm o f metallography is traced generally to the ploneenng efforts of Henry Chfton
Sorby, gifted British amateur soentlst, who m 1863 made the first observation of the micro-
structure of a pohshed and etched metal speomen. However, the mdustnal and soentlfic
world greeted this development with indifference and nearly 25 years passed before others
began to budd upon Sorby's work.
The growth of the steel industry after the Cwd War, spurred by developments such as the
Bessemer converter and the open hearth furnace, transformed technology and sooety. But this
growth could not be accomphshed without development of the soence of metals. Techniques
such as metallography made th~s possible
ASTM Committee E4 on Metallography was founded m 1916, 53 years after Sorby's lmtlal
observatmn of m~crostructure. Prior to that, ASTM had one committee, E 1, that covered all
methods of testing of metals and alloys and only one standard, E 1, containing two pages
devoted to metallography. It was recogmzed that more work needed to be done and a new
committee, E4, was formed for this purpose.
This symposmm, held on 8-10 May 1991, commemorates the 75th anmversary of com-
mittee E4 F~ttmgly, ~t was held m Atlantic C~ty, where ASTM met annually for many years,
up to about 1970
Committee E4 has been a leader m developing metallographlc test methods. Th,s has been
accomphshed by the combined efforts of hundreds of volunteer members over the past 75
years The enclosed historical rewew of E4 hlghhghts the techmcal achievements and the hves
of many of the responsible E4 members Putting together this history was difficult and it prob-
ably is imperfect. However, it does show the importance of drawing talented metallographers
into E4 actwmes
Many of the papers m th~s book discuss the historical developments of specific areas m met-
allography Knowledge of the past ~s important, not s~mply to maintain our perspectwe, but
as a foundation for growth. Too often, we ~gnore the past and find that we are merely rede-
velopmg what others have done before and, perhaps not as well
George F. Vander Voort Samuel M. Purdy

Carpenter Technology Corporatmn, Reading, PA Nattonal Steel Company, Trenton, MI 48183,
19612, symposmm cochmrman and coed,tor symposmm cochalrman and coedltor
Francis J. Warmuth Albert Szirmae

Cameron Forge Company, Houston, TX 77251, U S Steel Corporation, Monroevllle, PA 15146,
symposium cochmrman and coed~tor symposmm cochalrman and coedltor
Copyright
Copyright*by 1993
ASTM byInt'l
ASTM (all rights reserved); Thu Dec
International 29 00:42:12 EST 2011
www.astm.org
George F. Vander Voorf
The History of ASTM Committee E4 on

Metallography
R E F E R E N C E : Vander Voort, G F, "The History of ASTM Committee E4 on Metallography,"
Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F
Vander Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing
and Materials, Phdadelphla, 1993 pp 3-79
ABSTRACT. Organized on 10 October 1916 to estabhshed standard magnifications for micro-

graphs, Committee E4 has branched out into many different areas, far beyond its mlhal scope,
m the process producing forty-two standards, twenty-five STPs (this is the twenty-fifth), five
ASTM presidents, two other ASTM Committees, and the Joint Committee on Powder Dlffrac-
tmn Standards The committee has met 138 times, not counting separate task group meetings
ASTM E4 standards are used by many other countries, ezther m full, or m part As with all ASTM
committees, E4's members are volunteers Whatever success E4 has had is due to these volun-
teers and the support of their orgamzatmns
KEY WORDS: metallography, history, standards, testing
ASTM E4 on Metallography, organized on 10 October 1916, grew out of Committee E 1 on

Methods of Testing (as is true of many other E committees) At that time, standard E 1-16
(Standard Methods of Testing, originally adopted in 1910) consisted of five parts, the last enti-
tled "Methods for Metallographlc Tests of Metals" requlnng somewhat less than three pages.
The organizational efforts were chaired by Edgar Marburg, ASTM's Secretary-Treasurer, who
died m 1918
At that time, it was perceived that there was a need to estabhsh standard magmficatmns for
mlcrographs and that this work would be best performed by a new standing committee This
new group was called Committee E4 on Magnification Scales for Mlcrographs Actually, there
had been an earher committee called E4 on Methods of Samphng and Analysis of Coal, which
was disbanded m 1915 and there also was a &sbanded E3 at the time Hence, we could have
been known as E3 on Metallographyjust as easily as E4. At any rate, the original E4 name did
not last long because the members reahzed that the estabhshment of standard magnifications
was a simple task and many more complex problems needed to be solved. Subsequently, m
1920, the members decided to change their name to Committee E4 on Metallography, and
this name has been used since 1921 E4's original fifteen members, not counting Marburg,
hsted two ASTM presidents, Dr Henry Marion Howe, the dean of American metallurgmts at
that time, and George Kamball Burgess, famed director of the National Bureau of Standards
Howe was a founder of ASTM, his name is the first hsted on the charter, and he was the first
(and third) ASTM president serving a total of four years Burgess was ASTM's fourteenth
president
E4, as with all volunteer groups, has had its share of successes and failures History walljudge
E4 based mainly on its tangible accomphshments These can be viewed in several ways. Issu-
Supervisor, Materials Characterization, Carpenter Technology Corporation, Reading, PA 19612
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
4 METALLOGRAPHYPAST, PRESENT, AND FUTURE
ance of standards is an obvious yardstick. E4 has published forty-two standards Of these,

seven were discontinued (six of these were replaced by newer documents), five were transferred
to other standing committees, and thirty are now active Another good yardstick is symposia,
particularly those subsequently published E4 has sponsored or cosponsored numerous sym-
posia since 1936 and these have generated twenty-five special technical pubhcatlons (see list).
Two other E committees, E7 on Nondestructive Testing and E37 on Thermal Measurements,
were spun offE4, and they have been highly successful E4 members started the highly sigmf-
icant work of the Joint Committee on Powder Diffraction Standards, JCPDS, in Swarthmore,
Pennsylvania, and four E4 members have been officers of this organization Four E4 members
have served as vice president and five as president of ASTM and eight others have served as
directors or as members of the executive committee Thirteen E4 members were made hon-
orary ASTM members and thirty-four have received the Award o f Merit (five were made Fel-
lows prior to creation of the Award of Merit) Naturally, some of these men were also active
on other committees. The accompanying tables list E4 award winners E4 members have been
active in other societies, for example, nine E4 members have been presidents of the American
Society for Metals
It is more difficult, however, to gage how well E4 has served the metallographlc needs of
industry. Has E4 met the needs of the metallographic community in a timely fashion9 Have
other groups done a better job9 Has E4 led the way in standards development compared to
other technical societies, here or abroad, or industrial companies9 These are tough questions
to answer, but a little soul searching is necessary at times In general, we would conclude that
E4 has done a very good j o b overall as ASTM metallographic standards are the most widely
used in the United States, and many other countries have followed our lead No doubt we
could have been faster in many of our tasks. O f course, this is a totally unbiased, highly precise
evaluation, based upon a massive survey (of one) vBut, as Paul Harvey says, let's hear"the rest
o f the storyV"
E4 has met at least 138 times since its formation. This May's meeting was the thirty-first in
Atlantic City, New Jersey, the last being in June o f 1971 Philadelphia, New York, Pittsburgh,
and Chicago were the next most frequent meeting sites with 16, l 0, 9, and 8 visits, respectively
E4 membership (Fig 1) grew steadily over the years reaching Its peak in 1979 with 161 mem-
ben's. Since then, membership has been declining steadily These numbers are somewhat
deceptive as some of the members were consultants (nondues paying) and for the past ten years
we have been purging the roster of members who do not return ballots. Membership is
rebounding, however, due to recruiting efforts and new E4 activities However, compared to
the peak years, E4 has had a reduction in active meeting participants, although we have again
rebounded in this area
Despite a general drop In membership since 1979, Fig 2 shows that E4's standards devel-
opment effort has not decreased, but increased In 1979, E4 had 15 active standards In the
last eleven years, this number has doubled to 30 (see E4 Standards at a Glance) Prior to 1979,
E4 had developed twenty-four standards but nine were either transferred to other committees,
discontinued, merged with another, or replaced Since 1979, seventeen new standards have
been developed, one was transferred and one was replaced by a new standard Either way, the
past eleven years have been highly productive despite the loss of E4 membership
E4 Officers
Only thirteen people have chaired E4 (see officers list), largely because LeRoy L Wyman,
Sr. held the chairmanship for 28 years (1938-1966), an ASTM record E4 was not the only
committee W y m a n chaired W y m a n certainly qualified as a full-time, unpaid ASTM
VANDER VOORTON HISTORYOF COMMITTEEE4 5
200
150
~100
50
0 I I I I I I I I
1910 1920 1930 1940 1950 1960 1970 1980 1990 2000
Year
FIG. I --Graph of Committee E4 membership.
35
30
ii i i i i i.i!i.i.i.ii.i..i.i.i..i.i..i..i.i.i..i.i
25
.a 20
E
Z
15
10
.............. j ......... ~ ...............................................................................................................................................................
I I I I I I I I
0
1910 1920 1930 1940 1950 1960 1970 1980 1990 2000
Year
FIG. 2--Committee E4 active standards.
6 METALLOGRAPHYPAST, PRESENT,AND FUTURE
employee v More recently, E4 chairmen have been restricted to no more than two consecutive
two-year terms.
There have been thirteen E4 secretaries, the first elected in 1921 Three people held this
position for long p e r i o d s - - M a r y R. Norton (20 years), John J Bowman (ten years), and
George F. Comstock (nine years) In 1936, E4 appointed its first vice chairman, Dr Marcus
A Grossman, who held the position for eight years Grossman was internationally recognized
for his work on hardenabdlty He was followed by R Earl Penrod who held the position for
twenty years Wyman, Penrod, and Norton ran E4 for about a third of its existenceV E4 also
has the unique distinction o f having father and son chairmen, William D Forgeng, Sr and
J r , serving with only a two year interval between them
E4 appointed its first second vice-chairman in 1972 and eight people have held this position
for either two- or four-year terms Our first membership chairman was appointed in 1964 and
eight people have served in this capacity The accompanying table lists all of the past E4 officers
and their terms of office
E4 Subcommittees
E4 created fifteen techmcal subcommittees with the first started m 1920. Roman numerals
were used to number subs up until 1970, since then Arabic numbers have been used. 2 Only
eight subcommittees are now active, mainly due to mergers
Sub 1 on Sample Selection and Preparation and Photography was formed in 1920 as Sub I
on Preparation of Metallographic Specimens Its name was changed twice, in 1921 and 1988,
the latter due to the merging of Sub 4 on Photography into Sub 1 When many people think
of metallography, they think of Sub l's domain first Indeed, Sub l's activities have been
always a focal point of E4 concentration Sub 1 has prepared the greatest number of standards
and hasjunsdictlon over eight active standards, the most of any E4 subcommittee Sub 1 has
had ten chairmen with one person, Sam Purdy, serving during two different time periods for
a total o f 23 years (and still going strong!) The list of Sub 1 chairmen (see list of all subchalr-
men) is very impressive.
For many years, standard E 2 (Preparation of Mlcrographs of Metals and Alloys) guided
metallographers but it was discontinued In 1983 at the age of 66 The original version, intro-
duced in 1917 (they were offto a good start), was written largely by William H Bassett (Ana-
conda Wire and Cable). E 2 contained grain size measurement information, which really was
inconsistent with the specification title, until 1949, when this information was removed and
incorporated into new standard E 79 E 2 also had the first grain size chart for copper, added
in the 1930 revision This chart was developed by Edgar H Dlx, J r , Francis F Lucas, Henry
S. Rawdon, and Charles H Davis The actual mlcrographs were prepared by Davis and his
staffofthe American Brass Co in Waterbury, Connecticut
Standard E 3, Preparation o f Metallographic Specimens, has been one of the most Impor-
tant E4 documents In the early days of this century, there were few, if any, compilations of
preparation procedures and etchants. E 3, prepared largely by Henry Marion Howe, pulled
much of the existing information together, and this has been continually updated William
Campbell and George F. Comstock also contributed to E 3 (and also E 5, which was merged
into E 3 in 1935) as did E. C. Groesbeck of the then U.S. Bureau of Standards and a developer
of selective etchants [ 1]
In 1928, Sub l introduced metailographers to the use of Bakehte (phenolic plastic) for
mounting specimens. Later, in 1938, LeRoy L. W y m a n presented a detailed report on the use
2 In this text, 1 wdl used Roman numerals when referring to a sub and its actwltles before 1970 and
Arabic numbers for subsequent events
VANDER VOORT ON HISTORYOF COMMITTEEE4 7
of plastics for mounting [2] In 1932, W y m a n had replaced Wllham E. Ruder as General Elec-
tric Research Laboratories representatwe, thus beganmng a long, productive assocmt~on
Throughout the 1920s and 1930s, Sub 1 was constantly searching for sources of good cloths
for pohshmg W y m a n reported [3] that due to fashion changes m the 1920s, "kitten-ear"
broadcloth, a very popular pohshmg cloth, had become unavailable W y m a n canvassed the
garment district of New York City for possible subsUtutes E4 members tried these but without
success Eventually, they persuaded the Horne Co of Pittsburgh to produce k~tten ear for met-
allographers ASTM was conwnced to order huge rolls ofth~s cloth which was sold to metal-
Iographers at cost. After several years m the pohshmg cloth business, a newly formed metal-
lographlc supply house took over th~s function. Kitten-ear cloth is stdl commonly used for
final pohshmg, particularly for soft metals where scratch removal is particularly difficult
W~th each rews~on, standard E 3 grew and grew, from the mmal thirteen page 1921 version
to a s~xty-s~x page document m 1958. At this time, it was felt that E 3 was becoming cumber-
some Information on macroetch and m~croetch composmons and uses was removed from E
3 and used as the basis for new standards E 340 and E 407, respectwely In 1980, E 3 was
reduced to coverage of mechamcal pohshmg alone. Subsequently, E 1180 was written expand-
mg upon the brief description of sulfur printing found m E 3 up to 1980. The electropohshmg
mformahon m E 3 up to 1980 has not yet emerged as a new standard, but thas work is again
mowng forward
Sub l developed standard E 381, building upon ASTM A 317 (Macroetch Testing and
Inspection of Forgmgs), to describe classaficatlon and interpretation of macroetched sectaons
cut from wrought ingot-cast material (blooms, billets, and bars, for example) This is a general
purpose standard that complements other special purpose standards, for example, A561 and
A 604 Continuous casting has become increasingly popular due primarily to cost sawngs
Steels made by th~s process may be evaluated for macrostructure m the as-cast condmon,
unhke ingot cast material, or after hot reduction. The existing E 381 macroetch classification
charts are not really useful for continuously cast steels, particularly fftested m the as-cast con-
dmon An extenswe effort has been underway for several years now to expand E 38 l's
coverage
Another recent effort of Sub 1 has been the development o f E 1351 which describes how to
make and evaluate rephcas made m the field to estimate the remaining hfe of steam p~pmg m
power plants This standard began hfe as an emergency standard, ES 12, E4's only emergency
standard Thas approach was taken as a result of a serious accadent due to fadure of a mare
steam lane Many power plants are now at or beyond thear original design hfe Assessment of
the remnant hfe of components subjected to many years of h~gh temperatures and pressures
has rehed upon examination of mlcrostructural evolution and the formation and growth of
creep cawt~es under these operating condmons. Almost overnight, numerous people were
revolved m such evaluations, and there was an obvious need to standar&ze the procedures.
Sub 1 was approached by members o f the power generation industry to tackle thas problem
and they responded swiftly wath a h~ghly useful document
Sub 1 as now workmg on preparataon methods for thermally sprayed coatmgs These coat-
rags are used on a variety of products, for example, mrcraft engine components The m~cro-
structures tend to be rather heterogeneous and porosity is generally present Specimen prep-
aratlon can bade the porosity, or exaggerate ~t, depending upon the parameters chosen
Standard procedures are needed to insure that the true m~crostructure ~s revealed, otherwise
any evaluataon or measurement will be incorrect.
Sub 2 on Metallographlc Terminology and Nomenclature of Phase Diagrams was formed
m 1920 Originally, defimtlons were to be incorporated into standard E 2 and s~xteen terms
were first defined and balloted. However, only eleven of these made ~t through the ballot pro-
cess and a separate standard, E 7, was issued m 1924. It was soon noted that E4 on Metallog-
raphy had forgotten to define metallography so this term was added in 1926, but the definmon
was revised m 1927.
Henry C Boynton was Sub II's first chairman and Professor Arthur Phdhps (see biography)
of Yale Umverslty was the second Inmally called Sub II on Nomenclature and Definmons, it
was mactwe through most of the 1930s. Reactivated under Dr. Robert S Wdhams of Mas-
sachusetts Institute of Technology m 1939, it stayed active only two years as he recommended
against revis~ons to E 7
In 1946, efforts were made to revise Sub II, but nothing happened until 1948 when Dr Paul
A Beck ofthe Umversity of Notre Dame (later the Unwerslty ofllhnois) was appointed Chair-
m a n The sub was renamed Sub II on Definitions and Beck started a massive effort to turn E
7 into a comprehensive terminology standard Beck created a long list of potential terms and
turned this work over to Dr. Robert S Busk o f Dow Chemical Co. Nearly a thousand terms
were considered. In 1955, E 7 j u m p e d from twelve definitions to a forty-five page document
with 750 defimtlons.
After this massive effort, Sub II became inactive m the late 1950s until 1966 when Mary R.
Norton of Watertown Arsenal became chairman. She worked with then Committee E8 (on
Nomenclature and Definmons) to add metallography terms to the new ASTM glossary and
also with members of new Committee E25 (on Microscopy) to compare definmons for the
same terms in E 7 and in their terminology standard, E 175. This revealed twenty-three defi-
rations with &fferences to be reconciled, which was done Since 1955, there have been at least
thirteen additional revisions of E 7 revolving refinements to definmons, deletions of obsolete
terms, and addmons of new terms, for example, on electron metallography and ~mage analysis.
More recently, Sub 2 has been working on adding symbol and acronym secuons Beth Knuep-
pel is the current chairman of Sub 2.
Sub 3, formed m 1920 as Sub l l l o n ThermalAnalysis, has had an interesting history In
1920, E4 recommended to A S T M that a standard committee be formed on pyrometry as this
was too far outside the scope of E4 While temperature measurement per se was considered
too far afield, the interpretation of cooling curves and thermal arrests were not In the early
days of metaliography, one of the chief act~vmes was the construction of eqmhbnum phase
dtagrams and thermal analyses (both heating and cooling) was a major tool for such work
The first chmrman o f Sub III was George Kimball Burgess, director o f the U S Bureau o f
Standards who was replaced, after a few years o f mactwlty, by W d h a m E Ruder of General
Electric Co. Ruder and his subcommittee produced standard E 14 m 1925. This standard was
revised five times and then transferred to new Committee E37 (on Thermal Measurements)
m 1978 Howard Scott took over Sub III m 1928 but actwlty stopped by 1933.
In 1949, this committee was reactivated as Sub I I I on Nomenclature under Dr. Paul A
Beck Its goal was to establish a system of nomenclature for alloy phases in binary and more
complex systems The development and construction of eqmhbrlum phase dmgrams was not
standar&zed and the naming of phases was performed erraUcaUy. Beck pulled together a sub-
committee consisting of the major American and British experts on phase diagrams (not all
were ASTM members, h o w e v e r ) - - K W. Andrews, Max Hansen, W d h a m Hume-Rothery, F.
Laves, Taylor Lyman, John S. Marsh, G. V Raynor, Frederick N. Rhlnes, Cyril Stanley
Smith, and Arthur J. C. Wdson, besides knowledgeable E4 members such as Robert S Busk
and W d h a m L. Flnk. The latter became the subchmrman in 1960 and held this poslUon until
1978
This work, started by Beck and continued by Flnk, resulted m a new system [4,5] of alloy
phase nomenclature described in standard E 157, introduced in 1961 The SUbcommittee then
began work on rules for drawing phase diagrams suitable for publication This resulted m stan-
dard E 391 in 1969 Since then, aside from revisions to E 157 and E 391, which have been
minor, there has been no activity in this area and Sub 3 was merged into Sub 2 in 1988
VANDER VOORT ON HISTORY OF COMMITTEE E4 9
S u b IVon Pkotograpky was also estabhshed m 1920 V H Blhlman was the first chmrman,
followed by Henry S Rawdon and Leon V. Foster, each of whom served for long periods (12
and 17 years, respectively) Foster developed the well-known, very popular calcite prism polar-
lzer used on Bausch and Lomb metallographs Sub IV developed photomlcroscopy reforma-
tion that was Incorporated into standard E 2. The mtroducUon of E 883 m 1983, which was a
massive updating of the photographic reformation formerly m E 2, led by Fran Warmuth,
resulted in the withdrawal o f E 2
One of Sub IV's most slgmficant achievements was the sponsorship of the annual ASTM
photographic contest which started m 1936 but ended with the 1980 contest The decision to
stop the society-wide annual meeting made it very difficult to run the contest. Sub IV also held
a symposmm m 1948 on the use of color m photomlcroscopy (STP 86) At that time, such use
of color was m its infancy, and the symposium demonstrated the value of color After the issu-
ance of E 883, and the demise of the annual photographic contest, Sub 4 activity waned In
1988, Sub 4 duties were taken over by Sub 1
S u b 5 on Microindentation Hardness Testingwas created m 1923 as Sub V on Micro-Hard-
ness to evaluate the scratch hardness instrument developed by C H Blerbaum, an E4 mem-
ber Henry S Rawdon chaired the committee The method was found to be useful only m a
comparative manner to show &fferences m hardness between &fferent constituents [6] As no
other m~crolndentat~on eqmpment existed at that time, the sub was disbanded m 1927
Instrumentation, using both Knoop and Vlckers type indenters, was developed starting m
the late 1930s prompting E4 to reactivate the committee, now Sub V on Mlcrohardness, m
1948 under Alexander Gobus A round robin (the first of many) was lmtlated m 1950 to eval-
uate instruments At the request of Sub V, Bausch and Lomb developed a new stage m~crom-
eter m 1950 w~th 0 02 u m accuracy
Walter A. Shebest of the Frankford Arsenal took over Sub V m 1955 and the round robin
continued After a period ofmactwlty, Larry Toman, Jr. took over Sub V in 1965. One of his
first tasks was to define m~crohardness. Today, E4 tries to &scourage use of this term although
its use ~s thoroughly ingrained. Mlcrohardness, at face value, suggests a very small hardness,
which is not the retention. These tests produce a very small indentation due to application of
a rather low load, to determine the same hardness number (hopefully) as obtained using a bulk
test w~th a much h~gher load and much larger indent Consequently, the preferred term ~s
m~cromdentat~on hardness testing.
T o m a n and Sub V issued standard E 384 m 1969 to cover Knoop and Vlckers micromden-
tat~on hardness testing In 1975, the symbols HV and H K were adopted m preference to the
original VHN (or DPN) and KHN. Another round robin was begun m the late 1970s, but it
was dropped after only four laboratories completed the tests It was apparent that the approach
used was too complex The results appeared to show that most of the vanabd~ty of test results
occurred m the measurement of the indents, rather than m making the rodents
Yet another round robin was begun m the early 1980s Seven test blocks, three ferrous and
four nonferrous, were indented by one person using five rodents at each of six loads, with both
Knoop and Vlckers indenters The ferrous and nonferrous test specimens were separated and
sent to d~fferent compames Twelve people measured the rodents on the nonferrous specimens
and fourteen people (twenty-four &fferent people m all) measured rodents on the ferrous spec-
imens Tony DeBeihs tabulated all of the test results, but analys~s work was slow m coming
This writer agreed to evaluate the ferrous data After this was done, and the nonferrous data
were stdl untouched, I again volunteered. The results [ 7,8] of this round robin 0ts origins can
be traced back at least to 1972) were used to prepare a detailed precision and bins section for
E 384 Frank Toye is the current chairman of Sub 5
S u b 111 on X-Ray Crystal Analysis was started m 1924 The eminent metallurg)st Zay Jef-
fries was its first chmrman. Jeffnes [9] became interested m the new field of X-ray &ffractlon
10 METALLOGRAPHYPAST,PRESENT,AND FUTURE
after World War I when acting as a consultant to the Cleveland Wire Co. of General Electric
Co He hired a young metallurgist, Edgar Colhns Barn [ 10] (who later gained fame and fortune
with the United States Steel Corp ), to evaluate these new techniques
The mmal work of Sub VI consisted of introduction of standard E 15 (Radiographic Testing
of Metal Casting) written by Horace H Lester of the Watertown Arsenal in 1926, pubhcatlon
of a glossary of X-ray metallography terms [11] prepared by Louis W McKeehan of Bell Tele-
phone Laboratory (later at Yale University), and issuance of a superb review paper [12] on the
current status of X-ray metallography (prepared by Jeffries, Lester, McKeehan, and Bain).
In 1931, the name was changed to Sub VI on X-Ray Methods and in 1933 Dr Robert F.
Mehi of the Carnegie Institute of Technology (now Carnegie Mellon University) became chair-
man Mehl played a dominant role in the founding of the science of physical metallurgy His
mare contribution as an E4 member was the organization of E4's first symposium, held on 2
July 1936, on Ra&ography and X-Ray Diffraction Methods which became E4's first STP (STP
28) At that time, X-ray diffraction was unlocking the secrets of metal crystals It was the first
really powerful tool for studying the internal structure ofcrystalhne materials
In 1937, E4 recommended that a separate standing committee be formed to cover the
inspection aspects of X-ray methods, that ~s, ra&ography. Subsequently, E7 on Radiographic
Testing (now E7 on Nondestructive Testing) was founded [13] in 1938 under the chairman-
ship of Horace Hardy Lester Standard E 15 was transferred to E7 in 1939
Wllham L. Fink of Alcoa took over Sub VI in 1938 and continued as subchalrman until
1960 Under Flnk, standards E 43, E 81, and E 82 were developed. In 1940, Sub VI began
perhaps their greatest task, the estabhshment of a center for information on diffraction meth-
ods for chemical analysis In 194 l, they began work with an X-ray diffraction group of the
National Research Council providing the technical expertise and personnel to start a file cat-
alog of materials already Identified by X-ray diffraction Within a year, 250 sets of X-ray file
cards with 3936 entries had been prepared
This effort spawned the Joint Committee on Powder Diffraction Standards (JCPDS), in
Swarthmore, Pennsylvania, now jointly cosponsored by a number of organizations worldwide
[14] Their function has been to collect, edit, publish, and &stnbute powder diffraction data.
Solids were first studied by X-ray diffraction m 1912 and A W Hull (General Electric Co )
reported the need for a database of diffraction patterns in 1919 Hull demonstrated the unique
nature of each crystalhne substances diffraction pattern, which did not change, even when sev-
eral substances were mixed together Development of a diffraction pattern file was hampered
by the fact that they were recorded on a photographic negative A classification scheme for the
films was developed in 1936 and pubhshed [15] in 1939 by Joseph D. Hanawalt, Harold W
Rinn, and L K Frevel of Dow Chemical Co This paper began the cataloging effort as dif-
fraction patterns for a thousand substances were tabulated
Sub V I and the National Research Council (NRC) formed a joint committee, joined shortly
by the Institute of Physics of Britain who supplied a number of diffraction patterns NRC was
replaced by the American Society of X-Ray and Electron Diffraction (now the American Crys-
tallographic Society) and other groups have since joined JCPDS was housed initially at the
Pennsylvania State Umverslty m the office of E4 member and first JCPDS chairman, Dr
Wheeler P Davey It has been located m Swarthmore since 1970
The original method for searching the database has changed somewhat as the files have
grown Hanawalt revised his original method to one based on the three strongest peaks This
was later modified by William L Fink to a system of ordenng and reordering of the eight
strongest peaks. As the files continued to grow, hand searching became te&ous and other
methods [16-18] have been tried, for example, visual comparative search systems Despite the
magnitude of the file now, the information can be obtained in pnnted form and on microfiche
X-ray diffractomers can be equipped with the entire powder &ffraction file on a CD-ROM for
rapid computer searching. Besides JCPDS's massive effort to collect diffraction data published
worldwide, it also evaluates the quality of the d a t a - - a challenging task) E4 members Wheeler
P Davey, William L Fmk, LeRoy L Wyman, and Andrew W Danko have served as chair-
men and/or general manager of the JCPDS
Not all of Sub VI's efforts have been this successful In 1942, standard E 43 covering the
Hanawalt method for identifying substances by X-ray diffraction was issued It was intended
to be a companion to the newjoint committee powder diffraction database E 43 was revised
twice, In 1946 and 1949. Thereafter it was under a constant state of revision, even up to seven
years after it was withdrawn (in 1961) The subject was considered to be too complex for a
standard, and a book was started but never completed
More recent years have seen the development of an X-ray diffraction standard for measunng
the retained austenlte content of steels, written mainly by Robert W Hinton of Bethlehem
Steel Corp, and issued in 1984 Since then, activity has decreased and Sub 6 became Inactive
m 1987, then merged into Sub 11
S u b V I I on R e c o m m e n d e d Practice for Dilatometric Analysis was formed in 1938 with
LeRoy Wyman, Chairman of E4, as subehalrman as well Laurence H Carr (Edward Valves,
Inc ) took over from Wyman m 1940 and ran Sub VII for the next eleven years during which
E 80 (Dllatometrlc Analysis of Metalhc Materials) was developed and issued in 1949 E 80 was
reapproved but not revised through 1978 when jurisdiction was tranferred to new committee
E37
Donald I Finch of Leeds & Northrup Co took over Sub VII in 1951 and ran it for the next
nineteen years During his tenure, E 189 (Determining Temperature-Electrical Resistance
Characteristics of Metalhc Materials) was developed and issued in 1961 As with E 80, it was
transferred to E37 in 1978
S u b V I I I on Grain Size was a long time in formation as grmn size measurement procedures
were part of E4's first standard in 1917. Although E4 always has been active in the area of grain
size measurement, it was 1931 when a separate committee was estabhshed. This work was
assigned to a Special Committee on Grain Characteristics, rather than a subeommlttee, and
Clarence J Tobin of General Motors Research Laboratory was its chairman Their first effort
was to develop a procedure for assessing the grain growth characteristics of a given heat of steel
The method chosen was the McQuaid-Ehn carbunzlng test originally developed to assess the
smtablhty of a low-carbon steel for carburlzlng Harry McQuaid of Repubhc Steel Corporation
was a consulting member A chart was developed depicting the hypereutectold and hypoeu-
tectold regions of the carbunzed case of specimens with different grain sizes, and the method
and chart were issued as E 19 in 1933
In 1937, Dr Marcus A. Grossman took over the Special Subcommittee which became S u b
VllIon Grain Size m 1938 Although E 19 was an important development, and the orlgmal
chart was claimed to be a result often years effort, the chart was widely criticized as inaccurate
and was under constant revision up to 1961 when it was withdrawn Grossman formed three
separate groups under Sub VIII Group A was to revise E 19 and he headed it Group B was
to develop a ferrlte grain size rating method and was headed by R Earl Penrod Group C was
to develop methods for nonferrous alloys other than copper and was headed by Carl H.
Samans of Standard Oil Company of Indmna H P George (Dept. of the Army, Frankford
Arsenal) took over Group C in 1951 and Penrod replaced Grossman after he died in 1952
Their work resulted m three new standards, E 79 issued in 1949, E 89 issued in 1950, and E
91 issued m 1951. E 79, however, was for copper-based alloys and was largely the grain size
reformation stripped out ofE 2 This work revealed and confirmed comments from members
that gram size analysis was basically a problem of geometry and a single standard could be
developed [19,20] for all alloys. For comparison ratings, it would be necessary to have charts
developed that were realistic depictions of true structures. E 112 grew from these ideas and
replaced E 19, E 79, E 89, and E 91, the latter three having rather short lives The only grain
size chart that survived was the copper chart orE 79, but it too was modified Today, E 112 is
one of the most widely cited ASTM test methods. Nothing, of course, is sacred E I 12 has been
revised eleven times in its thirty-six year history, with a twelfth underway. The most significant
revision to E 112 occurred in 1974 when the three-circle intercept procedure, developed by
Dr Halle Abrams [21] of Bethlehem Steel Corp, was added along with a statistical evaluation
procedure to assess the quality of the measurement
While E 112 contains extensive reformation about grain size measurement procedures, the
most commonly used method is the chart comparison procedure Numerous approaches have
been suggested For example, the appropriate chart can be placed on the wall and the operator
examines the structure through the microscope eyepieces and then looks up at the chart. Ret-
icles can be also prepared depicting portions of the grain size pictures, and these can be super-
imposed over the image viewed through the eyepieces Clear plastic templates of the gram size
photographs can be placed over a projection screen Charles H Davis described [22] a projec-
tion box device produced for the Bausch and Lomb Euscope for grain size rating Frederick
C Hull of the Westinghouse Research Laboratories improved the comparison rating approach
revealing factors that affect its precision and developing correction factors for using alternate
magnifications [23]
E 112 is used for rating the grain size of equlaxed grain structures It has some guidance,
currently being improved, for measunng deformed grain structures However, other situations
exist that are not covered. In certain metals and alloys, we sometimes observe a few grains,
generally widely scattered, that are far larger in size than the rest of the grains. E 930, on the
ALA (as large as) method, describes how to measure these "rogue" grains E 930 was written
by Robert Sleplan and Fran Warmuth It is also possible to have larger amounts of these
mixtures, and a number of such patterns can be observed. Such specimens exhibit a non-Gaus-
sian distribution of gram sizes and are referred to as blmodel or duplex. E I 18 l, written by
Jeremy P Morse [24] covers these situations Fran Warmuth is the present chairman of Sub
8
Sub I X on Inclusions was formed in 1940 and was chaired for twenty-five years by Samuel
Epstein of Bethlehem Steel's Research Department until he retired. His six successors have
served for the following twenty-six years Al Brandemarte is the current Sub 9 chairman.
Epstein had developed an Inclusion measurement method m his previous job at Battelle
[25] Standard E 45 was issued in 1942 containing a chart rating method based on Swedish
work and the nonchart method developed by Epstein. In 1960, a second chart method was
added based on work by Walker [26] and two years later, the third chart was added, the mod-
ified J-K chart for steels with low inclusion contents. E 45 is also a widely referenced standard
and it has been revised nine times
Sub IX also developed a standard practice for detecting large inclusions in beanng steels by
ultrasonics [27], E 588 It was transferred to E7'sjunsdlCtlOn m 1984 Sub 9 is presently eval-
uating the electron beam melt button test for rating the inclusion content of superalloys
Sub X was not one of E4's big successes, either time it existed Formed first in 1949 as Sub
X on Decarburization, the sub members worked with the Society of Automotive Engineers
(SAE) and the American Iron and Steel Institute (AISI) to develop a measurement method,
but no E4 standard resulted, activity stopped m 1952, and Sub X was disbanded m 1956 In
1968, it was reborn as Sub X on Research. Whatever the original purpose was, nothing of sig-
nificance apparently resulted, and Sub X was again disbanded Sub X has two strikes against
it, but it has not yet gotten to bat for a third time
Sub X I on Electron Microstructure o f Steels was formed m 1949, and its name was changed
seven times m the next thirty-nine years, an E4 record Sub I 1 has had also the most chawmen,
eighteen since 1950, another E4 record Sub I l has also taken over the work of three other E4
subs, Subs 6, 15, and 16 Sub 11 has also sponsored more symposia and published more STPs
than any other E4 sub It has not been as prolific in developing standards, however, as it has
only developed two (E 766 and E 986, both written by Dave Ballard of the National Bureau
of Standards).
Sub I l had its origins at the 1947 annual meeting of the Electron Microscope Society of
America (EMSA) where discussions were held among transmission electron microscope
enthusiasts working with metals. They formally organized a group on 13 February 1948 and
then merged their group into E4 in 1949 Their first subchalrman, George E Pelhssier of U S
Steel C o r p , was appointed in 1950 They were a fairly large, very active group and published
seven detailed annual subcommittee reports in the 1950s before concentrating mainly on sym-
posia for this purpose
Electron microscopy was a hot topic in 1950 as the TEM provided at least an order of mag-
nitude increase in resolution over the light microscope at that time At that time, metal struc-
tures were only examined using replica methods, and Sub XI did outstanding work in devel-
oping these procedures Later, when thin foil methods were developed, Sub XI again played a
major role in developing this method Sub XI also produced a very popular manual on TEM
techniques, STP 547
While their initial work centered on ferrous alloys, Sub XI started a B group on nonferrous
alloys in 1954, the same year they published their first symposium as STP 155 A C group on
super strength alloys followed in 1956, and so did the STPs, STP 245 and STP 262 In 1960,
the C group topic was Electron Mlcrostructure of PH (precipitation hardened) AustenItic and
Ni-Based Alloys, a very active group A group on Electron Diffraction followed in 196 l, and
another STP, number 317. The electron microprobe analyzer was introduced and Sub XI got
interested A round robin was conducted on 316 stainless steel with Committee A l 0 .
In October of 1966, Sub XI formed a task group (number 6, numbers being used now) on
the Analysis of Extracted Phases in Superalloys under Matthew T Donachle, J r , of Pratt &
Whitney Aircraft. This group became a special task group, TG 001, in 1968, then in 1975 a
special subcommittee, E04 91, then in 1977 it became the only task group of a new subcom-
mittee as E04 16 0 l, then Sub 16 was merged back into Sub I l in 1983 and it was again a Sub
I l task group, completing a grand swing through E4V On the way, they did issue (in 1983) a
very fine standard, E 963, which describes a method for extracting second phases from NI-
based superalloys This T G was exceptionally active over the seventeen years, some of the
results of their round robins are described in Refs 28 and 29
Another very active task group was T G 1115 on fiber analysis, chaired by Kuldip Chopra of
ELKEM Metals Co. In the mid-1970s, there was a great deal of interest in contamination of
water and air by asbestos fibers However, there were no accepted methods estabhshed for sam-
piing water, or air, and then for identification There were Individuals performing such work,
for example, using polarized light examination, but the federal laws being passed would
require much greater testing, and many new laboratories would be doing such work New
approaches were being examined, for example, energy-dispersive spectroscopy (EDS) using
the relatively new scanning electron microscope (SEM) or electron diffraction (ED) using the
transmission electron microscope (TEM). Clearly, there was a need to establish standards. The
task group labored long and hard, but, alas, no ASTM standard was developed although a great
deal of insight was developed [30].
Sub 1 l's only standards (E 963 was written before Sub 16 was merged back into Sub 11)
have been in the area of scanning electron microscopy The SEM was commercially intro-
duced in 1965 and became an instant winner Dave Ballard of the National Bureau of Stan-
dards (now a consultant) wrote two standards, E 766 for SEM calibration [31] and E 986 for
SEM performance evaluation [32] In more recent times, Sub 11 has been conducting EDS
round robins, and a draft for a guide to energy-dispersive X-ray analysis (EDXA) has been
14 METALLOGRAPHY PAST, PRESENT, AND FUTURE
wntten by Dr John J Friel o f P n n c e t o n Gamma-Tech, current Sub 11 chairman Frank Vel-

try of Inco Alloys International organized the round robin
E4 never had a Sub 12, no one seems to know why, and, Sub 13 has been always the name
of our evening dinner activities at meetings, so we wliljump to Sub X I V o n Quantitative Met-
allography formed in 1960 As with Sub XI, George E Pelhssier of U S Steel Corp was its
first chairman One of their first activities was to work with Committee A3 on the graphite
rating charts in A 247 Work in 1963 was successful in adding the nodular graphite senes chart
to A 247 George A Moore of the National Bureau of Standards (NBS) made some very early
quantitative measurements of these chart pictures using a computenzed system developed at
NBS Dr Moore was an interesting person, and Sub XIV meetings were never complacent
events when he was present Legally blind, Moore could see more with his limited vision than
many people with 20-20 visionI
Sub 14 has sponsored four symposia and published each, the last being held in May 1990
and dedicated to Dr Halle Abrams, long time member and former Sub XIV chairman who
died of a heart attack in October 1989 Halle had been involved in all four of E4's MiCon
(Mtcrostructural Control) conferences, and this was the fourth when he died Sub XIV's initial
efforts in quantitative metallography were in the domain of manual methods. Its first standard
was E 562 on the point counting method Manual methods have not been forgotten as auto-
mated methods have become popular [33,34] Sub 14 wrote a standard practice for measunng
decarburlzatlon, the original goal of Sub X when it first formed in 1949, and has a manual
approach (which can be automated) for assessing banded or elongated mIcrostructures
George Moore's efforts in the 1960s and 1970s to develop image analysis procedures for mea-
sunng structures, like inclusions, have been achieved in the last several years with three image
analysis standards, E I 122, E 1245, and E 1382 E 1122 describes an Image analysis approach
for obtaining J-K inclusion ratings according to methods A and D of E 45, a manual chart
method It is presently being pursued aggressively by image analysis manufacturers and steel-
makers E 1245 descnbes a stereological approach for measuring second-phase particles, such
as inclusions, and it too IS gaining interest in the market place E 1382 descnbes approaches
for measuring grain size using semiautomatic and automatic image analyzers and hasjust been
issued With these three standards, E4 has been leading the way, pushing the development and
use of image analyzers Hence, they have been better than timely)
Sub 14 has several projects underway A new task group was formed to explore evaluation
procedures for thermally sprayed coatings. Sub 14 is also trying to develop an image analysis
procedure for assessing the shape of graphite in cast iron and is working on an approach to
classify grain boundary carbide films in sensitized austenltic stainless steels In the equipment
area, Sub 14 is trying to develop a calibration test slide that could be used also to test out newly
written computer measurement programs for precision and accuracy George Vander Voort
is chairman of Sub 14
Sub X V on Emission Microscopy was formed in December 1968 with Dr Erwin Eichen of
Ford Motor Co as chairman This sub was to cover scanning microscopy while Sub XI would
cover transmission microscopy. The work on the SEM resolution standard, E 766, actually
began under Sub XV, but was completed under Sub 11 Sub XV did hold a symposium, pub-
hshed as STP 485 In 1977, Sub XV was merged back into Sub XI Sub 16on Phase Identi-
fication in Metal Alloys was established in November 1977 with Rick Anderson-Decina as
chairman The work on E 963, reported above, was moved under Sub 16 In 1983, when E
963 was issued, Sub 16 was merged into Sub l 1
Sub 17 on Laboratory Evaluation and Safety began as special subcommittee E04.94 on
Standard Recommended Practice for Evaluation of Metallographlc Laboratories on 14
November 1977 under chairman Fran Warmuth of Special Metals Corp (now with Cameron
Forge Co ) At that Ume ASTM was recommending the E committees to create standards gov-
VANDER VOORTON HISTORY OF COMMITTEE E4 15
erning the evaluation of laboratones In 1981, this group became Sub 17, the same year that
they issued standard E 807 Sub 17 is now rewsmg E 807 and is working on a guide to labo-
ratory safety under Bob Nester.
Conclusion
Committee E4 has accomplished a great deal in its 75 years of voluntary service to the tech-
nical community Those accomphshments have come from the dedicated efforts o f m a n y indi-
wduals, both well known and not so well known, but all working together We need to remind
ourselves regularly of our goals so that we can continue to build upon the shoulders of these
grants of the past. There are still many worthwhde areas of endeavor for E4 activity despite
our past accomphshments
References
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pp 601-607
[2] Wyman, L L, "The Plastics for Mounting of Metallographlc Samples," Proceedings, Amencan
Sooety for Testing and Materials, Philadelphia, Vol 38, Part I, 1938, pp 511-5 t 5
[3] Wyman, L L, "A Mid-Century of Metallography--Retrospect and Aspect," Fifty Years o f Progress
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[4] "What Can Be Done to Improve Alloy Phase Nomenclatureg," Bulletin, American Sooety for Test-
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[5] Fmk, W L and Wyman, L L, "The New ASTM System of Alloy Phase Nomenclature," Materials
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[6] Rawdon, H S, "Report of Sub-Committee V on Micro-Hardness," Proceedings, Amencan Society
for Testing and Materials, Philadelphia, Vol 26, Part I, 1926, pp 572-580
[7] Vander Voort, G F, "Results of an ASTM E4 Round-Robin on the Preosion and Bias of Mea-
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[8] VanderVoort, G F,"OperatorErrorslntheMeasurementofMlcromdentationHardness,"Accred-
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[9] Mogerman, W D, Zay Jeffries, American Sooety for Metals, Metals Park, OH 1973
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1, October 1962, pp 842-843
[18] McMur&e, H F, "Progress in X-Ray Diffraction Data Compilations," Fifty Years of Progrcss in
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delphm, 1968, pp 192-200
[19] Wyman, L L, "The NewASTM Grain-Size Methods," Bulletin, Amencan Sooety for Testmgand
Materials, Phdadelphm, July 1956, pp 59-61
[20] Wyman, L L and Penrod, R E, "For a Unified Gram-Size Standard," Materials Research & Stan-
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1971,pp 59-78
[22] Davis, C H, "Gram Size Comparator," Bulletin, American Society for Testing and Materials, Phil-
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[23] Hull, F C, "A New Method for Making Rapid and Accurate Estimates of Gram Size," Transactions,
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451
[24] Morse, J P, "Standard Methods for Characterizing Duplex Grain Sizes," Standardization News,
Vol 15, December 1987, pp 44-46
[25] Epstein, S, "A Suggested Method of Determining the Cleanness of a Heat of Steel," Metals and
Alloys, Vol 2, October 1931, pp 186-191
[26] Walker, G W, "Rating of Inclusions ("Dirt Chart")," Metal Progress, Vol 35, February 1939, pp
169, 170 and 167
[27] "Detection of Inclusions in Beanng Quahty Steel by the Ultrasonic Method," Materials Research &
Standards, Vol 9, September !969, pp 21-24, 72
[28] Donachle, Jr, M J , and Knege, O H , "Phase Extraction and Analysis in Superalloys--Summary
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[29] Donachle, Jr, M J , "Phase Extraction and Analysis of Superalloys--Second Summary of Investi-
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[30] Chopra, K S, "Interlaboratory Measurements of Amphibole and Chrysotfle Fiber Concentration
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[33] Abrams, H, "Quantitative Metallography," Standardization News, Vol 5, December 1977, pp 16-
18
[34] Vander Voort, G F, "Advances in Microstructural Imaging--Directions m Metallography," Stan-
dardization News, Vol 16, November 1988, pp 50-57, and, Vol 17, February 1989, p 12
OIficers Committee E4 on Metallography
Chairmen
1916-1917 Edgar Marburg
1917-1924 Wdham Hastings Bassett
1924-1930 Henry C Boynton
1930-1936 Charles H Davis
1936-1938 John Torrey Norton
1938-1966 LeRoy L Wyman
1966-1972 Wdham D Forgeng, Sr.
1972-1974 Andrew W Danko
1974-1978 William D. Forgeng, Jr
1978-1982 Gunvant N Manmr
1982-1986 Halle Abrams
1986-1990 Francis J Warmuth
1990- George F Vander Voort
Secretaries
1916-1921 none
1921-1930 George F Comstock
1930-1936 Oscar E Harder
1936-1946 John J Bowman
1946-1966 Mary R Norton
1966-1970 Edward F O'Mara
1970-1973 John C Russ
1973-1974 Wdham D Forgeng, Jr
1974-1979 Robert M Sleplan
1982-1984 Albert Szlrmae
1984-1988 Donald R Green
1988-1990 Robert S Graham
1990- Richard K Wilson
First Vice Chairmen

1916-1936 none
1936-1944 Marcus A Grossman
1944-1964 R Earl Penrod
1964-1966 Wdham D Forgeng, Sr
1966-1972 Andrew W Danko
1972-1974 Larry Toman, Jr
1974-1978 Gunvant N. Mamar
1986-1988 Matthew J A Nousak
1988-1990 George F Vander Voort
1990 Donald R. Green
1990- Samuel M. Purdy
2nd Vice Chairmen

1916-1972 none
1972-1974 John C Russ
1978-1982 John A Hendnckson
1982-1984 Rick Anderson-Decma
1986-1988 George F. Vander Voort
1991- Albert V Brandemarte
Membership Secretary
1916-1964 none
1964-1965 Barn R Baner lee
1974-1976 Conme B Craver
1976-1979 Donald A Nail
1979-1981 TheresaV Brassard
1981-1986 GallV Bennett
1990- Thomas N Rouns
Honorary Officers
1964 (Vice Chairman) R Earl Penrod
1967 (Chairman) LeRoy L Wyman
1968 (Secretary) Mary R Norton
Subcommittee Chairmen
Sub I on Sample Selection and Preparation and Photography

1920-1927 Wdham Campbell
1928-1941 Edgar H Dlx, Jr
1947-1951 Joseph R Vdella
1951-1959 Frederick C Hull
1959-1966 Wdham D Forgeng, Sr
1966-1982 Samuel M Purdy
1982-1986 Roger Koch
1986- Samuel M Purdy
Sub 2 on Metallographic Terminology and Nomenclature of Phase Diagrams

1920-1925 HenryC Boynton
1925-1938 Arthur Phxlllps
1938-1940 Robert S. Wdhams
1948-1950 Paul A. Beck
1951-1955 Robert S Busk
1966-1974 Mary R Norton
1974-1978 Wdham D Forgeng, Jr.
1978-1985 Roger Koch
1985-1986 Gary Hamman
1986-1992 RobertS Graham
1992- Beth Knueppel
Sub III on Thermal Analysis/Sub 3 on Nomenclature

1920-1921 George K Burgess
1924-1928 Wdham E Ruder
1928-1933 Howard Scott
1949-1960 Paul A Beck
1960-1978 W d h a m L Flnk
1978-1979 Wdham L Mankms
1979-1985 MatthewJ A Nousak
Sub 4 on Photography
1920-1922 V H Blhlman
1922-1934 Henry S. Rawdon
1934-1951 Leon V Foster
1951-1957 Sidney Poole
1957-1968 George A Elhnger
1968-1971 Conme B Craver
1971-1975 Charles H. Brown
1975-1983 Rick J Anderson (later Anderson-Decma)
1983-1985 Gary Hamman
Sub 5 on Microindentation Hardness Testing

1923-1926 Henry S Rawdon
1948-1955 Alexander Gobus
1955-1958 WalterA Shebest
1965-1978 Larry Toman, Jr
1978-1980 William D Forgeng, Jr
1980-1982 Robert M. Slepian
1982-1983 Anthony DeBelhs
1989- Francis J Toye, Jr
Sub 6 on X-Ray Methods

1924-1930 Zay Jeffnes
1930-1933 Lores W. McKeehan
1933-1937 Robert Franklin Mehl
1937-1938 Horace Hardy Lester
1938-1960 Wdham L. Fmk
1960-1971 Robert K Scott
1971-1973 AndrewW Danko
1973-1986 Leo Zwell
Sub VII on Methods of Thermal Analysis

1938-1940 LeRoy L Wyman, Sr
1940-1951 Laurence H Carr
1951-1970 Donald I Finch
1971-1972 Wllham D Forgeng, Jr
1972-1977 CharlesH Brown
Sub 8 on Grain Size

1931-1937 Clarence J Tobm
1937-1952 Marcus A Grossman
1952-1964 R Earl Penrod
1964-1968 Harold S Link
1968-1972 Edward F O'Mara
1972-1975 Wdham D. Forgeng, Jr
1975-1977 Donald E Van Inwegen
1977-1978 Robert Mdlsop
1982-1983 Ernest C. Pearson
1989- Franos J Warmuth
Sub 9 on Inclusions
1940-1965 Samuel Epstein
1965-1968 Gordon Meldrum
1968-1969 George H Baile
1969-1972 Gordon Meldrum
1972-1975 Gunvant N. Manlar
1975-1984 John A Hendrlckson
1984-1988 SherryA. Majoy
1988- Albert V Brandemarte
Sub X on Decarburization/Sub X on Research

1949-1953 John J B. Rutherford
1968-1974 Donald I Finch
Sub 11 on X-Ray and Electron Metallography

1950-1951 George E. Pellissler
1951-1953 D MaxwelITeague
1953-1955 William L Grube
1955-1956 Robert M Fisher
1956-1959 S T. Ross
1959-1961 Norman A Nielsen
196 l- 1963 Charles M. Schwartz
1963-1965 John R Mihahsln
1965-1967 Banl R. Banerjee
1967-1969 Thomas P Turnbull
1969-1973 George E. Pelhssler
1973-1975 GunvantN Manlar
1977-1980 KuldipS Chopra
1985-1986 Chuck Bnckner
1986-1989 Donald R. Green
1989-1991 Albert Szirmae
1991- John J Frlel
Sub 14 on Quantitative Metailography

1961-1964 George E Pelhssler
1964-1966 SamuelM Purdy
1966-1967 Wllham D. Forgeng, Jr
1979-1981 James Hider Steele, Jr.
1981-1982 EdwardJ Korda
1982- George F Vander Voort
Sub XV on Emission Microscopy

1969-1976 Erwm Elchen
1976-1977 Kuldlp S Chopra
Sub 16 on Phase Identification in Metal Alloys

1977-1980 Rick J Anderson-Declna
Sub 17 on Laboratory Evaluation and Safety

1977-1982 FranclsJ Warmuth
1982-1983 GunvantN Mamar
1983-1988 JeremyP Morse
1988-1989 Raymond M Mlddleton
1989-1991 Lmda K Kern
1991- Robert C Nester
Committee FA Award Winners
Award of Merit
Halle Abrams- 1983
Wdlard Bablngton- 1962
Andrew W Danko-1970
Wheeler P Davey-1952
George A Elhnger-1967
Samuel Epstein- 1966
Donald I. Finch-1963
Wdham L Fmk-1956
Alexander Gobus- 1964
Joseph D Hanawalt-1965
John A, Hendnckson-1986
George O Hlers-1959
Fritz V. Lenel-1958
Horace H Lester-1951
Roger P Loveland- 1966
Gunvant N Manlar- 1984
Fred W Matthews-1968
Warren H Mayo-1965
George A Moore-1977
Mary R Norton-1959
Leander F Pease, III-1989
R Earl Penrod-1957
Samuel M Purdy-1989
Frederick N. Rhmes- 1962
Harold W Rmn-1971
Theodore G Rochow-1968
Robert M. Sleplan-1980
Albert Szlrmae- 1990
Ernest E Thum-1954
George F Vander Voort-1987
Andrew Van Echo-1973
Francis J Warmuth- 1985
Vmcent P Weaver-1958
LeRoy L Wyman, Sr -1950
Fellows Prior to the Award of Merit

Wllham H Bassett
Henry Marion Howe
James G Morrow
Honorary Officers
LeRoy L Wyman-Honorary E4 Chalrman-1967
Mary R Norton-Honorary E4 Secretary- 1967
Wdham Campbell-Honorary B2 Chmrman- 1934
Honorary ASTM Members

Donald I Finch (Leeds & Northrup)- 1976
Wdham L Flnk (Alcoa Res Labs.)-1966
Wdham D Forgeng, Sr (Umon Carblde)-1974
Henry Marion Howe (Columbia Umversity)- 1919
Horace Hardy Lester (Watertown Arsenal)-1953
Warren H Mayo (US Steel)-1978
James G Morrow (Steel Co of Canada)- 1958
Henry S Rawdon (National Bureau of Standards)-1950
Andrew Van Echo (ERDA)-1975
Joseph F Woodruff (Armco Steel)- 1975
LeRoy L Wyman, Sr (National Bureau of Standards)-1967
Past ASTM Officers

William H Bassett-Member of Executive Committee 1916-1918, VP 1932-1934, P 1934-
1935 (he died only a few weeks after taking office on 7/21/34)
William Campbell-Member of Executwe Committee 1924-1926
Donald I Finch-Director 1971-1974
William L Fmk-Dlrector 1958-1961
Henry Marion Howe-VP 1898-1900, P 1900-1902 and 1910-1912 (Howe's name is the first
hsted on the ASTM Charter)
Zay Jeffnes-Member of Executive Committee 1930-1932
Warren H Mayo-Director 1967-1970
James G Morrow-Member of Executwe Committee 1944-1947, VP 1947-1949, P 1949-
1950
Albert Sauveur-Member of Executive Committee 1913-1915
(Edgar Marburg-Secretary-Treasurer 1902-1918, Marburg suggested the original ASTM
name and was the founding chairman of E4, he died m 1918)
L. L. Wyman Award
Halle Abrams- 1977
Wlllard W Bayre-1977
Francis J Warmuth- 1980
Wdham D, Forgeng, Sr -1982
John A Hendrlckson-1982
Erme Pearson- 1984
Roger W Koch- 1986
Matthew J A Nousak-1988
Jeremy P Morse-1988
Joseph R. Vilella Award

1974--Bruce L Bramfitt, Arian O Benscoter, James L Kllpatnck and Arnold R Marder
"The Use of Hot-Stage Microscopy in the Study of Phase Transformations," Metal-
lography--A Practical Toolfor Correlating the Structure and Properties of Materials,

A S T M STP 557, 1974, pp 43-70
1979--Morris Cohen and Steven S Hansen

"Mlcrostructural Control m Mlcroalloyed Steels," MiCon 78: Optimization of Pro-
cessing, Properties, and Service Performance Through Microstructural Control,
A S T M S T P 672, 1979, pp 34-52
1979--Harvey D Solomon and Thomas M Devine, Jr
"Influence of M~crostructure on the Mechanical Properties and Locahzed Corrosion
of a Duplex Stainless Steel," MiCon 78: Optimization of Processing, Properties, and
Service Performance Through Microstructural Control, A STM STP 672, 1979, pp
430-461
1986--Ervm E Underwood
"Practical Solutions to Stereologlcal Problems," Practical Applications of Quantita-
~.tveMetallography, A STM STP 839, 1984, pp 160-179
Other Awards
Charles B. Dudley Metal (for a paper of outstanding merit in the field of materials research)
Samuel Epstein, 1933, "Embnttlement of Hot-Galvanized Structural Steel," Proceedings,
ASTM, Vol 32, Part II, 1932, pp 293-379
Frederick C Hull, 1962, "Effects of Alloying Ad&tlons on Hot Cracking ofAustenmc Chro-
mmm-Nlckel Stainless Steels," Proceedings, ASTM, Vol 60, 1960, pp 667-690
Wilbur C Blgelow, 1964, "The Development of Electron Microscopic Methods for the
Study of Metals," STP 317, Symposium on Advances in Electron Metallography and Elec-
tron Probe Microanalysis, 1962, pp 58-139
Edgar Marburg Lecture (promote knowledge of outstanding developments in englneenng
materials)
George L Clark, 1927, "The X-Ray Examination of Materials in Industry," Proceedings,
ASTM, Vol 27, Part II, 1927, pp 5-51
Albert Sauveur, 1938, "The Torsion Test," Proceedings, ASTM, Vol 38, Part II, 1938, pp
3-20
Gillett Memorial Lecture
Norman A Nielsen, 1970, "Observations and Thoughts on Stress Corrosion Mechanisms,"
Journal of Materials, Vol 5, No 4, December 1970, pp 794-829
Richard L. Templin Award (for an outstanding paper describing new and useful testing pro-
cedures and mechanical apparatus)
Theodore G Rochow, 1973, "A Microscopical Automated Mlcrodynamometer Mlcroten-
slon Tester," Materials Research and Standards, Vol. 12, April 1972, pp 27-30, 53-54 (R
J Bates coauthor)
H. V. ChurchillAwards (given by Committee E2 on Emission Spectroscopy)
Joseph F Woodruff, 1974
Robert D. Thompson Award (given by Committee E20 on Temperature Measurement)

Donald I Finch, 1976
Anthony DeBellis Memorial A ward (given by Committee E28 on Mechamcal Testing for slg-
mficant contrlbuUons in the field on hardness testing)
George F Vander Voort, 1990
Mary R. Norton Memorial Scholarship Recipients

Elane C Sanderson, Colorado School of Mines, 1975
Margaret D Weeks, Carnegie-Mellon University, 1976
Elma B Stapes, North Carohna State University, 1977
Loranne M Brydges, Ilhnols Institute of Technology, 1979
Knstme M Stanecki, Umverslty of Michigan, 1980
Phylhs Anne Klein, University of Illinois at Champalgn-Urbana, 1981
M~chelle W Gabriel, Massachusetts Institute of Technology, 1982
Judith Glazer, Umversity of California at Berkeley, 1984
Amta J HIll, Duke University, 1985
Carol-Ann Baer, California Polytechnic State Umversity, 1986-1987
Leshe S Steele, Umversity of Dayton, 1987-1988
Chrysanthe Demetry, Massachusetts Institute of Technology, 1988-1989,
Yvonne Field, State Umverslty of New York at Stony Brook, 1989-1990,
Ann M Redsen, Umverslty of Wisconsin at Madison, 1990-1991
Jennifer S Wheeler, Purdue University, 1991-1992
W Elan McGee, Cahfornla Polytechmc Umverslty, 1992-1993
a
Committee E4 Standards at a Glance
E 2--Preparation of Micrographs of Metals and Alloys

Issued m 1917, E 2 was revised twelve times, and the title changed twice before being dis-
continued and replaced by E 883 m 1983 Grain size measurement methods were described
in E 2 from 1917 The first comparative grain size chart, for copper, was added in the 1930
revision but was deleted in the 1949 revision when E 79 was issued Standard definmons were
balloted m the 1923 revision but transferred to E 7, instead Ironically, photomlcroscopy
guidelines were first ballotted as E 7-23, but then incorporated into the 1924 revision o f E 2
E 3--Preparation of Metallographic Specimens

Issued in 1921, E 3 has been revised ten times, and its title was changed twice The initial
13 page document swelled to 33 pages when m 1935 it was revised and combined with E 5
With further revisions, it grew to 36 pages (1939), 43 pages (1944), 46 pages (1946), and 66
pages in 1958, then shrank as new standards were formed based largely upon it, for example,
E 340 and E 407 Later, E 1180 was developed to cover the sulfur pnnt method, described
briefly in E 3 up to 1980 Also m 1980, the electropohshmg information was deleted but a new
standard has not yet emerged
E 5--Metallographic Testing of Non-Ferrous Metals and Alloys

Issued in 1923, it was revised twice before being merged into E 3 in 1935
E 7--Definitions of Terms Relating to Metallography

Terms were first defined in a 1921 proposed revision of E 2 Sixteen were proposed but this
dropped to 13 In she 1923 revision, still under E 2 In 1924, this document was renumbered
as E 7, with 11 terms, and Issued as standard Metallography was added as a term m 1926, but
this defimhon was changed in 1927 (and has remained unchanged since) After four revisions,
E 7 remained at 12 definitions until 1955 when it zoomed up to a 45 page standard with 750
definitions Since 1955, it has been revised twelve times, mainly editorially through the addi-
tion of terms approved in other standards
E 14--Thermal Analysis of Steel

Issued m 1925, it was revised five times before new Committee E37 on Thermal Measure-
ments took over its jurisdiction in 1978 (it was discontinued in 1983)
E 15--Radiographic Testing of Metal Castings

Issued m 1926, it was revised twice before new Committee E7 on Radiographic Testing (now
in Nondestructive Testing) took over jurisdiction in 1939 (It was discontinued in 1949 )
E 19--Grain Size Chart for Classification of Steels

Issued m 1933, E 19 estabhshed the McQuald-Ehn carbunzmg method as the standard pro-
cedure for evaluating the austemte grain s~ze and the gram-coarsening tendency of steels.
Revised three times, it was discontinued in 1961 when E 112 was issued The 1933 version
contained a single chart showing the hypoeutectoid and hypereutectold regions of carburlzed
steels with grain sizes from l to 8 The 1939 revision added a second chart, stylized grain struc-
tures (black boundaries on a white matrix and white boundaries against a black matrix) Nei-
ther chart was incorporated into E 112
E 43--Identification of Crystalline Materials by the Hanawalt X-Ray Diffraction Method

Issued in 1942, it enjoyed a brief but stormy life Revised in 1946 and 1949, it was under
constant revision from 1951 on, reportedly completed in 1960, but wxthdrawn in 1961 How-
ever, revision work continued at least up to 1968 The method was considered too extensive
for a standard and a text was started but never published
E 45--Determining the Inclusion Content of Steel

Issued in 1942 and revised nine times, E 45 is presently undergoing a major overhaul The
mmal standard contained only one chart, the J-K chart, used for Method A and a nonchart
method (B) developed by Sam Epstein Method C and Plate lI were added in 1960 and Method
D and Plate Ill were added in 1962
E 79--Estimating the Average Grain Size of Wrought Copper and Copper-Base Alloys
Issued in 1949, E 79 was based on the chart and methods formerly in E 2 Two micrographs
were added to the chart in 1949 This chart, and the method, were merged into E 112 when it
was written (the chart was again expanded by two mlcrographs) and E 79-49T was discontin-
ued in 1963
E 80--Dilatometric Analysis of Metallic Materials

Issued m 1949, it remained as written until new committee E37 on Thermal Measurements
assumedjurls&CtlOn in 1978 (E 80 was discontinued in 1986 and replaced by E 228 )
E 8 l--Preparing Quantitative Pole Figures of Metals

Issued in 1949, it has been revised three times E 81 is an X-ray diffraction method for detect-
mg and describing crystallographic texture.
E 82--Determining the Orientation of a Metal Crystal

Issued m 1949, adopted without change and revised editorially twice, E 82 describes the
back-reflection Laue method The technique is used to determine the crystallographic orien-
tation of single crystals (or large crystals in a polycrystalline material)
E 89--Estimating the Average Ferrite Grain Size of Low-Carbon Steels

Issued in 1950 and approved m 1952, E 89 introduced the first correlation between the aver-
age intercept length and the ASTM grain size It contained a ferrite gram size chart for ASTM
gram sizes 1-8 E 89 was discontinued in 1961 after E 112 was developed and its chart was
dropped
E 9 ! - - E s t i m a t i n g the Average Grain Size of Non-Ferrous Metals, Other than Copper, and
Their Alloys
Issued m 1951, E 91 contained two charts for rating gram size, one with a fiat etch and the
other with a contrast etch Both charts were for twinned austemte grams and each contained
17 mlcrographs for ASTM 2 to 10 E 91 was discontinued m 1961 after E 112 was adopted
and both charts were dropped
E l 12--Determining the Average Grain Size of Metals

Issued m 1955, E 112 was the culmination of 37 years work replacing E 19, E 79 (developed
from E 2), E 89, and E 91 Four charts for rating gram size are included, three were new m
1955 Plate I for rating nontwmned grams with a fiat etch underwent extensive minor correc-
tions through the 1980s to enhance the precision of the mlcrographs E 112 has been revised
eleven times in its 36 year hxstory, its name has been changed twice, and it is one of the most
widely cited ASTM standards Nevertheless, it is under rewslon now
E 157--Assigning Crystallographic Phase Designations in Metallic Systems

Issued In 1961, E 157 has been revised four hmes It defines nomenclature for alloy phases
based on composmon and crystal structure
E 189--Determining Temperature--Electrical Resistance Characteristics (EMF) of

Metallic Materials
Issued m 1961, E 189 was revised once, and ~ts name was changed, before new Committee
E37 on Thermal Measurements took over jurisdiction m 1978 (It was discontinued in 1987 )
E 340--Macroetching Metals and Alloys

Issued m 1968, E 340 was based on macroetch mformaUon formerly m E 3 It has been
revised twice and ~ts name was changed once
E 381--Macroetch Testing, Inspection, and Rating Steel Products, Comprising Bars,

Billets, Blooms, and Forgings
Issued m 1968, E 381 was revised twice and its name was changed m 1979 Two plates are
used to rate the macrostructure A task group has been working on a major revision of E 381
to extend coverage to the rating of continuously cast steels
E 384--Microhardness of Materials
Issued m 1969, E 384 has been rewsed five t~mes and Its name was changed m 1976 It is
currently being revised extensively, including another name change
E 391--Presentation of Phase Diagrams

Issued m 1969, E 391 has been rewsed three times E 391 provides rules for drawing binary
and ternary e q m h b r m m phase diagrams for pubhcatlon
E 407--Microetching Metals and Alloys

Issued in 1970, E 407 was based on etchant information formerly in E 3 Its organization
approach is ideal for pubhcatlon (each etchant is described and given a number while a table
lists the suitable etchant numbers for different metals anti alloys) as redundancy is avoided but
this makes it extremely difficult to revise The original document contained 209 etchants and
has not been revised However, a task group has begun a revision and plans to create a com-
puter database program which would enhance its use and simplify future revisions
E 562~Determining Volume Fraction by Systematic Manual Point Count

Issued in 1976, E 562 was revised three times E 562 describes the manual point counting
approach for determining the volume fraction of phases or constituents in mlcrostructures
E 588~Detection of Large Inclusions in Bearing Quality Steel by the Ultrasonic Method

Issued in 1976, E 588 covered ultrasonic inspection procedures for detecting the infrequent,
irregularly distributed larger Inclusions that the microscopic methods will rarely detect It was
transferred to E 7'sjunsdictlon in 1984 and was revised in 1988
E 766--Calibrating the Magnification of SEM Using NBS-SRM-484

Issued in 1980, it was revised in 1986 E 766 describes how to calibrate a scanning electron
microscope A second revision IS in ballot now
E 768--Preparing and Evaluating Specimens for Automatic Inclusion Assessment of Steel

Issued in 1980, but not revised since, E 768 contains a color plate illustrating correct and
incorrect specimen preparation as evaluated by differential interference contrast (DIC)
illumination
E 807--Metallographic Laboratory Evaluation

Issued in 1981, a revision of E 807 is now in progress
E 883--Metallographic Photomicrography
Issued in 1982 and revised twice, E 883 replaced the venerable E 2 standard
E 930--Estimating the Largest Grain Observed in a Metallographic Section (ALA Grain

Size)
Issued in 1983, edltonal changes were made in 1989 and a revision is now in progress E 930
is used to rate the size of one or a few very large grains m an otherwise fine-grained matrix, a
problem not covered in E 112
E 963--Electrolytic Extraction of Phases from Ni and Ni-Fe Base Superalloys Using a

Hydrochloric-Methanol Electrolyte
Issued in 1983 after an extensive seventeen year effort, E 963 has not been revised since E
963 describes a techmque for bulk extraction of second-phase constituents from superalloys
E 975--X-ray Determination of Retained Austenite in Steel with Near Random

Crystallographic Orientation
Issued m 1984, E 975 has not been revised to date E 975 describes how to determine the
amount of retained austemte in steels using an X-ray dlffracUon procedure
E 986--Scanning Electron Microscopy Performance Characterization

Issued m 1984, and rewsed in 1986, E 986 describes an approach for assessing the imaging
performance of a scanning electron microscope. A revision is being ballotted now
E 1077--Estimating the Depth of Decarburization of Steel Specimens

Issued m 1985, an editorial change was made in 1986 and it was revised m 1991
E 1122--Obtaining JK Inclusion Ratings Using Automatic Image Analysis

Issued in 1986, E 1122 is an automated approach for obtaining E 45 method A or D ratings
It is becoming widely used as Image analyzer capabdlty has improved The first revmion is
being balloted now
E 1180--Preparing Sulfur Prints for Macrostructural Examination

Issued in 1987, this standard greatly expands on the simple instructions given in E 3 but
deleted in its 1980 revision Sulfur printing has become a popular method for evaluating the
macrostructure of continuously cast steels.
E 1181--Characterizing Duplex Grain Sizes

Issued in 1987, E 1181 addresses characterization of non-Gausslan grain size distnbuUons,
a problem not addressed by E 112
E 1182--Measurement of Surface Layer Thickness by Radial Sectioning

Issued in 1987, E 1182 describes a simple, elegant, approach for measunng the thickness of
surface layers or coatings
E 1245--Determining Inclusion Content of Steel and Other Metals by Automatic Image

Analysis
Issued in 1988 and revised in 1989, E 1245 provides an approach for characterizing discrete
second-phase particles, such as inclusions, carbides, or nltrldes, using automated quantitative
microscopy It incorporates an automated E 562 approach to determine volume fractions with
other basic measurements
E 1268--Assessing the Degree of Banding or Orientation of Microstructures

Issued m 1988, E 1268 describes a quantitative method for characterizing banded or ori-
ented mlcrostructures
E 1351--Production and Evaluation of Field Metallographic Replicas

Issued initially as emergency standard ES 12 in 1987, it became a standard in 1990 The
standard was w n t t e n due to the need to assess creep damage in steam pipes
E 1382--Determining the Average Grain Size Using Semiautomatic and Automatic Image
Analysis
Issued m 1990, but revised in 1991, E 1382 describes a n u m b e r of approaches for determin-
ing gram size using either s e m i a u t o m a t i c or automatic image analyzers
Symposia Special Technical Publications by Committee

E4
STP Year Title

28 1936 Symposium on Radiography and X-Ray Diffraction Methods
28A 1942 Symposium on Radiography
86 1948 Symposium on Metallography in Color
155 1953 Symposium on Techniques for Electron Metallography
245 1958 Advances in Electron Metallography
262 1959 Symposmm on Electron Metallography
285 1960 Symposium on Methods of Metallographic Specimen Preparation
317 1962 Symposium on Advances in Electron Metallography and Electron
Probe Mlcroanalysls
339 1962 Symposium on Advances in Techniques in Electron Metallography
349 1963 Symposium on X-Ray and Electron Probe Analysis (with E2)
372 1963 Techniques of Electron Microscopy, Diffraction, and Microprobe
Analysis
396 1965 Advances in Electron Metallography
430 1966 Fifty Years of Progress in Metallographlc Techniques
480 1969 Applications of Modern Metallographlc Techniques
485 1970 Energy Dispersive X-ray Analysis X-ray and Electron Probe
Analysis
504 1971 Stereology and Quantitative Metallography
547 1973 Manual on Electron Metallography Techniques
557 1973 Metallography--A Practical Tool for Correlating the Structure and
Properties of Materials
672 1979 MiCon 78--Optimization of Processing, Properties, and Service
Performance Through Mlcrostructural Control
Performance through Mlcrostructural Control
839 1984 Practical Applications of Quantitative Metallography (with IMS)
889 1986 MlCrOlndentatlon Techniques in Materials Science and Englneenng
(with IMS)
Performance through Microstructural Control
1094 1990 M1Con 90 Advances in Video Technology for Mlcrostructural
Control
1165 1992 Metallography Past, Present, and Future (75th Anniversary
Volume)
Committee E4 Chairmen
William Hastings Bassett
(born 7 March 1868 m New Bedford, Massachusetts, died 21 July 1934 just a few weeks after
becoming president of ASTM)
Bassett, the first chairman of E4 (the founding chairman, Edgar Marburg, was the Secretary-
Treasurer of ASTM, an employee and neither a metallurgist nor a metallographer) graduated
from Massachusetts Institute of Technology m 1891 with a bachelor's degree in chemistry He
began his career as a chemist, first with Pope's Island Manufactunng Co ( 1891 ), then teaching
chemistry for the Swain Free School (1895), then with New Jersey Zinc Co, Newark, New
Jersey (1900) In 1902, he joined the American Brass Co at its Coe branch m Torrlngton,
Connecticut, advancing to chief chemist and metallurgist m 1903 and techmcal supennten-
dent and metallurgist m 1912 at their Waterbury, Connecticut headquarters He joined ASTM
in 1903.
Bassett was a leading expert m nonferrous metallurgy and has been credited w~th mtroduc-
Uon of metailographlc and spectrographic techniques to the copper industry For his efforts m
implovmg the quahty of copper alloys, he recewed the James Douglas Gold Medal of the
American Institute of Mining, Metallurgical, and Petroleum Engineers (AIME) in 1925 In
1930, he was president of AIME He also helped to bring Cyril Stanley Smith to the United
States from the Umverslty of B~rmmgham
Henry Cook Boynton
(born 16'Apnl 1874 in Wlllsborough, New York, died 28 March 1970)

Henry, a founding m e m b e r of E4, was its second chairman (1924-1930) and was the first
chairman of Sub II (I 920-1925) He attended Harvard University receiving A B (1900), S M
( 1901) and Sc.D (1904) degrees While his A B was in geology, the graduate degrees were m
metallurgy Boynton was the first to receive a doctorate from the Department of Metallurgy
and was Albert Sauveur's first doctoral student He remained at Harvard until 1906 teaching
metallurgy and metallography and assisting Professor Sauveur
In 1906 he joined John A Roebling's Sons Co (Trenton, New Jersey) as a metallurgist and
stayed with them until retirement on 1 January 1947 He worked on the manufacture of high
strength wire for suspension bndge cables, for example, for the Manhattan, Bear Mountain,
George Washington, and Golden Gate bridges For most of his career, he was chief metallur-
gist at Roebhng's After retirement, he joined Temple Umversity (on 1 September 1947) as
head of their new department of metallurgy and consulting metallurgist in their Research
Institute. He continued this work until 1955, remaining as a consultant until 1960 when he
again retired
Henry was also very active m the A m e n c a n Society for Metals with the Philadelphia Chap-
ter, serving as chairman m 1931 The Philadelphia Chapter ran an adult course m metallurgy
at Temple Umversity for many years and Boynton was a lecturer in th~s program from 1935
to 1939 Henry was a strong believer m tolerance and moderation m all aspects ofhfe, personal
and professional
Charles Hollister Davis
(born 5 November 1886 in Manchester, Connecticut, died 22 May 1945)

Davis chaired E4 from 1930 to 1936 and prepared the mlcrographs for E4's first grain size
chart, for copper and brass, added to E 2 m 1930 After graduating from South Manchester
HlghSchool, he entered Yale Umverslty, recelvlngaB A ln geology in 1909 He pursued grad-
uate education at Yale in 1909-1910, then moved west in July of 1910 The balance of 1910
was spent mining in Idaho, surveying in Washington, and tounng through the Pacific North-
west He was a teacher and vice-principal at Manzanlta Hall (Palo Alto, California) while
studying geology at the Leland Stanford University. He recewed an M A in geology in 1912
He assisted Professor James P e m n Smith m a study of the paleontology of the area south of
Mt Shasta
Next, he took a job, m 1912, with the American Brass Co in Waterbury, Connecticut The
geologist was now a metallographer) During World War I, he was in charge of most of the
laboratory inspection work as brass was an important m u n m o n material By 1925, he was in
charge of the chemical and metallurgical laboratory and worked closely with Wdham H Bas-
sett Later, he was assistant technical manager
John Torrey Norton
(born 13 November 1898 in Medford, Massachusetts, died 18 July 1989)

John Norton, chairman of E4 from 1936 to 1938, recewed an S B degree in physics from
the Massachusetts Institute of Technology (MIT) in 1918, then joined the MIT staff as a
research associate m 1920 He was made an assistant professor of physics m 1926 His father,
Charles L Norton was head of the department of physics at MIT and his brother, Frederick
H Norton was an expert m ceramics and a member of the MIT department of metallurgy
John became very interested m the use of X-rays and gradually concentrated h~s interests in
this field In 1930, he was promoted to assooate professor of metallurgy, and in 1932, he
received his Sc D from M I T m metallurgy In 1941, he was promoted to full professor m the
physics of metals During World War II, he was head of the Radiographic Laboratory at MIT
and used X-ray inspection methods to solve a number of defense related problems, including
the assessment of residual stresses He also did fundamental studies on the bonding of pressed
powder metals For his contributions to the new field of powder metallurgy, he was awarded
the Plansee Plaque at the Fourth International Plansee Seminar (1961) in Austria, the first
American so honored
John Norton was chmrman of the faculty of MIT (1956-1958) and acting dean of the grad-
uate school (1961) He played an active role in developing the graduate curricula in metallurgy
at MIT In 1964, he retired becoming professor emeritus, ending nearly 75 years of service to
MIT by the three Nortons
Before retirement, he launched a business career as one of the founders (1957) of the
Advanced Metals Research C o r p , now AMRAY, I n c , the largest U S manufacturer of scan-
ning electron microscopes John acted as president from 1961 to 1973, then as board chairman
from 1973 until his death at age 90
LeRoy Linwood Wyman, Sr.
(born 20 September 1899 in Kenosha, Wisconsin, died 12 May 1975)

Roy Wyman, chairman of E4 from 1938-1966 and chairman of Sub VII on dIlatometnc
analysis ( 1938-1940), was also chairman of Committee A 10 on Iron-Chrommm, Iron-Chro-
mium-Nickel and Related Alloys from 1958-1966 He was named an honorary chairman of
both committees. He also was a founding member and chairman (1945-1957) of the Com-
mittee on Simulated Service Testing, a founding member of Committee F4 on Surgical
Implant Materials, a member of the Committee B9 on Metal Powders, a member of the exec-
utwe committee of Committee A 1 on steel, and a member o f several other ASTM committees
He was also one of the founders and a chairman of the Joint Committee on Powder Diffraction
Standards (JCPDS) He was a member of five U S National Committees involved with inter-
national standards
Roy attended the University of Minnesota, receiving a B Sc in chemical engineering m
1923 He spent h~s first year after graduation as assistant professor of metallurgy at the Okla-
homa School of Mines, then joined the Edison Lamp Works of the General Electric Co as a
metallographer He made some of the earliest cemented carbides in the United States in this
Job In 1929, he transferred to the General Electric Research Laboratory m Schenectady, in
charge of metallography In 1931, he was also put m charge of the X-ray diffraction laboratory
He headed the department of metallography and X-ray diffraction for the next 13 years
In 1942, he was given a year's leave from General Electric to serve as research supervisor,
War Metallurgy Committee, Office of Scientific Research and Development, National Acad-
emy of Science In this posmon, he supervised research projects vital to the war effort He
returned to the General Electric Research Laboratory m 1944 as halson officer, metallurgy
From 1947 to 1953, he was in charge of alloy research at the Knolls Atomic Power Laboratory
of the Atomic Energy Comm~sslon
In 1953, W y m a n switched careers, joining the National Bureau of Standards as chief of
chemical metallurgy in their metallurgy dwlslon From 1961 to 1965 he was a consultant for
the National Bureau of Standards Following retirement, he took an active roll m the operahon
of the Joint Committee on Powder Dlffract~on Standards and was its chmrman at the time of
his death
W y m a n received numerous awards for h~s work He received the ASTM Award of Merit in
1950 and was made an honorary ASTM member in 1967 He received a Certificate of Merit
from the Office of Scientific Research and Development in 1945 and the Sdver Medal of the
U S Department of Commerce m 1958
William Daniel Forgeng, Sr.
(born 31 May 1909 m Scranton, Pennsylvama, died 4 June 1986)

Committee E4 has the unique distraction of father and son c h a i r m e n - - a n d with terms only
two years apart Bill Forgeng, Sr followed LeRoy W y m a n as chairman, his term was 1966-
1972 He also served as vice-chairman and chairman of Sub I on Selection and Preparation of
Samples
Ball senior received a bachelors degree m chemistry from Cornell University in 1930, then
did his Ph D. under Clyde W Mason (famed chemical microscopist) at Cornell in 1934 In
that year, he joined the Union Carbide Research Laboratories in Long Island City, New York
(moved m 1935 to Niagara Falls where Ball junior was born) Bill senior replaced Joseph R
Vdella who did not want to move away from New York City Vllella's wife, Eve, was a well-
known high fashion model in New York City Vdella joined U S. Steel's research laboratory
in Kearny, New Jersey, and also had an outstanding career
Bdl semor stayed with Union Carbide his enUre career, retiring in 1973 as semor research
fellow He pubhshed over thirty papers and had a half dozen patents He was recognized as an
expert m the metallography of stainless steels (he helped develop the 200 series), refractory
metals and other heat- and corrosion-resistant alloys He was also noted for his work on inclu-
sion identification, phase identification by X-ray diffraction, and color metallography During
World War II, he studied uranium production and fabrication under the Manhattan ProJect
He was made an honorary ASTM member m 1974.
Andrew William Danko
(born 11 December 1917 in Coraopohs, Pennsylvania, died 9 November 1987)

Andy Danko served as chairman of E4 ( 1972-1974), vice chairman (1966-1972) and chair-
man of Sub VI on X-ray methods (1971-1973) He joined E4 in 1952 After receiving his B S.
in chemical engineenng in 1940 from the University of Pittsburgh, he joined Westinghouse
Electric Corp in their Materials Engineering Department (became the Materials Research
Laboratory in 1960) as a chemist He progressed to supervisor of Optical, Electron and X-ray
Metallography, Materials D e p t , Astronuclear Laboratory at their Large, Pennsylvania site in
1962
In 1944, he introduced use of X-ray diffraction as an analytical tool at Westinghouse He
designed and built a number of X-ray instruments, for example, mlcroradlography cameras,
both film and dlffractometer pole figure gonlometers, and devices for measuring residual
stresses In 1956, he set up their first transmission electron microscope for service work In
1960, he recommended addition of an electron microprobe to the service group and devoted
subsequent efforts to standardization efforts for compositional work
Andy joined the Joint Committee on Powder Diffraction in 1956 and served as vice chair-
man from 1970-1973 and Secretary/General Manager from 1973 to 1979 He was also active
in ASTM Committees E2 and E3 and received the Award of Merit in 1970
William Daniel Forgeng, Jr.
(born 26 July 1935 in Niagara Falls, New York)

Bill Forgeng, Jr served as chairman of E4 only two years after his father, from 1974-1978
He also served as secretary and was chairman of five different subcommittees (an E4 record)"
Subs 2, 5, 7, 8, and 14 Bill j u m o r also received his bachelors degree (in metallurgical engi-
neering) from Cornell University (1958), then received a Ph D from Purdue University in
1962. Following graduation, he joined the Rochester Products Division of General Motors
C o r p , then in 1964joined U S Steel Corp In 1980, he joined the staffofthe Cahfornia Poly-
technic State University in San Luls Oblspo where he ~s presently a professor in the Depart-
ment of Materials Englneenng
Bill states that his career has been influenced by two great metallographers--hls teaching
was influenced by Dr Clyde Walter Mason, the chemical microscopist from Cornell Univer-
sity, and his hands-on skills were influenced by his father Bdl did not begin his career as a
metailographer His work with General Motors and his first assignments at U S Steel were in
the area of products and process development In 1966, Jim Alger of the apphed research lab
at U S. Steel was looking for a supervisor of a metallographlc service section Since he knew
of Bdl's educational background, and heritage, he offered the j o b to Bill, which he took and
held for the next thirteen years Bill got revolved in some ploneenng work in image analysis,
with the Quantimet B, in scanning electron microscopy, with a Cambridge Stereoscan, and in
automated polishing, with the Struers Abrapol Bill even made presentations on these subjects
at E4 symposia)
Bdl always enjoyed his A S T M actwmes. He parhculady enjoyed coming to meetings, partly
because his Dad would always buy droner) By 1979, Bdl had gotten disillusioned w~th the steel
industry and had grown t~red of coping w~th winters m P~ttsburgh Because he most enjoyed
the instructional side o f his j o b at U S Steel, Bill decided to go into academm He wanted a
posmon where teaching came first and found a position at Cahfornm Polytechnic, where it
never snows) Bdl has a heavy teaching load, usually averagang four lectures and four labs per
week. He has his students reading and using A S T M standards m their labs Bdl ~s still acUve
wRh E4 but generally cannot attend meetings now
Gunvant Nandlal Maniar
(born 27 May 1932 in Karachi, Pakistan)

Gunny, an E4 member since 1962, was chairman of E4 from 1978 to 1982 after serving
previously as First Vzce Chairman from 1974 to 1978. He also served as Chairman of Sub 9
(1972-1975),Sub 11 (1973-1975), and Sub 17(1982-1983) G u n n y w a s c o e d l t o r o f S T P 547,
Manual on Electron Metallography Techniques, and of STP 557, Metallography--A Practi-
cal Toolfor Correlating the Structure and Properties of Materials, and was editor of the first
MiCon conference proceedings, STP 672. G u n n y has also been active with the American Soci-
ety for Metals, (ASM) serving as chairman of the Lehigh Valley Chapter (1973-1974) and with
the national organization as a member of the Handbook Committee (1975-1980) and as
chairman of this committee (1978-1980) He was a member of the Long Range Planning
Committee ( 1981-1984) and an ASM Trustee ( 1988-1989) He received the Bradley Stough-
ton Award of the Lehigh Valley ASM Chapter m 1979
He received a B Sc. m chemistry and physics from Gujarat University of India (1953), and
M S in metallurgy from Stevens InsUtute of Technology (1958) and an M S E m metallur-
glcal engineenng from the Umverslty of Michigan (1960) He was employed by the Auditor
General's Office, Government of India, from 1953-1956 He acted as a teaching assistant
while at Stevens and as a research assistant while at Michigan In 1960, he joined Crucible Steel
Co m Pittsburgh as a staff metallurgist
After two years with Crucible Steel, G u n n y came to Carpenter Technology Corp as a super-
visor m their R&D Center in 1962 In 1973, he was promoted to manager of physical metal-
lurgy and m 1977 was made general manager of the R&D laboratories He is presently man-
ager of New Products Development, a posmon he has held since 1983 Gunny is a Fellow of
ASTM and ASM He holds three patents and has published about thirty papers
Halle Abrams
(born 16 January 1938 in New York, New York, died 15 October 1989)
Halle joined ASTM and E4 in 1970 and was extremely acnve with E4 over the next nineteen
years He was chairman from 1982 to 1986 following four years as first vice chairman (1978-
1982) and four years as second vice chairman (1974-1978) Halle was also chairman o f Sub 8
( 1985-1989) when he died and had earher been chairman of Sub 14 (1972-1978) Halle was
active with all four MlCon symposia and was an editor for two of the resulting STPs He also
co-edited STP 557, Metallography--.4 Practical Toolfor Correlating the Structure and Prop-
erties of Materials. Halle's work on the intercept method for measunng grain size was Incor-
porated into the 1974 revision of E 112 He was also heavily involved with the development
of E 562, our manual point counting standard Halle also served as E4's representative to the
International Standards Organizauon
Halle studied chemical englneenng at the Polytechnic University of New York graduating
cum laude m 1959 He obtained M S degrees m chemical engineering from the New Jersey
Institute of Technology (1965) and in metallurgy from Lehigh University (1964) In 1968, he
obtained a Ph D in metallurgy and materials science from Lehigh University
He began his industrial career m 1959 at the former Western Electric Allentown (Pennsyl-
vama) plant D u n n g his etght years there, he pubhshed seven papers, two of which concerned
electrolytic polishing While working on his Ph D thesis, Halle taught at Lehigh from 1967 to
1968 In 1968, he joined Bethlehem Steel's Homer Research Laboratory, where he worked
until his death His research centered on alloy development, chiefly with hneplpe and plate
steels, strengthening mechanisms, structure-property-processing correlations, and quantita-
tive metallography He developed Beth Star 80, Bethlehem's 80 ksi yield strength plate grade
He was heavily involved with hneplpe orders and headed HRL's involvement with the North-
ern Border and Trailblazer projects His work earned him the D J Bhckwede Research Rec-
ognmon Award in 1982 He held four patents and authored or coauthored thirty papers He
was a senior research engineer at the time of his death
In 1983, Halle received ASTM's Award of Merit and in 1977, he was named (along with W
W Bayre) coreclplent of the first L L W y m a n Memorial Award from E4 He received the
Michael Tenenbaum Award in 1986 for the best paper at the 1985 Mechanical Working and
Steel Processing Conference of the Iron and Steel Society of the American Institute of Mining,
Metallurgical, and Petroleum Engineers, "Statistical Analysis of the Trailblazer Plate Chem-
istry, Processing and Property Data Base to Optimize X-70 Llneplpe Requirements" Halle
believed in living life to its fullest--he worked hard, he played hard He was enthusiastic, even
to excess, he was brash but lovable
Francis Joseph Warmuth
(born 31 May 1937 in Utica, New York)

Fran was chairman of E4 from 1986 to 1990 following service as First Vice Chairman from
1982 to 1986 and secretary from 1979 to 1982 He is currently Chairman of Sub 8 since 1989,
and was the founding chairman of Sub 17, serving from 1977 to 1983 Fran received a B.A
degree in Chemistry from Utica College of Syracuse University in 1958 He joined Special
Metals Corporation m 1958 and served in a number of positions, particularly as supervisor of
the Metallography Department from 1963 to 1984 Fran took an early retirement offer from
Special Metals in 1986 a n d j o i n e d Leco Corp in 1987 In 1988, hejolned the Cameron Forged
Products Division of Cooper Industries in Houston, Texas as supervisor of metallography
Fran has had a hfelong interest in photography and he led the work on Guide E 883 He has
one patent and has pubhshed a dozen papers He is a fellow of ASTM and received the L L
W y m a n Memorial Award
George Frederic Vander Voort
(born 1 September 1944 in Philadelphia, Pennsylvama)

George is the current ASTM chairman having served as first vice chmrman and second vice
chairman previously He has been chairman of Sub 14 on quantitative metallography since
1982 He was a coorgamzer of MiCon 86 and chairman of the MiCon 90 conferences, and
cochalrman of the Metallography Past, Present, and Future (75th Anmversary Volume) sym-
posium. He ~s the primary author of seven ASTM standards and is the current E4 represen-
tative to the International Standardization Orgamzatlon
George received a B S in metallurgical engineering from Drexel University m 1967 and an
M S in metallurgy and materials science from Lehigh Umverslty m 1974 In 1967, he joined
the metallurgical department of the Bethlehem Plant of Bethlehem Steel Corp. where he held
various positions In 1972, he transferred to Bethlehem's Homer Research Laboratory where
he was a research engineer m the metallurgical services and investigations group In 1983, he
joined Carpenter Technology Corp. as supervisor of their metal physics research group
George is well known for his work in light microscopy, particularly for color etching tech-
niques, and for his work in linage analysis He is the author of over eighty pubhcatlons includ-
ing Metallography: Principles and Practice (McGraw-Hill, 1984) He has been active with the
American Society for Metals (ASM) as an instructor in their Metals Engineering Institute and
for their video course, Principles of Metallography. He is a fellow of ASM as well as ASTM
He has also been active with the International Metallographic Society and was their president
from 1981 to 1983 George is an avid photographer and hiker and enjoys reading mystery
stones
Committee E4 Notables
Paul Adams Beck
(born 5 February 1908 m Budapest, Hungary)

Paul Beck chaired Sub II on terminology (1948-1950), starting the work that led to the vast
expansion o f E 7, and Sub III on nomenclature (1949-1960) He set up the prestzg~ous rater-
national committee of phase diagram experts that produced E 157
Beck studied mechanical engineering at the Royal Hunganan Technological InsUtute m
Budapest and then recewed an M S m metallurgy at the M~ch~gan Technological Institute in
1929 Next, he performed post-graduate work w~th M~chael Polanyl at the Kaiser Wilhelm
InsUtute of Metallurgy in Berhn and with Pierre Auger at the University of Paris His Industrial
career began m 1931 as a research engineer with the Vatea Electric Company m Hungary In
1933, he joined the Institute of Chemistry and Physics in Pans, followed by work as a patent
engineer m Budapest m 1935 Returning to the Umted States m 1937, he was a research met-
allurglst with the American Smelting and Refining Co in New Jersey In 1941, he joined the
Berylhum Corp (Reading, Pennsylvania) as chief metallurgist Then, in 1942, he became
superintendent of the metallurgical laboratory o f the Cleveland Graphite Bronze Company
In 1945, he entered academia as an associate professor of metallurgy at Notre Dame Pro-
moted to professor m 1949, he moved to the Umverslty of Illinois in 1951 as a research pro-
fessor In 1976, he officially retired, although he has continued active research on spmglass
alloys
Professor Beck has recewed numerous awards for research He is a fellow of the American
Physical Society, The Metallurgical Society of the American Institute of Mining, Metallurgi-
cal, and Petroleum Engineers (AIME) and the American Society for Metals (ASM) Interna-
tional and a member of the National Academy of Engmeenng He recewed the Mathewson
Gold Medal Award of AIME, the Albert Sauveur Achievement Award of ASM, the Alexander
Humboldt Award, the Heyn Memorial Award of the German Metallurgical Society, and he is
an honorary member of the Hungarian Physical Society He received an honorary doctorate
from the Montanumvers~tat m Leoben, Austria in 1976
John James Bowman
(born 29 May 1907 m Mlllersburg, Pennsylvanm, died 10 October 1950)

John Bowman was E4's third secretary, holding that office from 1936 to 1946 He became
secretary of Committee B7 on Light Metals and Alloys m 1944 and held that posmon until his
death from a heart attack at age 43 m 1950 He was also a sub chairman for Committee B6 on
Die-Cast Metals and Alloys and was acUve with the ASTM Pittsburgh D~stnct, serving two
terms as its chairman
Bowman graduated with honors from Pennsylvania State College (now University) in June
1929 with a bachelors degree in electrochemical engtneenng After graduation, he joined the
A l u m i n u m Research Laboratories of ALCOA Dunng the WWII, he served on the War Pro-
ductlon Board in Washington in the Conservation Dwlslon From 1943 to his death, he was
executive assistant to the chief metallurgist
Robert Schoiley Busk
(born 13 December 1915 in Brooklyn, New York)

Robert Busk chaired Sub II on terminology from 1951 to 1955 continuing the work started
by Paul Beck, the masswe enlargement o f E 7 He received a B.A in chemistry from Colgate
University (1937) and a D Eng in metallurgy from Yale University (1940) Joining Dow
Chemical Co. in 1940, he became director of the metallurgical laboratory (1956-1966), busi-
ness manager of wrought products (1963-1966), R&D manager of the Metal Products Depart-
ment (1966-1972), and assistant &rector of research (1968-1972) He retired from Dow in
1972 and opened his own business, International Magnesium Consultants, Inc
Busk is a fellow of the American Society for Metals International In ASTM, he was also a
m e m b e r of B6 and B7 and served as chmrman of subcommittees B06 07 and B07.04 He has
also been very active in the International Magnesmm Association serving as a member of their
board from 1978 to 1987 He was named an honorary lifetime member in 1988 He ~s the
author of Magnesium Product Design (Marcel Dekker, 1986) and holds 15 patents
Theresa Mary (Vandecar) Brassard
(born 3 January 1929 in Cohoes, New York)

Theresa served as E4 membership secretary from 1979 to 1981, worked with the ASTM
photographic contest and was a major contributor to E 768, particularly with regards to the
DIC photographic adjunct She served as secretary for Subs 1 and 17 and was a participant in
several task groups She will be remembered always for her innovative use of available mate-
rials in specimen preparation (for example, yellow tablet paper or brown paper towels rather
than cloths for pohshmg, "Never-Dull--the Original Magic Wadding Polish" for field polish-
mg ship propellers, etching BI-50 Sn with "Fresca," and so on)
Theresa gained her knowledge of metallography through selected courses at local colleges,
the American Sooety for Metals (ASM) Metals Engineering Institute courses and U S Army
correspondence courses, plus on-the-jobtrial-and-errorexpenmentatlon Shebegan hercareer
m 1953 as a metallographlc technician with Allegheny Ludlurn's research laboratory in Water-
vllet, New York In 1959, she joined the corporate R&D Center of the General Electnc Co in
Schenectady as a metallographer m the metals and ceramics laboratory In 1967, she became
a metallographer at the Benet Weapons Laboratory, ARRADCOM, of the Watervhet Arsenal,
Watervhet, New York. In 1983, she moved west, becoming a metallographer m the quahty
assurance laboratory at Long Beach Naval Shipyard, Long Beach, Cahforma. She retired in
1988
Theresa has also been acUve m ASM, with the Eastern New York chapter, and with the
International Metallographlc Sooety (IMS) She received several awards for her work with the
Eastern New York ASM chapter (President's Award in 1974 and 1977) and received the ASM
Metallurgical Engineering Assistants Award In 1975 Between 1959 and 1987, she received 37
awards in metallographic and ceramographlc contests sponsored by ASM, 1MS, ASTM, and
ACS.
William Campbell
(born 24 June 1876 m Gateshead-on-Tyne, England, died 16 December 1936)

Campbell, first chairman of Sub I and main author of standard E 2-17T, graduated from
Kang's College, London, m 1892, then studied at St. Kenelm's College, Oxford, from 1892-
1894 He recewed an assocfate in science degree from Durham University College of Science
in 1896, a B S degree m 1898, an M S. m 1903 and a D Sc in 1905 He came to Columbia
Umverslty m 1902 as University Fellow and was a Barnard Fellow the following year He
became an instructor m Metallurgy m 1904, adjunct professor m 1907, associate professor in
1912, and full professor m 1914 In 1924, he became the first Howe professor of metallurgy at
Columbia Aside from his academic experience, Campbell worked as a metallographer for the
U S Geological Survey (1907-1911) and the Bureau of Mines (1911-1921) Dunng World
W a r I, he was a metallurgist at the Brooklyn Navy Yard. In 1918, he was a lieutenant com-
mander m the Naval reserve, and he maintained this activity for many years
Campbell joined ASTM in 1903 and was Chairman of Committee B2 from its organization
m 1909 untd his retirement from Columbia in 1934 He was made honorary chairman of B2
He collected corns, both modern and ancient. He was often requested to clean and restore
ancient corns for various museums and collectors He published about fifty papers mclud-
lng"A List of Alloys" (ASTM Proceedings, 1992, revised m 1930), one of the earliest collec-
tions of alloy designations and compositions
George Frederick Comstock
(born April 1886 m New York, New York, died 2 August 1982)
George Comstock was E4's first secretary (1921 to 1930) and chaired Sub I twice, 1927-
1928 and from 1941 to 1947 As a chdd, his health was poor; hence, his schoohng began at
home by tutor Later, he recewed manual training at the Horace Mann School which spawned
a hfelong interest m woodworking His health improved with time and summers in the A&-
rondacks By 1908, he had made 53 ascents of fourteen mountains in the Adirondacks, includ-
ing cutting of a trail up Giant Mountain
Comstock entered Columbia University and received A B and Met E degrees in 1907 and
1909 Chess dominated his spare time, playing fourth board on Columbia's Championship
team (his exploits were recorded in the New York Sun n e w s p a p e r - - a far cry from today v)
He began his professional career in 1909 with the Vanadium Alloy Company's smelter in
Newmlre, Colorado A dam burst during a flood which closed down the railroad line and shut
down the smelter He then joined the Maryland Steel Company at Sparrows Point, Maryland
(now part of Bethlehem Steel Corp,) and then with Crucible Steel Co of America in Pittsburgh
as assistant to the chief metallurgist In 1912, he joined the Titanium Alloy Manufacturing
Co (TAMCO) in Niagara Falls, being placed In charge of their new physical testing laboratory
(built at a cost of $10 0001) He progressed to chief metallurgist and was assistant director of
research from 1946 to 1951 when T A M C O became a division of National Lead Co He retired
in 1951, but remained active as a consultant until 1954
Comstock published numerous papers on the use of titanium in irons and steels and two
books--Titanium in Steel (with Stephen F Urban and Morns Cohen, published by Pitman
in 1949) and Titanium in Iron and Steel (pubhshed by John Wiley & Sons and by Chapman
& Hall for the Engineering Foundation in 1955) He was an abstractor for ChemicalAbstracts
for many years
Besides devoting his professional career to the development of titanium alloys and titanium
additions to iron and steels, Comstock was literally "branded" with titanium, as he liked to
tell people In 1930, an experiment went awry causing an explosion which sprayed him with
molten titanium, "the titanium brand," and several mflhgrams embedded in his body ever
afted
Constance Lovell (Beams) (Brodie) Craver
(born 14 May 1911 in Newark. New Jersey)

Connie was the E4 membership secretary from 1974 to 1976 and chairman of Sub 1 from
1968 to 1971 She was a member of most of the E4 subcommittees and was quite active with
the ASTM photographic contest, which she chaired in 1966 for E4's 50th anniversary meeting
Connie began her professional career as a dietitian after graduating from Pratt Institute in
Brooklyn In 1930, Edgar Baln of the U S. Steel Research Laboratory in Kearny, New Jersey
decided that metallography would be a good field for women He contacted Pratt Institute in
his search for a woman to tram Connie expressed an interest in trying laboratory work in this
newly emerging, but unknown, field She worked for Baln for a year but moved to Schenectady
after her m a m a g e finding employment at the General Electric Research laboratory as an assls-
t a n t m e t a l l o g r a p h e r w o r k l n g f o r L e R o y L W y m a n Eventually she became head ofthe metal-
lographlc section. She learned her trade the hard way by good, old fashioned on-the-job
tramlng.
Conme left General Electric in 1950 to work for Allegheny Ludlum at their Watervllet
research facility Again, she worked with another eminent pioneer, Dr Gunther Mohhng,
inventor of A-286 In 1955, she was a coreclplent of the Lounsberry Award for her study of
precipitation hardening of alloy A-286. Connie trained Theresa Brassard when Theresa began
her career at Allegheny Ludlum In 1959, the laboratory was transferred to their Brackenndge
facility
In 1970, Connie retired from Allegheny Ludlum Steel Corp However, Conme was not
ready to rest and play shuffleboard No, she joined Rensselaer Polytechnic Institute and was
gwen responslblhty for the graduate school metallographic laboratory Finally, in 1980, after
fifty years of metallography, she retired for good Conme o n c e said, "I feel like a pioneer since
I have been privileged to see metallography grow from more or less an art to a science. It has
been an excmng experience"
Edgar Hutton Dix, Jr.
(born 11 August 1892 m BalUmore, Maryland, died 26 January 1963)

"Dixie" graduated from Cornell University in 1914 with a bachelors degree in mechanical
englneenng He dld some postgraduate studles and taught matenals testmg at Cornell Hethen
entered industry at the Morse Chain C o , then the Baltimore Copper Smelting and Rolling
C o , then as chief of the testing department of the Bureau of Aircraft Production, next as assis-
tant engineer of tests of the Aluminum Castings C o , then as chief of the metals branch, eng~-
neenng division, U S Air Service In 1923, he joined the Aluminum Co of America and
became chief metallurgist of the New Kensington and Cleveland laboratories in 1930 He was
appointed assistant director of research m 1942 and stayed with them until retirement
Dlx joined ASTM in 1919 and was a member of six committees, serving as chairman of our
Sub I from 1928 to 1941 He is best known as the inventor of Alclad sheet, the first major
development of an aircraft structural material since Wllm's duralumin in 1910 Alclad revo-
lutiomzed mrcraft construction He also developed AI-SI alloys as a new class of alloys and
developed a theory for stress corrosion cracking (24th Edward de Mille Campbell Memorial
Lecture of the American Society for Metals in 1949) He also served as chairman of the Insti-
tute of Metals division of the American Institute of Mining, Metallurgical, and Petroleum
Engineers. Dix received numerous awards, for example, the FrancisJ Clamer Medal fromthe
Franklin InsUtute in 1947, the Frank Newman Speller Award from the National Assocmtaon
of Corrosion Engineers m 1954, the Distinguished Public Service Award from the U S Navy
m 1958, and an honorary doctorate from the Carnegie InsUtute of Technology in 1958
George Austin Ellinger
(born 31 October 1900 in Lewlstown, Pennsylvania, died 27 Apnl 1985)

George Elhnger chaired Sub IV on photography from 1957 to 1968 and was active with the
ASTM photographic contest He was also active in Committees A5, B3, E25, and G1 He
received a B.S degree in mining and metallurgy in 1922 from Pennsylvania State College
Later, he took additional courses at the National Bureau of Standards (NBS) graduate school
George began h~s career in 1922 with the Standard Steel Works Co in Pennsylvania, as a
laboratory metallurgist In 1923, he joined the Atchison, Topeka & Santa Fe Railroad Co in
Kansas, as a metallurgist Two years later, he joined the Page Steel & Wire Co in Pennsylva-
nia, as chief chemist In 1927, he became a research metallurgist with Page In July, 1929, he
joined the metallurgy division of the National Bureau of Standards as an assistant physicist
In 1936, he became an associate metallurgist, then metallurgist in 1940, senior metallurgist in
1944, chief of the optical metallography section in 1946, chief of the corrosion section in 1950,
and in 1962, he was named chief of the Metal Reactions section and Assistant Chief of the
Metallurgy Division He retired on 1 January 1968 but remained active as a consultant
One of his first major efforts at NBS was the study of broken bridge wire from the failed Mt
Hope bridge This work was followed by studies of the weldablhty of armor plate, high tensile
strength steels, and some nonferrous alloys This knowledge was applied subsequently to the
construction of tanks and other armored vehicles where welding replaced riveting. Later, he
was deeply involved with the study of failures o f Liberty ships and T-2 tankers that occurred
during World War II.
Elhnger received the A S T M award of merit in 1967 His welding stu&es were honored by
the Lincoln Gold Medal of the American Welding Society in 1942 and the Meritorious Service
Award of the Department of Commerce in 1949.
Samuel Epstein
(born 27 November 1896 in Russia, died 15 Apnl 1972)

Sam Epstein, the first chairman of Sub IX on inclusions (1940-1965), was the pnnclpal
author of E 45 (one of the most widely cited ASTM standards) and its two major revisions in
1960 and 1962 His parents emigrated to Amenca and settled m Brooklyn when Sam was a
child Epstein graduated from the College of the City of New York (CCNY) in 1918 with a
B S in chemistry He took an Army Ordnance course in metallurgy at Carnegie and then was
stationed by the Chemical Warfare Service in the metallurgy &vision of the Bureau of Stan-
dards, Washington, D C He stayed at the Bureau until 1929 While at the Bureau, he was a
special student at George Washington University receiving an M.S m 1929 He developed an
automatlcpollshlngdevlcewhlleattheBureau Hejolned the Carnegle-Illinols Steel Co (later
part of U S Steel Corp ) in 1929 and in 1930, joined the recently formed Battelle Memorial
Institute in Columbus, Ohio
At Battelle, he authored volume 1 of Alloys of Iron and Carbon (McGraw-Hill, 1937) Also,
while at Battelle, he discovered that steels could be made fine grained by additions of small
amounts of aluminum and later determined that aluminum nitnde was responsible for grain
size control, not aluminum oxide as widely believed In 1932, he received ASTM's Dudley
Metal for his paper on embnttlement of structural steel by the galvanized zinc coating He
joined Bethlehem Steel's research department on 8 June 1936 and remained there until his
retirement on 31 January 1964 From 1950 to 1958, he was division head of the Steel Products
section of the research department. He developed the first nonagmg rimmed steel, developed
mtrlded ferrromanganese (for adding nitrogen to steel), did ploneenng work on leaded steels
(for improved machlnablhty), and developed a high-strength nvet steel He also did research
on the Fe-N phase diagram During World War II, he worked on beanng alloys for rolling mills
with a reduced tm content, tin being in short supply For this work, the Assocmtlon of Iron
and Steel Engineers gave him (and coauthor Richard C Hess) the John Frederick Kelly Award
in 1944 He developed a weathenng type structural steel, Mayarl R He received the Bradley
Stoughton Award of the Lehigh Valley Chapter of the Amencan Society for Metals in 1950
He received the ASTM Award of Ment in 1966. After retirement, he (and Robert E Somers)
rewsed the Welding Research Council book Weldability of Steels (2nd edmon, 1971)
Donald Ira Finch
(born 20 July 1907 in Grand Rapids, Michigan, died 28 September 1981)

Don Finch was chairman of Sub VII on Thermal Analysis from 1951 to 1970 and chairman
of Sub X on Research from 1968 to 1974 Don was also involved with the ASTM photographic
contest Finch received a B S in chemical engineering from the University of Michigan in
1929 Don pursued graduate studies, but left in 1930 to join Leeds and Northrup Co and
worked for them until 1972 He was a research metallurgist from 1930 to 1933 and 1935 to
1945, chief of the R&D metallurgical division from 1945 to 1955, head of the R&D metallur-
gical section from 1955 to 1968, then principal scientist from 1968 until retirement in 1972
Flnch's work centered on metals and alloys used with or within furnaces and furnace instru-
mentation He was also involved with temperature measurement systems for nuclear reactors
Don joined ASTM in 1945 Besides his E4 activity, he was a founding member and chair-
man of E20 on Temperature Measurements Don also served as a member of the ASTM board
of directors from 1971 to 1974 He chaired the Advisory Committee on Thermocouples to the
National Bureau of Standards and served as vice president and president of the Philadelphia
Chapter of the American Institute of Mining, Metallurgical, and Petroleum Engineers
Finch received numerous awards He was an honorary member of ASTM and a fellow. He
received the E20 Robert D Thompson award for 1976
William LaVilla Fink
(born 14 September 1896 in Falrmount, Indiana, died 2 April 1992)

Bill Fink studied at the University of Michigan receiving his B S E (1921), M S E (1923),
and Ph D in Chemistry (1926) Fink's thesis work at Michigan, under Edward DeMille Camp-
bell, utilized X-ray diffraction and showed that the strengthening phase in steels, martenslte,
was a solid solution of carbon in iron with a body-centered tetragonal crystal structure Prior
to this work, martenslte was believed to consist of extremely fine fernte grains Flnk measured
the lattice parameters and was the first to define the c/a ratio He also showed that tempenng
ehmlnated the bct structure producing a bcc structure. After this important contribution to
the understanding of the strengthening of ferrous alloys, Fink joined the Aluminum Co of
America in 1925 and never worked on Fe-based alloys again v He was chief of the physical
metallurgy division ( 1943-1958), then science coordinator until he retired in 1961 He taught
physical metallurgy at the Carnegie Institute of Technology (1936-1937) He was one of the
founders of the Joint Committee on Powder Diffraction Standards (JCPDS), later served as its
chairman He joined E4 m 1930
Flnk, an expert in X-ray techniques, served as chairman of Sub VI on X-Ray Methods from
1938-1960 and of Sub III on Nomenclature from 1960-1978 He is known as the "father" of
E 157 and played a major role in the development of E 391 The "Fink Method" for identi-
fying unknowns using the JCPDS Search Manual was named in his honor He served on the
ASTM Board of Directors (1958-1961), received the Award of Merit m 1956 and was made
an honorary member in 1966 He was also a member of E7 He received the C H Mathewson
Award of the American Institute of Mining, Metallurgical, and Petroleum Engineers for his
publication (with D W Smith) on the theory of precipitation hardening. Fink published over
forty papers and held twelve patents He was a fellow of the American Association for the
Advancement of Science
Leon Victor Foster
(born 11 August 1895 in Fulton, New York, died 26 July 1971)

Leon Foster was chairman of Sub 4 on Photography from 1934 to 1951 and was actwe with
the ASTM photographic contest He received a B S m liberal arts from Syracuse University
m 1917 He joined Bausch & Lomb Optical Co in 1917 and spent his entire career with them
From 1917 to 1920, he was a "computer," from 1920 to 1926, a lens designer, then group
leader (1926-1932), and section head (1932-1945) of the lens design group From 1945 to
1950, he was acting head of the science bureau of the microscope design section In 1950, he
became director of the defense engmeenng department, and, in 1960 he was liaison engineer
until he retired at the end of 1960
Foster developed the legendary Foster calcite pnsm used with B&L metallographs to pro-
duce polarized light This prism was apparently rather challenging to construct but did pro-
duce superb polarized light and was highly regarded by users who depended on it to study
metals and alloys, such as beryllium, uranium and its alloys, niobium, and zirconium and Its
alloys
Foster joined ASTM In 1932 and was also active with D20 (Plastics), A3 (Cast Iron), El2
(Appearance), and D 13 (Textile Matenals) He was a member of the Optical Society of Amer-
ica, the American Microscopical Society, the Society of Motion Picture and TV Engineers,
and the Electron Microscopy Sooety of America
Marcus Aurelius Grossmann
(born 15 September 1890 in Youngstown, Ohio, died 21 May 1952)

Grossmann, E4's first vice chairman (1936-1944) and chairman of Sub VIII on grain size
from 1937 until his death in 1952, played a major role in developing E4's gram size standards
that led to E 112 (three years after his death) Grossmann, famous for his work on hardena-
blhty, recewed a B S from the Massachusetts Institute of Technology (MIT) in 1911, later
recewed a D Sc from Harvard m 1930
After a year as an assistant at MIT, Marc joined Pittsburgh Testing Laboratories (1912-
1915), then Vanadium Corp of America ( 1915-1917), the Bureau of Standards ( 1917-1919),
again at Vanadium Corp (1919-1920), then the Electric Alloy Steel Co which became the
Atlas Steel Corp (1920-1924), next the Umted Alloy Steel Corp which became the Central
Alloy Steel Corp and later the Republic Steel Corp (i 924-1931), and, finally, the Illinois Steel
Co which became the Carnegie-llhnols Steel Corp and later part of the U S Steel Corp (1931
until his death in 1952) He became director of research at Carnegie-Illinois in 1935
Grossmann was noted for his wit, his wide range of knowledge, his skills m writing and
speaking A series of his lectures became the well known book, Principlesof Heat Treatment,
published by the American Sooety for Metals (ASM) in 1935 The fifth edition (1964) was
revmed by Edgar Bain after Grossmann's death He also translated Emil Heyn's book, Physical
Metaliography, pubhshed m 1925 by John Wiley Together with Baln, they pubhshed High
Speed Steel with John Wiley m 1931
Grossmann received numerous major awards for his work His doctoral thesis ("Oxygen in
Steel"), under Albert Sauveur, was the subject of his Campbell Memorial Lecture in 1930 His
paper on "Hardenabihty and Quenching, and Some Quantitative Data" (Transactions, ASM,
194 l, co-authored with M Asimow and S F. Urban) received the Henry Marion Howe Medal
while his paper "Hardenablllty Calculated from Chemical Composition " (Transactions,
AIME, 1943) received the Robert W Hunt Gold Medal He was a chairman of three different
ASM chapters, national trustee ( 1939-1941), vice president (1942) and president (1943) of the
American Society for Metals
Joseph Donald Hanawalt
(born 6 July 1902 in Royersford, Pennsylvama, died 26 June 1987)

Don Hanawalt was a long time member of Sub VI of E4, beginning in 1935, a member of
E7 since 1941, and was a founder and chairman of the Joint Committee on Powder Diffraction
Standards (JCPDS) Don studied at Akron University and Jumata College He received an
A B from Oberhn College m 1924, an M A from the University of Wisconsin m 1926, and a
Ph D in physics from the University of Michigan m 1929 He was a National Research Coun-
cd Fellow, Rockefeller Foundation from 1929 to 1931 and an International Research Fellow
at the University of Gronmger (the Netherlands) in 1931 He joined Dow Chemical Co as a
physicist m 1931, advancing to director of the spectroscopy laboratory m 1934, director of
metallurgical research m 1940, head of the magnesium department in 1946, vice president m
1953 and vice president of Dow Metal Products m 1959 He retired m Apnl of 1964 and joined
the University of Michigan as professor of chemical and metallurgical engxneenng where he
taught and continued his interests m magnesium technology until 1972
The publlcanon of his landmark paper on chemical analysis by X-ray dlffracnon m 1938
opened the way for the implementation of a powerful new tool The data pubhshed m this
paper became the foundation for the ASTM card file for compound ldennficatlon, now under
control of JCPDS In his magnesium research, his 1941 paper estabhshed the influence of
heavy metal impurities, for example, iron, mckel and copper, on the corrosion rate of mag-
nesium and magnesmm alloys From this work evolved a number of alloys with vastly
improved corrosion resistance He also developed a fluxless melting procedure for melting
magnesium, for which he received the Directors Award from the Magnesium Association m
1972 He held 30 patents and received a number of awards, for example, the Mathewson Gold
Medal of the Insntute of Metals of the American Insntute of Mining, Metallurgical, and Petro-
leum Engineers (1943), and the Gold Medal of the American Sooety for Metals (1965) He
was a Fellow of ASM and ASTM
Oscar Edward Harder
(born m 1883 m Frankhn County, Arkansas, died 10 July 1956)

Oscar was the second secretary of E4, serving from 1930 to 1936 His parents were pioneers,
traveling by covered wagon from Tennessee to Arkansas where he was born m a log cabin
While a boy, they moved to Texas and later to Oklahoma in a prairie schooner Although he
never graduated from either grade school or high school, he was admitted as a special student
to the University of Oklahoma m 1905 He received a B A m chemistry in 1910 and an M S
m 1911 After a brief period of employment as a food chemist, he enrolled at the Umverslty
of Illinois m Urbana and received a doctorate m chemistry in 1915
His first contact with ASTM came at the Lewis Institute in Chicago where he stu&ed cement
and concrete for an ASTM research committee and the Portland Cement Assoclatmn Next,
he held an alloy scholarship ( 1918-1919) at the Mellon Institute of Pittsburgh studying ura-
nium In September 1919, he succeeded Samuel L Hoyt as professor of metallography at the
Umverslty of Minnesota In his eleven years there, he taught a unique course m dental met-
allography and &d work on gold alloys, drill rod, bearing alloys, rail steel, and steel castings
In 1930, Oscar came to the Battelle Memorial Institute (founded in 1929) as assistant direc-
tor He retained this posmon until his retirement in 1949 and continued as a technical advisor
and consultant until his death m 1956 at age 73 He held more than 100 patents in twenty
counmes for his developments He is best known for two developments, leaded steels known
as "ledloy" and a corrosion-resistant, nonmagnetic alloy for watch spnngs called "elglloy"
(40Co-20Cr- 15N1-7Mo-2Mn- 15Fe-0 15C-0 05Be heat treated to 380 ks1 tensile strength, 702
HB)
Harder was active with several technical societies He was a trustee ( 1930-1932), vice-pres-
ident (1940), and president ( 1941 ) of the American Society for Metals (ASM) He was presi-
dent of the Minnesota Section of the American Chemical Society and was a section editor of
ChemicalAbstracts (1930-1953) He received the Henry Marion Howe Medal in 1928 for his
paper "Studies on Normal and Abnormal Carbunzing Steels" (Transactions, ASM, 1928)
Henry Marion Howe
(born 2 March 1848 m Boston, Massachusetts, died 14 May 1922)

Howe, first president of ASTM, a founding member of E4 and main author of standard E
3, was the nation's outstanding metallurgast of his day His father, Dr Samuel Gndley Howe
left for Greece shortly after recewmg his medical degree and parUclpated for six years m their
war for independence He pubhshed a History of the Greek Revolution m 1828 Returning to
America m 1831, he began working w~th the blind and headed the Perkins Institute for the
Bhnd His mother, Juha Ward Howe, author and reformer, began pubhshmg poems at age 16
She wdl be forever remembered for her "Battle H y m n of the Repubhc" written to the tune of
"John Brown's Body" whde she was at the front during the Cwd War (1861).
Howe attended the Boston Latin School, then entered Harvard graduating m 1869 with an
A B degree He recewed a B S from the Massachusetts Institute of Technology (MIT) m 1871,
and an A M degree m 1872, m metallurgy, from Harvard He then spent a year m Troy, New
York studying the production of iron and steel and in 1872 became superintendent of the
Bessemer Steel Works m Johet, Illinois followed by the Blmr Iron & Steel Co (1873-1874)
Next, he spent five years on the metallurgy of copper m Chde and designing plants m Quebec
prownce and Bergen Point, New Jersey for the Orford Copper & Nickel C o , followed by man-
aging the Plma Copper & Smelting Co of Arizona This work was the nucleus of his first book,
Copper Smelting, pubhshed m 1885
At age 35, he changed his career path and became a consultant m Boston whde also teaching
at MIT untd 1897 when he was offered the chmr of metallurgy at Columbm Umverslty He
remained their untd retirement in 1913, as professor emeritus He continued to perform
research at his laboratory at h~s home "Green Peace" m Bedford Hdls, New York, untd his
death in 1922 at age 74 He also acted as a consultant to the Bureau of Standards from 1918
untd h~s death
In 1891, Howe pubhshed The Metallurgy of Steel, which collected all of the knowledge at
that u m e on steeimakmg, be ~t m Enghsh, French, or German Th~s book &d much to change
steelmakmg from an art to a science In 1903, he pubhshed Iron, Steel, and Other Alloys, and
in 1916, The Metallography of Steel and Cast Iron (m two parts). This later book was an mtro-
ducUon to the new science of metallography In 1910, Howe chmred an international com-
mittee on nomenclature under the International Assocmt~on for the Testing of Materials The
other U S delegates were W d h a m Campbell and Albert Sauveur whde the foreign delegates
were Flons Osmond and Leon Gudlet (France), H C H Carpenter, John E Stead and Walter
Rosenham (England), Carl Benedlcks (Sweden), F Wust and Emd Heyn (Germany), and A
Stansfield (Canada) Howe named the constituents femte, cemenute, and pearllte (the latter
based on Henry Clifton Sorby's "pearly" constituent) and the term eutecto~d
Howe was very active m professional orgamzat~ons, besides serwng twice as president of
ASTM In 1893 he was president of the American Institute of Mining, Metallurgical, and
Petroleum Engineers which he joined m 1871 He was acting president of the International
Assocmtlon for Testing Materials (1902-19 t 2) He recewed a host of honors, including three
honorary doctorates and medals from many countries, including Russia, France, England,
Germany, and Sweden He was a prohfic author with over 300 publlcaUons to his credit
Frederick Charles Hull
(born 9 November 1915 in Alliance, Ohio)

Fred Hull was chairman of Sub I from 1951 to 1959 and was an active contributor to E4's
grain size standards He developed improved approaches for performing companson grain size
ratings and the approach used when working at magnifications other than that of the chart
Fred received a B S in metallurgy from the University of Michigan in 1937 and a D Sc in
metallurgy from Carnegie Institute of Technology in 1941
Fred spent his entire professional career w~th Westinghouse at their research laboratories In
Pzttsburgh He started in 1941 as a research engineer In 1951, he was made manager of the
metallurgical sectton, in 1954 he became assistant manager of the metallurgy department, and,
m 1957, he was named advisory metallurgist He retwed in 1981 but worked as a part t~me
consultant unnl 1985
Besides his life long interest an grain size work, Fred has been active m alloy development
He is the inventor of Dtscaloy, a h~gh temperature alloy, and Kromarc, a stainless steel He
has eleven patents and twenty-s~x pubhcauons
In 1962, Fred received ASTM's Charles B Dudley medal for his paper "Effects of Alloying
Elements on Hot Cracking of Austenmc Stainless Steels" In 1974, he received the James F
Lincoln medal of the Amencan Welding Society (AWS) for his paper"Effects of Composmon
on Embnttlement of Austenmc Stainless Steels." The Institute of Metals (London) gave Fred
an "Elegant Work" award in 1989 for his paper"Plane and Spatml Charactenstlcs of Equmxed
Beta Brass G r a m s " Fred is a Fellow of the Amencan Society for Metals
Zay Jeffries
(born 22 April 1888 m Wdlow Lake, South Dakota, died 21 May 1965)
Zay Jeffnes, one of the outstanding metallurgists of this century, recommended that E4
establish a subcommittee on the new field of X-ray diffraction and was Sub VI's first chmrman
(1924-1930) Jeffnes developed the plammetnc method of grain s~ze measurement that was
incorporated into E4's first standard, E 2, and is now m E 112 He was a graduate of the South
Dakota School of Mines (mechamcal englneenng, 1910) and became an instructor at the Case
School of Applied Science m 1911 His first major paper was gwen at the February 1916 meet-
lng of the American Institute of Mining, Metallurgical, and Petroleum Engineers, on "The
Determination of Grain S~ze m M e t a l s " Zay stu&ed w~th Albert Sauveur at Harvard and
received his Ph.D. m 1918 for his study of secondary recrystalhzatlon
Jeffnes must have been an mcre&bly busy person as he led two careers s~multaneously. He
was a consultant to the lamp &ViSIOn of the Cleveland Wire Works ( 1914-1925) of the General
Electric Co (GE) and to the Cleveland &vision (1920-1936) of the Alcoa Research Laboratory
(he was &rector of research (1916-1920) of the Lymte Laboratory of the Aluminum Casting
C o , taken over by Alcoa m 1920). After six years of teaching at Case, he dwlded his t~me
between Alcoa and GE W~th R. S Archer, Zay developed aluminum alloys 2025, 5051, and
2014 and they wrote the popular book, The Science of Metals, m 1924 Jeffnes headed Alcoa's
research laboratory m Cleveland and Edgar Dlx headed the one m New Kensington, Penn-
syivanm With GE, he worked on problems with tungsten filaments, for example, the sag prob-
lem He installed the first X-ray spectrometer used by industry and hired a young graduate by
the name of Edgar Colhns Barn to operate it Barn later became a pioneer m the use of X-rays
and had an outstanding career with U S Steel (he was also an E4 member) W~th GE, he was
a consultant to the incandescent lamp department ( 1925-1936), techmcal &rector of the lamp
department (1936-1945), and vice president of the chemistry department (1945-1949). He
was Chairman of the Board of their subsldmry, The Carboloy C o , which produced smtered
carbide cuttmg tools He retired m 1950
Jeffrles suceeded Henry Marion Howe and Albert Sauveur as metallurgy's representaUve to
the National Academy of Science D u n n g World War II, he was chmrman of the Office of
Production Management on Strategic Metals He was president of the American Society for
Metals in 1941 As m~ght be expected, Zay recewed nearly every major award, several hon-
orary degrees, and was on the board of several restitutions
Horace Hardy Lester
(born 30 December 1883 in Shelburn, Indiana (see below), died on 11 November 1955)
Horace Lester ("Doc") was chairman of Sub VI on X-ray Methods from 1937 to 1938 His
pioneenng 1926 Sub VI report became the first ASTM standard on radiographic testing, E 15-
26T He was the founding chairman o f Committee E7, from 1938 to 1948 He was also active
with the Joint Committee on Powder Diffraction Standards He received the ASTM Award of
Merit in 1951 and was made an honorary member in 1953
Lester was the son of Mark and Sarah Jane (Rigley) Lester who were m a m e d in England in
1878 and emigrated to the United States in 1879 They settled in Shelburn, Indiana and began
naturalization proceedings However, in 1883, they rented their house for an indefinite penod
and returned to England Horace was born in the home of his maternal grandmother in Aws-
worth, Nottinghamshire, England He was about nine months old when the Lesters returned
to Shelburn, which he used as his legal birthplace When he was three, they moved to Carhsle,
Indiana where he grew up He graduated from Carlisle High School in a class of two students)
The high school program was for only three years Lester graduated from Vincennes Univer-
sity preparatory department m 1902 He worked his way through school at Vincennes Um-
vers~ty Jumor College graduating m 1904 He was a bus boy at the Grand Hotel m Vincennes
and tended the coal furnace m the home where he was staying Dr Eugene Manchester, pres-
ident of Vincennes Umverslty, took an interest m Lester's mathematical and scientific skills
and progress Manchester took a job with the Umverslty of Minnesota and Lester went with
him After recexvlng his bachelor's degree at Minnesota m 1906, Horace moved to the Um-
verslty of Washington where he obtained a master's degree in 1912 Again, he worked to cover
his hving expenses, this nine as a high school teacher m Anacortes (1906-1908) and m Bel-
lingham (1908-1910) where he taught botany and astronomy He became a night watchman
for fishing traps and began smoking a pipe (forever after!) He moved back east to Pnnceton
University where he received a Ph D in physics in 1915 He returned to the University of
Washington as an instructor (1915-1917) This was interrupted by World War I when he was
enlisted to install radio eqmpment on naval vessels m the Puget Sound Navy Yard (1917-
1920)
Lester again returned east and worked briefly for Westinghouse Lamp Co (Bloomfield, New
York) from 1920-1921, then took a teaching posmon at the Case School of Apphed Science
in Cleveland He had barely settled m at Case when he recewed an offer to work at the Water-
town Arsenal Laboratory General Tracy C Dickson had obtained X-ray eqmpment for radm-
graphic testing and X-ray dlffracnon, both areas were new at that time Dr F C Langenberg,
head of the laboratory, recruited Lester for the new posmon created by Dickson He started as
a research physicist m July, 1922 and, within a year, published "Radmgraphy of Metals," and
" X - R a y Examination of Steel Castings" The following year, 1924, he pubhshed (with the
A m e n c a n Society for Steel Tesnng (ASST), later the Amencan Society for Metals (ASM)) "X-
Ray Tests Apphed to Problems of the Steel Foundry" for which he received the Henry M a n o n
Howe medal in 1925 Lester quickly recogmzed the need to standardize radiographic tests
which led to his hfelong involvement with ASTM E4 and E7
Mary Norton reported that when Doc was doing desk work, he generally put on his lab coat
(rarely used when he did experimental work)), and an old peaked cap and then fired up his
pipe On a Saturday afternoon one summer, Arsenal personnel had left for home and their
month long vacation About an hour later all of the Building 73 employees who could be
reached by telephone were summoned back to work On the front lawn, General Dlckson was
conducting an mveshgatlon of a small fire that was discovered m Building 73 just after noon
The fire was caused by a nail that was d n v e n through a section of BX cable The fire had broken
out above a door on which Doc's lab coat was hanging The general was lambasting Lester's
p~pe for causing the fire since he knew that Doc often tucked it into his lab coat pocket, stdl
ht Naturally, the lab coat contained numerous burn holes)
Lester became a close friend of Albert Sauveur, the father of metallography in the United
States Sauveur invited Lester to teach an X-ray metallography course at Harvard for his grad-
uate students He did this from 1931 to 1936
Besides being a founder and first chairman of E7 (then called "on Radiographic Testing")
from 1938 to 1948, he was a founder and first president of the Society for Nondestructive Test-
mg In 1943, the Society for Nondestructive Testing established the Lester Honor Lecture in
recognmon of his accomplishments Their first handbook, published in 1960, was dedicated
m his memory and he was their first honorary member In 1944, he received the Civilian Ser-
vice Award from the War Department He received the ASTM Award of Merit (! 951) and was
named an honorary member (1953) ASM honored Lester with the Albert Sauveur Achieve-
ment Award m 1953 He was also a fellow of the American Physical Society and the American
Society for the Advancement of Science On May 17, 1960, the Army's first nuclear reactor
was dedicated as the Horace Hardy Lester Reactor Lester began the research project that ulti-
mately led to the mstallahon of the reactor at the Watertown Arsenal Research conducted
with this reactor demonstrated the phenomenon of radiation hardening He pubhshed twenty-
five papers, nearly all on radiography or nondestructive testing He retired in 1953, at age 70,
but continued as a consultant to Ordnance Matermls Research until his death
Francis Ferdinand Lueas
(born 7 August 1884 m Glens Falls, New York, died 20 June 1951)
Franczs Lucas was never an officer or subchmrman of E4 but he was a long time member
who contributed actively, for example, in the construction of the first grain size charts He was
widely regarded as one of the premier metallographers of his time and his advice was sought
Lucas was a self-educated man with no formal technical education At age 16 in 1902, he began
his career with the Bell System as a groundman with the Hudson Rwer Telephone Co He rose
to the posmon of district wire chief Next, he joined the Engineering Department of the
Southern Bell Telephone Company, and, m 1910 he joined the Western Electric Englneenng
Department, the predecessor orgamzatlon of the famed Bell Telephone Laboratories
H~s interest m m~croscopy began when he was placed in charge of respecting t~mber prod-
ucts As part of h~s inspection, Lucas purchased a microscope to study the wood In the early
1920s, hght microscopes were hmlted to about • 1000, or • 1500 with immersion objectwes
Lucas devoted considerable efforts, with the help of the Zelss works m Jena, Germany, to rais-
ing these hm~ts--first to • 3500, then to • 5000 and ulUmately, to nearly • 7000 These very
h~gh magmficat~ons were chiefly obtained by refinement oftechmques to permit utd~zaUon of
ultraviolet hght with its shorter wavelength and improved resolution The ultrawolet micro-
scope was not a new tool Biologists had attempted to utlhze them nearly twenty-five years
earher However, there are a great many problems revolved with the use of ultraviolet (UV)
hght, which ~s outside the v~s~ble spectrum How do you focus a hght that cannot be observed9
This and other problems, caused biologists to give up the UV m~croscope and ~t fell into
obscurity
Lucas was frequently revolved with consulting work In World War II, he examined the
mlcrostructure of paint films on sh~p hulls For the Pubhc Health Service, he made a motion
picture o f the hfe cycle of the syphflhs spirochaete Lucas was probably the first person to
observe the very fine m~crocracks that act as lnmat~on s~tes for fatigue fractures These cracks
were found to be assocmted with coarse, plate martens~te, the first recognmon of such cracks
Lucas published forty papers, about ten of whxch were devoted to the UV microscope, p e r
s e Others demonstrated the value of "the most powerful microscope m the world" for the
study of m~crostructures One paper studied austemte, two were on martens~te, one was on
fatigue lnltmtlon sites at martenslte m~crocracks, and two were on troost~te In the 1930s there
was considerable debate about the "lamellar famfly"--pearhte, troost~te, and sorblte Lucas's
ultrahigh magmficatmn work helped to show that troost~te was simply very fine pearhte where
the mterlamellar spacing was too fine to resolve with standard hght microscopes Lucas studied
other materials as well, for example, the surface of phonograph records, tumor cells in mice,
hvmg sperm cells m grasshoppers, and latex rubber He developed an "optical sectioning" pro-
cedure to produce complete plan wews oforgamc cells or metal crystals He had at least three
patents, one for an Insulating material, another for a steel alloy for submanne cable armor,
and the third for a method to detect fingerpnnts
In 1924, the American Society for Steel Testing (ASST) (later the American Society for Met-
als (ASM)) awarded him the Henry Marion Howe Medal for his paper on "High Power Pho-
tomlcrography of Metallurgical Specxmens." In 1931, he dehvered the American Institute of
Mining, Metallurgical, and Petroleum Engineers, Henry Marion Howe Lecture "On the Art
ofMetallography " A l s o m 1931, Professor Bradley Stoughton and Lehigh University awarded
Lucas an honorary D Sc He retired from Bell Labs on 31 August 1949 In 1957, ASM estab-
hshed the Francis F Lucas Award for excellence m metallography whxch was endowed by the
late Adolph E Buehler, founder and Presxdent ofBuehler, Ltd Lucas was ASM's delegate to
the World Engmeenng Congress in Tokyo m 1929 He was a fellow of the American Assoc~-
atxon for the Advancement of Science The Royal Photographic Society of Great Britain
awarded him medals for his work in 1926 and 1929 The Frankhn Institute conferred upon
Lucas the John Price Wethenll medal m 1935
Taylor Lyman
(born 13 September 1917 m Lemon, South Dakota, died 8 February 1973)

For many years, E4 had a close relat~onshlp with the American Society for Metals (ASM)
as Taylor Lyman and Ernle T h u m were both long time E4 and ASTM members, as well as
ASM employees Taylor Lyman's main E4 activity was as a member of Subs II and III He was
one of the experts on phase diagrams on Paul Beck's subcommittee that eventually developed
E 157 and, later, E 391 Lyman also enhsted a number of E4 members to prepare articles for
the American Society for Metals (ASM) Metals Handbooks.
Taylor was born m a private home next to the home of the doctor who delivered him, w~thm
sight of the plains of North Dakota Several days later, he and his parents returned to the log
cabin built by his father on their homestead claim m Thunder Hawk, South Dakota Later, he
regretted missing th~s opportumty to have been born, Lincoln-style, m a true American log
cabin H~s first ancestor m the New World, Richard Lyman, emigrated from England m 1631
and, w~th Thomas Hooker and Samuel Stone, founded the town of Hartford, Connecticut
(Hartford was originally called Newton) m 1636
Lyman a n d h l s famdy m o v e d t o Mt Vernon, South Dakota just before he entered grammar
school He was an excellent student and a hard w o r k e r - - d e h v e n n g the Sioux City Journal,
the Saturday Evening Post, the Ladies' Home Journal and the Country Gentlemen whde keep-
mg up with the routine chores of a country boy, such as chopping and stacking cords of wood
Besides academics, Taylor excelled in athletics Baseball was h~s favorite sport In high school,
he was captain of the basketball team and second m the discus throw in the state At Stanford
University, he played varsity baseball--the coach was Lefty O'Doul (he won National League
batting champlonsh~ps m 1929 and 1932 w~th Phdadelphm and Brooklyn)
Taylor began his college career in 1935 at Yanktown College hopmg to become a mmmg
engineer After a year, he took a job in Fort Peck, Montana He saved his money and subse-
quently entered Stanford University Ray Lyman Wilbur, h~s father's cousin, was president of
Stanford after servmg as Herbert Hoover's Secretary of the Interior At Stanford, Taylor dis-
covered metallurgy which was taught along with mining courses He recewed an A B m engl-
neenng in 1940 and was awarded a Gordon McKay Fellowship m metallurgy and metallog-
raphy at Harvard At Harvard, he learned of a recent graduate, Alexander R Tromno, who
had left to teach at Notre Dame
In 1941, he recewed an S M at Harvard and he moved to Notre Dame to study under
Tromno He recewed his Ph D m 1944, his thes~s toplc was "The Isothermal Transformation
of Austemte " He stayed on as an Instructor and worked part time w~th Bendix Aviation
The sixth edmon of the ASM Metals Handbook was pubhshed m 1939 and repnnted in
1942 and 1944 Although m need of revision, thxs task was deferred dunng the war ASM
began a search for a staffedltor to lead this rewsmn and Trolano recommended Taylor Lyman,
after convincing Taylor that his lack of edltonal experience was overshadowed by his other
quallUes H e j o m e d ASM m the summer of 1945
In 1948, the 7th edition of the Metals Handbook (and perhaps the most popular edition)
was published using a larger page format than p n o r edmons and containing far more infor-
mation (1332 pages. 40% larger than the 6th edition). The 7th edition also contained the first
extensive collecUon of phase d~agrams published in the United States
The 8th edmon of the Metals Handbook was a major change as the single volume work
increased to eleven volumes w~th more than 4600 author-contnbutors Taylor, however, was
stncken w~th illness m the summer of 1972 near the completion of Vol 7 of the 8th edition.
Robert F Mehl, chairman of the volume 7 committees, was also senously ill from dmbetes
F r o m his hospital bed, Taylor rewewed pages and planned Volume 8 He died at Umversity
Hospital m Cleveland on 8 February 1973
Louis Williams McKeehan
(born 31 March 1887 m Mmneapohs, Minnesota, died 31 March 1975)

Louis McKeehan was the second chairman of Sub VI from 1930 to 1933 Originally titled
Sub VI on X-Ray Crystal Analysis, it was changed to Sub VI on X-Ray Methods m 1931 In
1926, McKeehan published m the A S T M Proceedings an extensive glossary of terms relating
to X-ray metallography
McKeehan began his academic career at the U S Naval Academy (1903-1905), then
returned home to the Umverslty of Minnesota receiving a B.S m Engmeenng m 1908, an M S
m 1909 and a Ph.D in physics m 1911. He was a member o f t b e faculty from 1906 to 1919
In 1927, he received an honorary M A from Yale University
He was a physicist with Western Electnc C o , Bell Telephone Laboratones, from 1921 to
1927 where he began his interest in X-ray techniques He then joined Yale Umverslty in 1927
as professor of physics (1927-1955) He was the director of the Sloan Physics Laboratory at
Yale from 1927 to 1941 and from 1946 to 1954 In 1955, he was named professor emeritus
McKeehan received the Legion of Ment and a Mentonous Pubhc Service Award of the U S.
Navy m 1965
Robert Franklin Mehl
(born 30 March 1898 m Lancaster, Pennsylvama, died 29 January 1976)

Bob Mehl orgamzed E4's first symposium m 1936 which became its first specml techmcal
pubhcaUon (STP 28) and was chairman of Sub VI on X-ray methods from 1933 to 1937 He
was a pioneer m the development of gamma-ray radiography for the study o f steel castings. He
received a B.S from Frankhn and Marshall College m 1919 and a Ph D m physical chemistry
from Pnnceton m 1924. He taught chemistry at Jumata College (1923-1925), became a
naUonal research fellow at Harvard Umverstty ( 1925-1927), then supenntendent of the Divi-
sion of Physical Metallurgy, Naval Research Laboratory ( 1927-1931), then assistant director,
Research Laboratories of the American Rolhng Mill Company (Armco, 1931-1932) In 1932,
he joined the Carnegie Institute of Technology as director of the Metals Research Laboratory
and professor of metallurgy
Mehl's interest m chemistry began as a boy when he built a chemical laboratory m the base-
ment of his home He once said "'I scared the daylights out of my m o t h e r - - t o say nothing of
myself" In 1914, when Bob was m high school, he and another student placed uranyl acetate
on top of a key, then placed the key over photographic film, thus producing a radiograph of
the key X-ray radiographs were already well known at that time. Soon after Rontgen discov-
ered X-rays m 1896, Albert Sauveur (a young man in Belgmm at that time) made an X-ray
radiograph of a weldment When Mehi went to the Naval Research Laboratory (NRL), he was
shmulated by a brief Russmn note about the use of gamma rays. Mehl knew that the absorp-
tion coefficient of gamma rays was lower than for X-rays which suggested greater penetrating
power. Also, g a m m a ray sources could be portable whde X-ray generators were not Mehl con-
vmced the Navy m 1928 that thts work was worthwhde and actwe work began in 1929 The
Howard Kelly Hospital m Baltimore had 5 g of radium and regularly pumped offradloactwe
radmm emanation, radon The first gamma-ray radiograph was made m the hospital base-
ment. In this work, Mehl was joined in 1929 by Drs Charles S Barrett and Gdbert Doan In
1930, Roy A. Gezehus, Herman F Kmser, and Charles W. Bnggs joined Radiographs were
made of sections up to 12 5 m thtck, while X-rays were limited to 3 in at that time. The first
"commercial" test of gamma-ray radiography was made later m 1930 on the sternpost casting
on the cruiser "Chester." The radiograph found large hot tears that d~d not come out to the
surface. Naturally, tt was kept m service and the tears propagated to the surface
Mehl was head of the department of metallurgy from 1935 to 1959 and dean of graduate
studLes from 1953 to 1960 From 1960-1966, he was on leave from Carnegie as a consultant
to U S Steel Corp Next, he acted as vtsmng professor at the Umverslty of Delaware and at
Syracuse University. D u n n g World War II, he and his colleagues performed research for the
U.S Army. In 1945, he was an attache with the U S Embassy m London working with the
Techmcal Intelligence Investigating Committee m Germany evaluating their iron and steel
industry He subsequently served on a number of government committees Ship Steel Com-
mmttee, National Research Council (chairman, 1948), the Metallurgy Committee, Research
and Development Board (chairman, 1950), and, the Metallurgical Advisory Board, National
Research Council (chairman, 1951) He also chaired the Commission of Technical Coopera-
tive Administration under President Truman's Point Four Program and was an advisor to the
Atomic Energy Commission Dr Mehl was interested in developing metallurgy outside of the
United States He made a number of trips to Brazil, for example, to stimulate work there In
1944, at the request of Nelson Rockefeller (coordinator o f inter-American affairs at that time),
he organized a lecturing and technical liaison mission to Brazil and helped orgamze Brazil's
first metallurgical society H e a l s o s t u d l e d B r a z i l ' s m e t a l s i n d u s t r y u n d e r t h e U S State Depart-
ment's Point Four program
Meht put together an illustrious staff at the Metals Research Laboratory of the Carnegie
Instmtute of Technology consisting initially of Charles S Barrett, Maxwell Gensamer, Cyril
Wells, Frederick N Rhlnes, and Gerhard Derge Mehl and these five colleagues had a major
influence on the establishment and development of the field of physical metallurgy He pub-
lished over 200 papers He enjoyed oil painting and tennis as hobbles Mehl mentioned that
on one ofhms traps to Brazil, "the reporters asked me what I liked to do mnmy spare time I told
them I paint and used to play tennis So they wrote 'Dr Mehl is the best known amateur artmst
in the United States, and he msa tennis champion He would like very much to meet some of
the Brazihan c h a m p i o n s ' "
Mehl presented fifteen honorary lectures and received thirteen medals and numerous
awards, for example, election to the National Academy of Sciences ( 1958), fellow of the Amer-
ican Institute of Mining, Metallurgical, and Petroleum Engineers (AIME) (1964), honorary
member of the Iron and Steel Institute (UK) in 1969, the John Scott Medal, certificate and
prize from the Dmrectors of the Board of City Trustees, City of Philadelphia, for development
of gamma-ray radiography (1934), the Henry Marion Howe Medal of the American Society
for Metals (ASM) (1939), the James Douglas Gold Medal o f A I M E (1945), the Gold Medal of
ASM (1952), the LeChateher Medal of the Soci&6 Franqalse de M&allurgle (1956), the Plat-
m u m Medal of the Institute of Metals (1962), and six honorary degrees Two awards have been
named after him The Society of Nondestructive Testing established the Mehl Honor Lecture
at its first meeting, 17 October 194 l, with Charles W Briggs as recipient Mehl was the recip-
ient of this award on 18 October 1971 but gave his lecture by tape, "in absentia," due to ampu-
tation of both of his legs, as a result o f diabetes
George Andrew Moore
(born 14 February 1913 in New York, New York)

George Moore, although never an officer or subcommittee chairman, was an active E4
member for about 30 years He was a tireless worker on Sub 14, particularly in the areas of
volume fractmon, grain size, and inclusion measurement In 1960, at the suggestion of LeRoy
Wyman, he started work on the storing, manipulating, and measuring of microstructural

images with a digital computer His subsequent report on the potential for computerized quan-
titative microscopy stimulated creation of Sub 14 George was also quite active in the devel-
opment of improved A247 graphite charts and wrote several classic papers in STPs
George was trained as a chemist and metallurgast receiving a B.S degree in chemistry from
Union College in 1934, an M S in metallurgy from Harvard in 1935, and a Ph D from Prince-
ton in 1939 in chemistry and metallurgy While at Princeton, he was an assistant instructor
from 1935-1939, then an instructor until 1940 At that time, he joined the Battelle Memorial
Institute as a research engineer where he was involved with work on hydrogen in steel and in
fractography, using the light microscope, with Carl Zappfe In 1948, he joined the University
of Pennsylvania as an associate professor of metallurgy In 195 l, he joined the National
Bureau of Standards where he performed his work in quantitative metallography He retired
in 1979 He was a lecturer at the University of Maryland from 1954 to 1962. He was also a
long-time member of the International Society for Stereology and chaired its Fourth Inter-
national Congress for Stereology in 1975. Thoroughness was a hallmark of George Moore's
work He was a total purist in all his endeavors
Mary Rose Norton
(born in June 1905 in Cambridge, Massachusetts, died 30 January 1974)

Mary Norton served as secretary of E4 from 1946 to 1966 and as chairman of Sub II on
Definitions from 1966 until her death in 1974 Mary attended Emmanuel College in Boston
and received an A.B in chemistry and mathematics in 1926 Next, she enrolled in Columbia
University and received an A M in chemistry in 1928 Before, during and after her graduate
studies, she worked in the research laboratory of the Merrlmac Chemical C o , North Woburn,
Massachusetts Mary's entrance into the ordnance field and metallography is an interesting
story
General T C Dlckson, commanding officer of the Watertown Arsenal in 1928 was
intrigued by the work of Francis F Lucas of the Bell Telephone Laboratories, a consultant to
the Arsenal General Dlckson wanted to establish a similar high-resolution light microscopy
laboratory at the Arsenal to investigate ordnance steels He ordered that the new facility should
duplicate that of Dr Lucas, even to having a woman assistant whose background was soence)
Arsenal personnel called local colleges and recruited Mary as the woman assistant Mary
enrolled in metallurgy courses at both Harvard and Massachusetts Institute of Technology
(MIT), particularly with professors Robert Wllhams and Arthur Homerberg at MIT
Mary learned her craft well receiving numerous commendations for her work Other orga-
nizations requested her help, for example, the U S. Geological Survey, the U S Navy Bureau
of Ships, Harvard Observatory, independent test laboratories, and industrial companies such
as Republic Steel The Arsenal purchased a Zelss Neophot metallograph in 1935 Mary loved
to use its 1 60 NA (numerical aperture) oil-immersion objective for high magnification stud-
les Mary quickly discovered that even the best microscope was useless if the specimens were
not polished properly and she devoted her energies toward mastering this necessary skill This
interest led her to study surface finishing techniques During World W a r II, she developed,
prepared and cahbrated standards for ordnance finishes used for quality control In 1942, she
was assigned leadership of the Metallurgical Structures Section in the Physical Metallurgy
branch In this position, she contributed to the knowledge of how to best utlhze high strength
steels and did notable work on temper embrittlement
Mary received the War Department's Meritorious Civilian Service Award in 1945 The
ASTM Award of Merit was bestowed in 1959, and she was named honorary secretary in 1966
In 1974, Committee E4 established, with the help of many of her friends, the Mary R Norton
Memorial Scholarship Fund for women studying metallurgy
Robert Earl Penrod
(born 22 July 1887 in Johnstown, Pennsylvania, died 11 September 1971)

Earl Penrod served as vice chairman o f E4 (1944 to 1964) and as chairman of Sub VIII on
Gram Size (1952-1964), replacing Marc Grossmann after his death. He took over the work of
unifying E4 grain size methods into one standard, E 112, issued in 1955
Penrod joined the Cambria Iron Works on 1 September 1902 at age fifteen This plant was
acqmred by Bethlehem Steel and became their Johnstown Plant Penrod did not attend col-
lege, he did attend summer courses on metallography with Albert Sauveur He worked his way
up to chief metallurgist in 1927 and held that position until his retirement on 31 August 1955
after 53 years
Penrod was active in the Johnstown community, as a member of the industrial council of
the Greater Johnstown Chamber of Commerce and as the chief fund raiser for the Johnstown
Symphony Orchestra He received the ASTM Award of Merit in 1957 and was named hon-
orary vice chairman of E4 m 1964
George Edward Pellissier
(born 15 March 1915 m Spnngfield, Massachusetts, died 24 June 1982)

George Pelhssler was the first chairman of Sub XI ( 1950-1951 ) and Sub XIV ( 1961-1964)
He chaired Sub 11 again from 1969 to 1973 George was also achve with E24 on Fracture
Testing of Metals, where he chaired Sub 1 (on High-Strength Metals) from 1965 to 1969 and
was the founder and first chmrman of Sub 2 (on Fractography) from 1963 to 1965 George
recewed B.A and M A degrees m chemistry from Cornell Umverslty m 1936 and 1938,
respecUvely, He started doctoral work at Carnegie InsUtute of Technology m Metallurgy m
1938, but this work was interrupted in 1941 by World War II
From 1942 to 1945, he was group leader for Manhattan Project work performed at Colum-
bm Umversity He apphed transm~ssion electron microscopy to the determination of
extremely fine pore sizes m gaseous isotope diffusion separation barriers under development
and to the study o f " d u s t " plugging problems This work was performed using one of the first
commercially available electron microscopes m the United States
After the war, George joined the Apphed Research Laboratory of the U S Steel Corp as a
research associate. In 1947, he was named section head, physics and analytical chemistry, then
division chief m 1955 In 1959, he was manager, advanced applied research In 1966, he
became senior consultant m physical metallurgy until he retired m 1968
George continued his interests m electron m~croscopy when he joined U S Steel developing
rephcat~on methods, the only approach for studying fine structure at that time He also worked
on developing the extraction replica techmque as an offshoot of the X-ray reflecUon-dlffrac-
tion concentration technique He uUhzed these methods m h~s efforts to develop tougher, high-
and ultrahigh-strength steels
Pelhssier became interested m electron fractography in 1962 when he began to study frac-
ture modes and mechamsms of h~gh-strength alloys He used one of the first prototype scan-
nmg electron microscopes for fractographlc work
After retirement, George became laboratory manager for Ernest F Fullam, I n c , Schenec-
tady, New York, a major supplier of electron metallograph~c eqmpment He continued m this
role until 1971 when he joined RRC International, Inc as department manager He main-
tamed this association until shortly before his death m 1982
George pubhshed over twenty-five papers, including his classic work on "The Interlamellar
Spacing of Pearhte" (Transactions, ASM, December 1942) He held four patents Three are
on methods of measunng coating thicknesses He was a fellow of the American InsUtute of
Chemists and a fellow of the American Society for Metals (ASM) He was a charter member
of the Electron Microscope Society of America and of the International Metallographic Soci-
ety In 1961, he was a member of an inspection tour of metallurgical research msututes in the
Soviet Union, sponsored by the Electrochemical Society and the U S State Department In
1970, he gave the Albert Sauveur memorial lecture for the Philadelphia Chapter of ASM
a
Arthur Phillips
(born 3 February 1892 in Troy, New York, died 25 December 1977)

Arthur Phillips was chairman of Sub II on Terminology from 1925 to 1938 Phillips
attended public school in New Haven, Connecticut and graduated from Hlllhouse High
School Phillips received a bachelor of phdosophy degree from the Sheffield Scientific School
o f Yale University, graduating summa cum laude. Continuing at Yale, he received his M S
in metallurgy in 1915--he was the first person to receive an M.S in metallurgy from Yale
Phllhps joined the Bridgeport Brass C o , but four years later returned to Yale as an assistant
professor (1919-1928) He advanced to assooate professor (1928-1934), then professor
(1934-1959) and emeritus professor in 1959 F r o m 1950 to 1959, he was head of the depart-
ment of metallurgy.
He was a student of Champion H Mathewson Their paper "The Recrystalhzation of Cold-
Worked Alpha Brass on Annealing" (Transactions, AIME, Vol. 54, 1917) had a major impact
on the understanding ofrecrystalhzatlon In 1942, with Robert M Brick, he published the well
known text Structure and Properties of Alloys (McGraw-Hall Book Co ) This book was built
upon lectures by Mathewson, instructor o f both Phillips and Brick.
When Phllhps was working on the recrystalhzatlon of brass m the 1920s, there were few
sources of graded abrasives for pohshlng. The metallurgy department was located m the Ham-
m o n d Laboratory at that time. This was a large, open building on the inside, several stones
high and equipped with gnnding equipment The dust from grinding would settle on the walls
as there was no exhaust or dust collection system at that time. Phillips would climb up a ladder
to different levels and brush the dust into coin envelopes. The higher he went, the finer the
dust. Much of the dust was iron oxide. Hence, he utilized gravity to grade the iron oxide by
s~ze, that is, height above the floor!
In 1944, Phdhps gave a series of lectures at the University of Sap Paulo, Brazil and received
an honorary Ph D from them, and also from the Stevens Institute of Technology in the same
year He was an active consultant, particularly for the Henry D Thompson C o , manufacturer
of saw blades At the time o f his death, he was a director ofth~s company
Samuel Moreau Purdy
(born 27 May 1926 in Bethlehem, Pennsylvania)

Sam, current First Vice Chairman of E4, has had a long association with Sub 1 as its chair-
man from 1966 to 1982 and from 1986 to the present From 1983 to 1988, he was chairman
of Sub 5 on MlCrOlndentation Hardness and from 1968 to 1972, he chaired Sub 14 on Quan-
titative Metallography Sam has left his l m p n n t on many ASM standards, such as E 3, E 340,
and E 381 The most recent is E 1351 on the production and evaluation of replicas made in
the field to evaluate creep damage in electric power plant components, which began life as an
emergency standard, ES 12-87, E4's only emergency standard He also was our representative
to the International Standardization Organization from 1977-1981
Sam, a descendant of early English colonial settlers around Manhattan, received a B S in
metallurgical englneenng from Lehigh University in 1948 Following graduation, he joined
Carpenter Steel Company, starting as a hot mill observer He transferred to their research
department and became supervisor of stainless steel development, then supervisor of physical
metallurgy In 1962, he joined Youngstown Sheet and Tube as supervisor of the metallo-
graphic laboratories, a position he held until their demise in 1979 He then joined Jones and
Laughlin Steel as a senior research engineer and in June 1980, joined National Steel Corp as
senior research engineer, later senior research associate, his current position He is an avid
reader (British history and French revolution) and gardener--he usually grows twelve varieties
of Mexican and Oriental peppers!
Henry S. Rawdon
(born 7 June 1880 in Derby, England, died 14 May 1954)

Henry Rawdon was the first chairman of Sub V (on "Micro-Hardness") and was chairman
of Sub IV on Photography from 1922 to 1934 Sub V was established in 1923 to evaluate the
Blerbaum micro-character tester, a scratch indentation tester performed with the aid of an
upright microscope with a scratch indenter The work concluded that it was of comparative
use only and the Sub was disbanded in 1926
Henry came to America when he was four years old His family settled in Michigan with
relatives on a farm in a small village Educated in the ungraded district schools, he studied at
home and passed the examination for country teacher when he was 17, the m l m m u m age for
such lobs However, it was difficult to get a position, so he entered the Michigan State Normal
College in Ypsllantl He worked his way through school and graduated in 1903 with a life
certificate in teaching For the next six years, he taught high school at Marlette, M i c h i g a n - -
for the first three years, he taught soence and for the last three years, he was superintendent
He decided to make chemistry his career and, in 1909, entered the englneenng college of
the University of Michigan Metallurgy courses were being introduced into the chemical engl-
neenng program and Henry's interest in metals was fostered by these courses and by Professor
Edward DeMflle Campbell, the famous blind metallurgist Rawdon acted as his personal assis-
tant dunng his senior year. In 1912, he received a B Ch E and started to do graduate studies
when he was recruited by the new division of metallurgy at the U S Bureau of Standards to
work in metallography as an assistant physicist
Rawdon spent his entire career at the Bureau becoming Chief of the division of metallurgy
m 1929, a position he held until he retired in 1945 Henry attributed his interest in metallog-
raphy and the structure of metals to his earlier training in biology with the transmitted light
microscope He had an abiding interest m studying structure-property relationships He was
also fascinated by corrosion mechanisms, problems, and solutions His book, Protective
Metallic Coatings, published in 1928 by the American Chemical Society, was a pioneering
effort m this field He had 88 publications He served on the Metallurgy Advisory Board of the
Ordnance Department for the National Advisory Committee for Aeronautics and for the
National Academy of Sciences During World War II, he was on advisory committees to the
Army and Navy Munitions Board, Office of Production Management, War Production Board
Frederick Nims Rhines
(born 25 July 1907 in Toledo, Ohio, died 10 Apnl 1986)

Fred Rhlnes was one of the phase diagram experts recruited by Paul Beck to help develop
standard nomenclature and presentation procedures leading to E 157 and E 391 He mare-
tamed this interest with E4 for more than thirty years Fred was more active on B9 on Metal
Powders and Metal Powder Products, than on E4 He,loined B9 in 1944 and E4 in 1949 He
chaired B09 01 on Nomenclature and Technical Data from 1944 to 1965 He also contributed
substantially to the development of a "Glossary of Terms for Powder Metallurgy" and to many
other projects He received the Award of Ment in 1962 He was also a member of the former
E8 committee
Fred received a B S.E. from the University of Michigan in 1929 He worked as a metallurgist
m the Research Laboratories of Alcoa from 1929 to 1931 In the summer of 1932, he studied
at the University of Berlin and received a language certificate In 1933, he received a Ph D
from Yale University He was a laboratory instructor at Yale from 1933-1934, then joined
Robert F Mehl at Carnegie Institute of Technology as a member of the staff of the metals
research laboratory and the metallurgical engineering faculty From 1946 to 1959, he was
Alcoa professor of light metals at Carnegie Institute of Technology
In 1959, Rhines left Carnegie and headed south where he established the department of
materials soence and materials engineering at the Umverslty of Florida (Gainesville). Fred was
professor of metallurgy and materials engineering and head of the metals research laboratory
engineering industrial experiment station from 1959 to 1973 He was chairman of this depart-
ment from 1963 to 1973, then became distinguished service professor He retired in 1978.
Fred received the C H Mathewson American Institute of Mining, Metallurgical, and Petro-
leum Engineers best paper awards in 1939 and 1942 He received the Henry Marion Howe
Medal of American Society for Metals (ASM) in 1947 and 1960 and the Albert Easton White
Dlstmgmshed Teacher Award of ASM m 1970 In 1970, he received the Willis R Whitney
Award from the National AssocmUon of Corrosion Engineers He was a fellow of ASM,
ASTM, and AIME He also conducted excellent pioneering studies m quantitative microscopy
and was coeditor with Robert T. DeHoff, of the book Quantitative Microscopy (McGraw-Hill,
1968) His classic 1956 text, Phase Diagrams in Metallurgy (McGraw-Hill Book Co ), was
used by colleges for many years
William Ernst Ruder
(born 22 December 1886 in Stockdale, Pennsylvania, died 10 February 1963)

Bill Ruder was chairman of Sub III on Thermal Analysis from 1924 to 1928 After gradu-
ation from the Pennsylvania State College in 1907 with a B S. in electrical engineering, he
joined the General Electric Research Laboratory (10 July 1907) He had earlier received a
teacher's certificate after studying at the state teacher's college in California, Pennsylvania, He
spent his entire career with General Electric, retlnng in 1952 as manager of the metallurgy
department of their Research Laboratory He was well known for his research on magnetic
alloys, both soft and hard
His first patent, issued in 1914, covered the manufacture and processing ofslhcon electrical
sheet steel This work led to improved efficiency and lower electric costs His work on the rate
of grain growth, with Zay Jeffrles, helped to demonstrate the importance of a large grain size
for high temperature applications He helped develop methods for obtaining large grain sizes
and was one of the first to demonstrate the importance of crystal orientation in reducing mag-
netic hysteresis losses Later, he devoted attention to work on permanent magnets In 1934,
he received his first patent for Alnico-type permanent magnet materials In the United States
Ruder was known as the father of the Alnico magnet His initial research on these materials
occurred at the same time as Mlshima of Japan
In 1938, he was named head of the Metallurgy Department For seventeen years, beginning
in 1933, he was a director of the Allegheny Ludlum Steel Corporation, a manufacturer of mag-
netic materials He served as a member of their executive committee and their research advi-
sory council He held 19 patents by the end of his career
John James Brown Rutherford
(born 26 August 1908 m Hamilton, Scotland, died 19 March 1967)

Rutherford was the primary author of an important early paper (Metals andAlloys, Vol 8,
Dec 1937, pp 345-348) on the correlation between planar and spatial gram size Conse-
quently, he was a long-term participant in E4's grain size standards work, although he never
chawed Sub VIII He did organize Sub X on Decarbunzation and was its first, and only, chair-
man ( 1949 to 1953) This sub worked with the Society of Automotive Engineers and the Amer-
ican Iron and Steel Institute on decarburlzatlon measurement Rutherford was actually more
active on other ASTM committees than on E4 He was a member of A l, A 10, E7, E9, and
several other ASTM activities
John began his academic training at Her~ot-Watt College in Edinburgh, Scotland He came
to the United States in 1928 as an exchange student before fimshlng his degree Instead of
returning and finishing his studies, he joined the American Chain and Cable Co in Bridgeport,
Connecticut working as a research metallurgist under A V deForest He pursued further stud-
les at New York University and at Columbia University but never did complete his degree
requirements In 1929, he joined U S Steel's Research Laboratory in Kearney, New Jersey
He helped E S Davenport with his isothermal transformation studies of steel He also did
some pioneering work on the lntergranular corrosion of austenltlC stainless steels w~th R H
Aborn On 20 June 1938, he joined the Babcock and Wilcox Company an Beaver Falls, Penn-
sylvania, as a research metallurgist At the time of his death, he was chief metallurgist He held
a number of patents on the processing of stainless steels In 1957, he gave the 24th Annual
Sauveur Lecture of the Phdadelphla Chapter of the American Society tbr Metals
John was a descendant of Jean Armour who married the Scottish poet Robert Burns ("Auld
Lang Syne") in 1788 John spoke Gaelic and was a frequent speaker at Bobby Burns Clubs on
the anniversaries of the poet's birth He was an avid golfer and gardener
Carl Hubert Samans
(born 27 January 1909 in Greenville, Pennsylvania, died 22 March 1981)

Carl Samans was not an officer or subcommittee chairman of E4 In 1937, when Marcus
Grossman took over the Special Subcommittee on Grain Characteristics (which became Sub
VIII on Grain Size in 1938), Grossman established three groups (now called task groups) to
work on specific aspects of gram size analysis Group C was set up to develop methods for
nonferrous alloys other than copper Group C was headed by Carl until 1951 when H P
George took over Standard E 9 l, issued in 195 l, resulted from this work
Samans received a bachelor's in chemical engineering from Rensselaer Polytechnic Institute
in 1929 He then joined the research laboratory of Chase Brass and Copper Co and obtained
his M S (1932) and Ph D (1934) in metallurgy from Yale University while with Chase He
then joined Lehigh University as an instructor in metallurgy (1934-1935), then taught at
Rensselaer Polytechnic Institute (1935-1937) while acting as a consulting physicist for the
International Nickel Co In 1937 he joined the metallurgy faculty at Penn State.
Samans returned to industry In 1941 joining the American Optical C o , moving up to chief
of the metallurgical section of their Research Department In 1949 he joined Standard Oll Co
(Indiana) as associate director, engineering research In 1960, he became director of this
department
Samans was president of the American Society for Metals (1968-1969) after previous terms
as a trustee ( 1959-196 l) and as secretary ( 1964-1966) Samans authored two books Engi-
neering Metals and their Alloys and Metallic Materials in Engineering.
Ernest Edgar Thum
(born 20 November 1884 at Hamsonvllle, Missouri, died 10 April 1961)

Ernle was never an officer or subcommittee chairman o r E 4 but he was active with E4 and
ASTM from 1924 until his death in 1961 He was also a member of Committees A 1 on Steel,
B2 on Non-Ferrous Metals and Alloys, E5 on F~re Tests of Material and Construction, B6 on

Die-Cast Metals and Alloys, B9 on Metal Powders and Metal Powder Products, and was E4's
representative to E 1 on Methods of Testing (at that t~me) He was most active with B2 where
he served as secretary (1928-1939), chawman (1939-1948), and honorary vice chairman
( 1948 until death m 1961) He recewed the Award of Merit m 1954, mainly for his B2 work
Erme recewed a bachelor's degree in m m m g engineering from the Colorado School of Mines
m 1906 He joined the Anaconda Copper Mmmg Co as a field engineer after graduation.
From 1908-1910, he was chief clwl engineer for the constructmn of the Tooele Smelter of the
International Smelting and Refining Co. m Utah In 1910 he became engineer in charge of
construction of The Great Falls (Montana) Smelter of the Anaconda Copper Mining Co. He
switched career paths at this ume, 1915, when he joined the University of Cincinnati as pro-
fessor of metallurgy
In 1917, Erme again changed his career path becoming associate editor of Metallurgicaland
Chemical Engineering, a popular monthly trade journal published by McGraw-Hill From
1924-1927 he managed the technical pubhclty department of the Union Carbide and Carbon
Corporation He returned to pubhshmg m 1928 as pnnclpal associate editor of The Iron Age.
In 1930, he joined the American Society for Metals (ASM) as the founding editor of Metal
Progress. In 1947, he took on the task of superwsing book pubhshmg for ASM During his
tenure as editor m chief of Metal Progress, ~t was widely recogmzed as one of the premier
metallurgical journals He also pubhshed a number of books, such as The Book of Stainless
Steels and Modern Steels.
Erme recewed numerous awards for his work He received a Dlstmgmshed Service Award
from ASM m 1948 and was made an Honorary Member m 1958 His alma mater gave him
their Silver Medal m 1951
Clarence Jory Tobin
(born 29 May 1896 m Calumet, Michigan, died 4 March 1978)

Clarence "Tobe" Tobin, a long time E4 member, was the chairman of the Special Com-
mittee on Grain Characteristics from its formation in 1931 until 1937 This committee's first
goal was to develop a procedure for evaluating the grain growth tendency of steels The
McQuald-Ehn carburlzing test was subsequently adopted and standard E 19 incorporated the
method A grain size chart depicting the hypoeutecto~d and hypereutectold regions for grain
sizes 1 to 8 was Included in the lmtlal version orE 19 (a second chart was added in 1939) Tobe
was also an active member of Committee B2 on Non-Ferrous Metals and Alloys
Tobe received a B S in chemical engmeenng from the University of Michigan in February
of 1920 He then joined the Dodge Brothers, Inc as a metallurgical troubleman and metal-
Iographer In March of 1925, he joined the General Motors Central Laboratories (now the G M
Research Laboratones) as a metallurgist In 1933 he became assistant department head of the

metallurgy department, a position he held until his retirement on 1 June 1961 He was noted
for his contributions in the field of gear metallurgy, automotive component failure analysis,
and metallographlc methods His 1938 paper (Transactions, ASM, Vol 26), co-author with
A. L. Boegehold, on "Factors Governing Selection of Type of Carbunzed Case" was consid-
ered a classic paper on this subject He had two U S patents on brake drums
Tobe was also quite active with the A m e n c a n Society for Metals (ASM), particularly in the
Detroit Chapter where he was its chairman In 1932 He was elected a Fellow of ASM in 1974
and was a fifty-year member
Jose ("Joseph") Ramon Vilella
(born 11 August 1897 in Lares, Puerto Rico, died 27 November 1971)

Joe Vllella, perhaps the best-known metaliographer in his day, was chairman of Sub I from
1947 to 1951 An active E4 member for many years, he also was involved with the ASTM
photographic exhibit He was also a member of Committee El
Vilella's studies at Pennsylvania State College (now Pennsylvania State University) were
interrupted by service dunng W W I with the U S Army as a second lieutenant ( 1917-1918)
He returned and graduated from Penn State in June 1921 with a B.S in chemistry He then
worked as a physiological chemist for two years at the Psychiatnc Institute in Mornstown,
New Jersey In 1923, he joined the Union Carbide Research Laboratory as a microscopist/
metallographer
Vilella married Eve Edwards, a noted fashion model in 1930 Several years later, Union
Carbide decided they wanted to move their research laboratory (in Long Island City) away
from the New York City area to Nmgara Falls Because of Eve's career (Joe was a modern
man), Joe decided to change career paths On 1 May, 1934, hejolned the U S Steel Research
Lab, then in Kearny, New Jersey, as a senior scientist In 1956, when U S Steel moved this
lab (Fundamental Research Lab) to Monroeville, Pennsylvania, Eve had "retired" and the
Vilellas moved to Pittsburgh Bill Forging, Sr replaced Vilella at Union Carbide
Joe retired from U S Steel on 31 August 1962 a n d j o m e d the metallurgy facility of the Uni-
versity of Pittsburgh on the following day as an adjunct professor Vllelta had taught at Rutgers
Umversity during his last year with Union Carbide, 1933-1934 Joe taught at the University
of Pittsburgh for six years between September 1962 and his second retirement m July 1971
Joe is best known, especially today, as a ferrous metallographer and for his development of
"Vilella's reagent," an alcoholic mixture of picnc acid and hydrochloric acid However, Joe
began his career as a nonferrous man, he even coauthored a book on aluminum Aside from
the well known Vilella's microetch for steels, there are at least five other reagents also known
as "Vilella's reagent" used for microetchlng aluminum and alloys, copper-lead alloys, lead and
alloys, tin and dilute tin-lead alloys, and for macroetchlng high alloy steels)
Joe had one U S patent (for a levlgated alumina for polishing) and thirty-four pubhcatlons
In 1937, he gave a series of education lectures for the American Sooety for Metals which were
pubhshed in 1938 in book form as Metallographie Technique for Steel. In 1951, he gave the
Henry Marion Howe Memorial Lecture for the American Institute of Mining, Metallurgical,
and Petroleum Engineers
In September 1972, the ASTM board approved the creatmn of the Vdella award of E4.
This award recognizes papers published by ASTM that are of outstanding significance to
metallography
Robert Seaton Williams
(born 11 July 1880 in Hartford, Connecticut, died 11 December 1961)

Robert Wllhams was chairman of Sub II from 1938 to 1940 and a long time ASTM member
He received an S B degree in 1902 from the Massachusetts Institute of Technology (MIT) and
was an assistant m analytical chemistry at MIT beginning in the fall of 1902 until he began
graduate school in 1905 at the University of Gottlngen where he studied under Gustav Tam-
man and received his Ph D in 1907 He returned to MIT in 1907 as an instructor in the chem-
istry department He was named assistant professor in 1911 and associate professor in 1917
In 1921 he was named associate professor of chemistry and metallography, and, in 1926, pro-
fessor of physical metallurgy He was head of the metallurgy department at MIT from 1937 to
1946 and dean ofenglneenng from 1942-1945 He retired in 1946 but continued as a lecturer
untd 1951
During W W I, Dr Williams worked on problems with shell cases and conducted research
with Alcoa on bearing metals for aircraft and tanks At MIT, he was a mare force m developing
courses in metallography, heat treatment, spectroscopic analys~s, and X-rays Dunng W W II,
he was revolved with studies on berylhum and its use in aluminum alloys He also served as
technical advisor to the Division of Research and Development m the Quartermaster Gener-
al's Department where he worked on problems with mdltary equipment
With V O Homerberg, he authored Principles ofMetallography m 1919 The fifth edmon
of this very popular book was issued in 1948 He also coauthored The Examination of Iron,
Steel and Brass m 1924 and translated two books pubhshed originally in German
Acknowledgments
Arthur Phdhps--Courtesy o f the Yale Picture Collection, Manuscripts and Archives, Yale
University Library
Charles H Davis--Courtesy of Manuscripts and Archives, Yale University Library
L W M c K e e h a n - - C o u r t e s y of Manuscripts and Archives, Yale University Library
Leon V Foster--Courtesy of Syracuse University Library
F F Lucas--Courtesy of AT & T Archives

Henry M Howe--Courtesy of Columbia University
W Campbell--Courtesy of Columbia Umverslty
George A Elhnger--Courtesy of The National Institute of Standards and Technology
Henry S Rawdon--Courtesy of The National Institute of Standards and Technology
LeRoy L Wyman, Sr --Courtesy of The National Institute of Standards and Technology
R S Williams--Courtesy of the MIT Museum
Edgar H Dlx--Courtesy of the Cornell Umverslty Library
H C Boynton--Courtesy of the Harvard University Archives
Light Microscopy
Theodore G. R o c h o w I
Some Incidental History of Metallography and

ASTM Committee E4
REFERENCE: Rochow, T G , "Some Incidental History of Metailography and ASTM Com-
mittee E4," Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP
1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, American Society
for Testing and Matenals, Philadelphia, 1993, pp 83-87
ABSTRACT: Pioneenng investigations were by Sorby (1826-1908) at Sheffield, England, fol-

lowed by other European metallurgists at the turn of the century "Dean" of Amencan metal-
lurg~stswas Professor Sauveur at Harvard He designed the Sauveur metallograph~cmicroscope
and named the investigated area, "metallography "As Professor of Metallurgy at Sheffield Um-
verslty and F~sher lecturer at Cornell, 1931-1932, Cecd H Desch called attentmn to the coop-
eratmn of umversmes, lndustnes, and governments m research and development m soence and
engineering ASTM, m general, and Committee E4, m pamcular, added consensus of standards
of nomenclature, testing, instruments, procedures and evaluatmns
The modental wews m this paper s~mplysupplement the up-to-date scholarly h~stoncalreview
by the present chmrman of ASTM Committee E4 on Metallography, George F Vander Voort
KEY WORDS. metallography, metallurgical specimens, mlcrostructure, metallographlc tech-

niques, history, standards, testing, nomenclature, instruments
Origin of Metallography
When ASTM Committee E4 was estabhshed m 1916 (see the complete historical review in
Ref 1), the principles of metallography were based on the pioneering microscopical investi-
gations of Henry Clifton Sorby ( 1826-1908) He was the son of the owners of the famous Shef-
field iron and steel works in England He could afford to spend his long hfe as a truly amateur
microscopist, purposely looking through up-to-date microscopes by current techniques,
answering his own questions, such as What makes a good or a bad iron ore, limestone, smelter,
or heat treatment? He saw variations in both structure and morphology Above all, he thought
about the "mechanism" that brought about the resultant physzcal and chemical changes He
taught himself to prepare specimens, vary modes of illumination, and think through to con-
cluslons [2] He published effectively [3] and taught others He was not an ordained scientist,
but was a close associate of the University of Sheffield, where his portrait (Fig l) and some of
his preparations of metalhc speomens are now on display [4]
Professor A Martens added much (1892) [5] to Sorby's methods as did F Osmond (1892)
[6], C T Heycock and F. H Neville (1904) [7], and many others at the turn of the century
Albert Sauveur (1863-1939), who coined the terms "metallography" and its denvauves,
was an ordained scientist At Harvard University, he investigated, taught, and wrote about
"The Mlcrostructure of Steel and the Current Theories of Hardening" in 1895 [8, 9] He used
the term "metallographlst" in 1898 While instructor in Metallurgy at Harvard, he designed
Associate Professor, Ementus, N C State University at Raleigh, home address 740 Smallwood Dnve,
#33, Ralogh, NC 27605
83
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
FIG 1--Henry Chflon Sorby (1826-1908) Photograph of the portratt that ts hangmg m Ftrth Hall at
the Umverstty of SheJfield (taken by the author, July 1965)
the Sauveur metallographlc microscope in 1899 He was made a full professor m 1924 and
professor ementus in 1939 [8] His book, The Metallography and Heat Treatment of Steel,
was published by the Harvard Umverslty Press m 1935 [10] (see Fig 2 [8]
Cambridge, Massachusetts, m the 1930s, was also a busy center for the mechamcal pohshmg
and microscopical examination of ore minerals and such, by means of the Graton-Vanderwllt
type of"mechanical" grinding and pohshmg machine It was developed ongmally for Profes-
sor L C Graton of the Laboratory of Economic Geology at Harvard Umvers~ty by Vanderwilt
and produced by the Mann Instrument Company (MICO) in Cambndge [11] This type of
pohshmg machine was designed to keep hard and soft mineral constituents In the same pol-
ished plane by using successive metal (lead) laps embedded with abrasive grains or pohshing
powder [ 12] An example may be tiny particles of gold in a quartz matrix By the same token,
a larger boundary is maintained between two large parts, such as galena contacting pynte
Starting m 1935 at the Experimental Laboratory of the American Cyanamid C o , the present
author and associates used the Graton-Vanderwilt type of mechamcal pohshIng machine to
pohsh thin layers of steel on soft ~ron cores that had been case hardened with calcmm cyamde
made from calcmm cyanamlde The Graton-Vanderwxlt automatic pohshmg machines have
been proven valuable to maintain such hard and soft constituents within a reasonable level
The same ~s true for composites containing metal, resin or rubber, or both (such as automobile
Ures), or adhesives for aluminum sheets [13]
Metallography came to Cornell via Emil M o n n m Chamot (1868-1950) (Fig 3), who, dur-
ing the first quarter of this century, developed the course in Chemical Microscopy that became
one of those reqmred for the Bachelor of Chemistry degree Among Chamot's graduate stu-
dents was Clyde Walter Mason (1893-1983) (Fig 4) He later collaborated with Chamot in
ROCHOW ON HISTORY OF ASTM COMMITTEE E4 ON METALLOGRAPHY 85
FIG 2--Albert Sauveur (1863-1939) The dean o[ Amertcan metallurgists named his textbook, Met-
allography Heat Treatment of Iron and Steel, and developed the Sauveur mwroscope for opaque
speumens
FIG 3--Emtl Monnm Chamot (1868-1950) Duphcates of this" photograph were autographed by Pro-
/es sor Chamot and ~ent to/ormer students and other frlend~
FIG 4--Clyde Walter MaJon (1893-1983). on the occaston of one ofhls lectures to the New York Mtcro-
~optcal So~tety. 3 Aprtl 1964
their famous Handbook o f Chemtcal Microscopy [14] Mason introduced the chapter on
"Metallographlc Microscopes."
In 1934, Professor Mason's two laboratory assistants were the present author and Wflham
D Forgeng (1909-1986) who majored in metallography for his Ph D His thesis was "The
Effect of Bxsmuth on the Mlcrostructure of Tin " H e joined the U m o n Carbide Research Lab-
oratones as a metallographer, became Senior Research Fellow in 1968, and retired in 1973
He joined ASTM and Committee E4 in 1940 and was chairman between 1968 and 1972
Metallography at Cornell Umverslty received a b~g boost from the Professor of Metallurgy,
Cecil H Desch of Sheffield University, as nonresident Lecturer (1931-1932) at Cornell, under
the George Fisher Baker Foundation In his lectures, Dr Desch frequently referred to Sorby's
use of the microscope m the study of the structure of iron and steel, pursued purely as science
But Dr Desch also pointed up that this information was quickly applied by industry to
improve products and to invent new ones He also referred to some large mdustnal research
laboratories in the Umted States where both pure and apphed sciences were researched [15]
In February, 1932, Professor Desch became Supenntendent of the Metallurgical Department
of the National Physical Laboratory in England [16]
ASTM Committee E4 on Metallography is a key example of the cooperation among indus-
trial corporations, universities, scientists, engineers, and specmhsts One such industry is the
ROCHOW ON HISTORY OF ASTM COMMITTEE E4 ON METALLOGRAPHY 87
General Electric Company, and the metallographer around 1938 was Leroy L Wyman, Sr,
who later transferred to the U S Bureau of Standards He was chmrman of Committee E4
from 1938 to 1966, 28 yearsl By 1950 he already had won the ASTM Award of Ment for &s-
tmgulshed serwce "to the cause of voluntary standar&zat~on" H~s serwce to ASTM contin-
ued to grow, and m 1967 he was elected an Honorary Member for h~s "specmlly meritorious
service to the Society [17] " N o t that he did not have expert help The secretary of Committee
E4 for 20 years was Mary R Norton, for whom the Memorial Scholarship Award for Women
is named And there was Joseph R Vdella, of the U n i o n Carbide Corporation and Umted
States Steel Corporation, leader m the preparaUon of specimens for metallograph~c exam~-
nation, for whom the Vflella Award was named for outstanding "merit m the field of metal-
lography [1 7] " T h e r e were, of course, many others who contnbuted to the size, actwlty, pro-
ductwlty, and health of Committee E4 during those 75 yearsV
References
[1] Vander Voort, G F, "75 Years of Metallography The ASTM Committee E4 Perspective," Stan-
dardtzatton News, Vol 19, May 1991, pp 58-77
[2] Sorby, H C, "On Microscopical Photographs of Various Kinds of Iron and Steel," BnUsh Associ-
ation Report, Part II, 1864, p 198
[3] Sorby, H C, "Microscopical Structure of Iron and Steel," Journal oflron and Steel Instttute, 1887,
p 225
[4] Rochow, T G, review of MICRO-65, InternationalSymposium on Applied Microscopy, University
of Shetfield, England, 6-9 July 1965, Apphed Opttcs, Vol 5, 1966, pp 420, 461,462
[5] Martens, A, "Die Mlkroskopiche Untersuchungder Metalle," Glaser's Annalen, 1892, p 201
[6] Osmond, F, "Sur la metallographlc mlcroscoplque," Rapport presente' b,la commission des meth-
odes d6ssal des materlaux de construction le 10 f&ner, 1892
[ 7] Heycock, C T and Neville, F H, "On the ConstltuUon of the Copper-Tin Series of Alloys," Phdo-
sophwal Transacttons', Vol 202, Senes A 1, 1904
[8] "Our Front Cover, Albert Sauveur ( 1863-1939)," Cenco News Chats, No 63, p 3
[9] Sauveur, A, "The Mlcrostructure of Steel and the Current Theories of Hardening," Transac'ttons,
American Institute of Mining, Metallurgical, and Petroleum Engineers, 1896, p 867
[ 10] Sauveur, A, The Metallography and Heat Treatment o! Iron and Steel, The Umverslty Press, Cam-
bridge, MA, 1935
[11] "The Role of the Microscope m Ore Dressing," Ore Dressing Notes, No 5, American Cyanamid
Co, Oct 1935
[12] Vanderwllt, "Improvements in the Pohshmg of Ores," Economzc Geology, Vol 23, 1928, p 292
[13] Rochow, T G and Rochow, E G, Resmography, Plenum Press, New York, 1976
[14] Chamot, E M and Mason, C W, Handbook ofChemlcalMtcroscopy, Vol 1, Wiley, New York,
1930
[15] Desch, C E, "Pure and Applied Science," Sctence, Vol 74, No 1925, 20 Nov 1931, pp 495-502
[16] Vander Voort, G F (note, Dec 1990) notice m Metals andAlloys, Vol 2, No 3, Sept 1931
[17] ASTM 1985 Directory, American Society for Testing and Matenals, Phdadelphm, 1985
Wilham G. Frlcke, Jr. 1
Research Under the Microscope

REFERENCE: Frlcke, W G , Jr, "Research Under the Microscope," Metallography Past,
Present, and Future (75th Anniversary Volume), ASTM STP 1165, G F Vander Voort, F J
Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing and Materials, Phll-
adelphm, 1993, pp 88-106
ABSTRACT. Microscopes help man to see All microscopes and ,maglng devices have an inher-
ent resolution that limits the maximum magmficatmn at wh,ch they can be used The pnnclple
of scanning greatly simplifies an ~magmg instrument and sometimes is the only way a picture
can be made Any s~gnal that varies in various areas of a sample can, m pnnople, be used to
make an image
KEY WORDS. m~croscopes, scanning, transm~ssmn electron microscope, electron m~croprobe,

auger, image analysis, local orientation, metallography, metallurgical speomens, mlcrostruc-
ture, metallographlc techmques
Come, let us ramble in the world of microscopes that I have known in my 37 years at Alcoa
and along the way look at research--research, first of all, as we use a microscope to do it, but
then let us put research itself under the m,croscope and wax philosophical You might call this
talk, "Microscopes I Have Known "
We sometimes say a p~cture is worth a thousand words I suggest that pictures are more
~mportant than that When you look into a microscope, you not only see an image, but with
your mind you interpret what you see and get an overall impression, capture the very essence
of the specimen You appreciate what the Germans call its "Gestalt " Y o u become part of the
material when looking through a microscope and, through emotion, know what to do about
thmgs
I deplore the kind of engineer who sends samples to a microscopist and says, "Send me back
a p i c t u r e " He then looks at the picture and does not bother discussing it with anybody, all he
wants ~s a pretty picture to suck m a report to say, "This is my material " Instead, you really
must get familiar with the samples you're working with You have to understand, become one
with the material
Everyone who was around 48 years ago remembers what he was doing on 7 December,
1941, Pearl Harbor Day, when the United States got into World War II Actually, the Euro-
pean war had started two years earlier than that, in September 1939 It was about that time
that something happened when I was walking to school I was in seventh grade, 13 years old
It was a foggy morning and I heard an airplane flying overhead. With my thoughts being on
the war, which had just started, I imagined that someday I might be up there in a plane hke
that, I might want to look through clouds and see what I wanted to bomb So I invented some-
thing I called the cloud-piercing telescope (Fig l) I knew that infrared radiation could go
through clouds a lot easier than visible light could, and so I Imagined a device where infrared
hght coming from the ground went through a lens and was focussed onto an array of photo-
cells--hundreds of them in each direction The individual photocells each put a tiny electrical
Fellow, Alloy Technology Division, Alcoa Laboratories, Alcoa Center, PA 15069
88
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FRICKE ON RESEARCH UNDER THE MICROSCOPE 89
FIG. 1--The cloud-piercing telescope invention.
current into individual wires that went up to a viewing screen in front of the pilot. There each
of these wires had a little light bulb; and the light would get bright if a lot of radiation was
hitting the corresponding place in the detector array, or dark if only a little bit of light was
hitting it. The overall effect would reproduce an image of the ground.
I was so proud of the concept that I submitted that idea to the War Department, and they
even acknowledged my letter. They were kind to me, but even as a seventh grader, I knew there
were a couple of things wrong with that idea. For example, it was too complicated. Look at all
those wires and cells. There are too many things to go wrong and it was too heavy. But worse
than that, with those light bulbs in there, even in the little shadow boxes I visualized, the points
of light were just too big. All you would really see would be a bunch of light bulbs, some lit,
some not lit. In order to get a true impression of the scene below, you would have to back up
quite a bit so the lights would blend into each other, and even then you could never hope to
see objects in the image smaller than the individual photocells. The resolution was not good.
Two things were wrong: the instrument was too complex and the resolution--the ability to
distinguish fine detail--was poor. I could have made the whole apparatus a lot simpler if I had
realized that I did not have to have all of those detectors connected to all of those output
devices simultaneously. In fact, it could be done by one set moving row by row, point by point,
to build up the picture. I would not have a simultaneous picture, but I could have a picture
accumulated over time. Our television sets do that.
This limitation called resolution is a problem that's always with us in any kind of imaging
device. The situation is that of Fig. 2. Here two fellows are looking at two very different instru-
ments, one a microscope and one a telescope. Both see somewhat similar things and they both
are saying (probably under their breath), "If I only had a little bit more resolution! This is great,
90 METALLOGRAPHY:PAST,PRESENT,AND FUTURE
FIG. 2-- The dilemma of resolution.
but I know there's something in there that I just can not see. If I could only improve things
just a little bit, it would be wonderful." Of course, if they did get an improvement then they
would say, "Just a little bit more." We always want more than we can get.
From now on, we will be looking at various kinds of microscopes, seeing what limits their
resolution in each case, and looking at the principle of scanning to see what a powerful concept
it is in giving us information.
l.ight Microscope
Someone asked me one time, "If you could only have one microscope, which one would it
be?" I said, "'Give me a low-magnification stereographic microscope." Many problems are
solved completely at low magnification, but more importantly, to appreciate a material you
must start with a magnification just a little bit more than what the human eye can see. Only
after you appreciate what you arc seeing at low magnification can you go on to higher and
higher magnifications and use the more sophisticated microscopes.
The h u m a n eye, without any lens, can see detail of 0.11 mm, 110 ram. You can not see
anything finer than that because the spacing of the rods and cones in your eye do not allow it.
So, if there is something out there in the world that you want to look at that is smaller, you
need the aid of some sort of a microscope. To see a 1-urn particle, you have to magnify it in
order to get up to the 100-um size that your eye can see. And you have to do it faithfully,
without blurring. A light microscope does that for you by sending light waves to the sample,
and after the light interacts with the sample, say the particle of Fig. 3, you have a lens that
collects the diffracted rays that make up the image that the eye sees. Obviously, that particle
has to change that incoming ray somehow or the eye on the other end will not know it is there.
There are rules of optics that allow you to estimate the fineness of detail, the resolution, that
you can get with a particular lens (Fig. 4). The equation says, among other things, the resolu-
tion depends on the wavelength of the illumination. We commonly use wavelengths about
that of green light where the eye is most sensitive. Resolution also depends greatly on the angle
FIG. 3--Electromagnetic radiation illuminating a sample. Since a microscope collects diffracted rays
to make an image, the particle will not be seen unless it is larger than half of a wavelength.
over which the bottom lens of the microscope collects light, the so-called numerical aperture.
It also depends, to a slight degree, on the medium between the lens and the sample, the index
of refraction.
When you put typical numbers in the equation, you find that the best light microscope can
resolve detail of a quarter of a micron or larger. How far can you magnify that detail to the
size where the human eye can see it (make it 110 um across)? If you magnify only X400, you
can see that quarter-micron object in the image. It does not do any good to magnify more than
X 400, because the detail is not in the original image. Actually, though, the human eye appre-
ciates having a little bit of fuzziness, so you can conveniently go up to magnifications of about
X 1000 in the light microscope.
So much for resolution; what about the subject of scanning? Even light microscopes some-
times do scanning. Here is one that I like in concept (Fig. 5). One problem with light micro-
scopes is that they focus only on one plane. Anything higher than that or lower than that is out
of focus. So if you have a material that extends into the third dimension, all you can see is a
ring around objects at the plane of focus. Anything about that plane or below it would be out
of focus and makes blurry areas in the image. Well, this microscope shown says if certain areas
FIG. 4--Equation for resolution when electromagnetic radiation is used.

FIG 5--A hght mlcro~6ope that scans
are going to be out of focus anyway, let us not illuminate them Let usjust illuminate the parts
that are in focus The illuminator projects a plane of light intercepting that specimen along
that line that is in focus Let us take a picture of that and then scan the illumination and the
microscope together so successively new areas will be illuminated and in focus Ultimately, we
will have a whole picture with the whole specimen in focus and well lit and we've done it a step
at a time The confocal light microscopes that are appearing on the market work similarly
They scan points ofhght not only up and down, but sideways as well Once you begin thinking
of scanning as a potential fix to your problems, you get all sorts of Ideas
Transmission Electron Microscope

Before we look further at scanning-type instruments, let us look at another that, like the light
microscope, has the picture present all over at one time, the transmission electron microscope
(TEM) When I came to work 37 years ago, we had two kinds of microscopes the light micro-
scope and the TEM The TEM at that time was a little thing, a desk with a short microscope
column about a foot high It took pictures at two magnifications • 600 and • 6000 In order
to change from one magnification to the other, you had to take out the entire lining tube, put
it aside, and get the one for the other magnification I took a few mlcrographs in that instru-
ment personally, but the experts tried to keep me away from it The electron microscope was
too complex, too sophisticated, for a young engineer like me
How does the TEM solve the problem of resolution9 Why are we able to go to the very high
magnifications known today, over ten times higher than that early electron microscope9 The
primary advantage is the wavelength of the illumination used Electrons typically have wave-
lengths on the order of four hundredths of an angstrom (Fig 6) This is many orders of mag-
nitude finer than the radiation used In a light microscope and so the resolution IS much better
Unfortunately, a typical TEM also has poor numerical aperture, the angle through which the
illumination comes from the sample is small Fortunately, the favorable wavelength effect
Transmission Electron Microscope
At 100 KV, ~. = 0.037 ~,
Typically:
cz = 0 o 3 0 '
sin ct = 0.01
Resolution = 0.2 nm
FIG 6--Resolution m the transmission electron microscope determined by the equauon o f Fig 4
overpowers this negative aperture effect, and so we get resolutions typically two-tenths of a
nanometer With care, we can do better than that these days, all because we have changed the
illumination from light to electrons
Nowadays, many TEMs even do scanning (making them STEMs), they measure crystallo-
graphic orientation and do chemical analysis. But the classical TEM and the light microscope
are alike in that they have the image present all over, all at once If we start exposing a picture
in this kind of microscope and stop the exposure halfway through, what we have is the picture
that is half exposed--but it is a full picture If we did that with a scanning microscope--stop
halfway through--we would have half a picture, but that half of a picture would be fully
exposed
Electron Microprobe
The next instrument I was associated with ( 1961) was the electron microprobe Notice, I did
not say the scanning electron microscope (SEM) The SEM came later, it is a modified micro-
probe As a matter of fact, our first microprobe, when we got it, did not do scanning Some-
where around 1965, we added ordinary oscilloscopes that provided the ramping voltages to
both scan the beam m the instrument and the beam in the cathode-ray tube used for viewing
An ordinary oscilloscope camera photographed the screen and that was the micrograph In
those days, charged pairs of plates were used to steer the beam over the specimen
What happens when an electron beam hits a material9 Every one of the signals shown in
Fig 7 has been used to make pictures Figure 10, for example, will show a micrograph made
with the electrons captured in the sample (shown schematically at the bottom of Fig 7) We
also have backscattered electrons coming from the impacted areas, electrons that bounce out
of the sample They too can be used to make a picture Secondary electrons, low energy elec-
trons that get jostled out, can make a picture and are the most common source for SEM micro-
graphs Some of these electrons (auger electrons) have particular energies that give us lnfor-
matLon about the kind of atoms in the sample and these can make a composition image X-
rays also give us compositional information Some samples will give off visible light, and you
can get a light mlcrograph out of a microprobe or a scanning electron microscope Anything
else that happens in the material when it is prodded with an electron beam or some other
energy source can, m principle, be used to make pictures if we have a detector for it
Figure 8 shows, m more detail, the paths that individual electrons make as they go down
through a material Most of these electrons follow tortuous paths as they bounce offofatoms
Some even come back out of the sample These are the backscattered electrons Along the way,
secondary electrons are generated throughout that entire bulk However, since secondary elec-
trons have low energies, it 1s only the ones near the surface that can emerge from the material
FIG 7--StgnaA artsmg [rom a sohd sample when struck by an electron beam
and get detected and appear in the picture It is only that area right around the incoming beam
that is seen by a SEM in the secondary electron mode That is why resolution ~s much better
for secondary electrons than backscattered electrons or X-rays
In the lower part of Fig 7 are circled points where its calculated X-rays emerge A quantum
of X-ray comes o f f o f e a c h point indicated It can be seen that the X-rays are generated from
a large volume and they also escape from the specimen easily The resolution for X-rays and
for backscattered electrons IS consequently rather poor, several microns for aluminum
Figure 9 is a light mlcrograph of a casting alloy and Fig 10 shows images of this same area
taken o f f o f o u r original microprobe, the one with electrostatm deflection The first mlcrograph
of this area was made using the electrons conducted through the sample, the ones captured by
the sample Because different areas of the sample captured more or less electrons from the
beam, contrast was built up Most people are used to seeing backscattered electron pictures,
this is the opposite phenomenon, the electrons that are not backscattered The remaining pho-
tos are X-ray maps If we had a light microscope and used it to look down at the sample and
could see particular X-rays coming off, these images are what we would see If we could see
iron X-rays, we would see them coming from those outer particles that contain iron, and we
would also see some silicon X-rays coming from the same ones, even a little bit of copper The
inner particles there contain magnesium and slhcon, as seen in those pictures
We have here an analytical tool, but it is awfully qualitative We would get more quantitative
results from a stationary beam sitting on a particle However, human beings so like pictures,
so hke to think with images, that they often prefer this kind of information Therefore, we end
up giving them both the quahtatlve image and the quantitative analyses
Scanning Electron Microscope

Let us move on to the variation of the microprobe that is intended primarily to make elec-
tron pictures of bulk samples the scanning electron microscope We have an electron beam
that moves over the specimen in a series of parallel lines, while simultaneously, a point ofhght
on a cathode-ray tube (CRT) (a television-hke screen) is moving In the same pattern (Fig 11)
They are doing this scanning in synchronization with each other Now, all we must do to make
up a picture is to measure some signal from the specimen and ask, " H o w many electrons are
~c
96 METALLOGRAPHY: PAST, PRESENT, AND FUTURE
FIG. 9--A photomicrograph of an aluminum casting alloy (light microscope).
coming off of each of those points as I go over them?" Feed that information into the CRT
and make the spot on the screen bright or dark, as the signal changes, and we build up a picture
like this (Fig. 12). As we went over one area of the sample and there were a lot of electrons
coming off, we would paint the picture bright. When we went over another area and there was
a medium number of electrons coming off, we would put a medium brightness light on the
screen, and so forth. Notice that, in principle, the image is divided up into a bunch of little
squares, like my original cloud-piercing telescope, and the finest of the detail (the resolution)
has to do with how tiny an area on the specimen is emitting that signal. For X-rays, those
squares are relatively big; for secondary electrons, the squares are small. In other words, the
effective size of the squares (pixels) making up the pictures is the resolution itself.
Before we leave the SEM, let us look at just one scanning micrograph to illustrate a point as
well as to pique your curiosity. Figure 13 (left) is a SEM shot of a sample etched in caustic. See
the little craters on the surface in the left photograph? It so happens that we can ordinarily
believe our eyes when we look at a SEM micrograph, even though the picture was made with
electrons and our eyes are not used to seeing electrons. Fortunately, the impression we get is
the same as if we were looking with light, and since we are educated to interpret things with
light, we can quickly appreciate what we are looking at there. (Incidentally, that is not true
with TEM; we have to sit down and consciously think what is causing contrast in the TEM.)
On the fight of Fig. 13 there is another micrograph that looks completely different, but in real-
ity, is the same picture turned upside down. The reason it looks different is that our mind is
interpreting changes of illumination as ups and downs. SEM micrographs usually appear to
have oblique illumination. As long as we keep the apparent source of illumination coming
FIG 10-- lJhcropmbepi~tmes o/ H~e same area as big 9 The hrsl photo used spec tmen emrenl and the
others used X-ra~ s o/ parttL ular ~ ave/en,~lhs lhal ~ould be tdenldted ~ ith lhe elemenls mdtcated
from the t o p ( l d t p h o t o ) , o u r m i n d interprets surface c o n t o u r s correctly If we turn the picture

upside d o w n ( r l g h t p h o l o ) , the a p p a r e n t source o f i l l u m i n a t i o n ~s c o m i n g from the b o t t o m , but
o u r m i n d rejects t h a t W e n e v e r h a v e a s~tuatlon zn real hfe where s u n h g h t zs c o m i n g out o f
the g r o u n d A n d so we say, " N o t h a t c a n n o t be n g h t , the light has to be o u t there, the s u n is
o u t t h e r e s o m e p l a c e a n d so I a m going to interpret those features as hills r a t h e r t h a n
depressions "
FIG 1l - - T h e ra ~terpattern u~ed In scanning The dashed hne Is the retrace path
Auger Spectroscopy
We said a while back that s o m e o f the secondary electrons c o m i n g off the sample have par-
ticular energies that are characteristic o f the elements in the sample These are auger electrons
Although an auger instrument usually works with a stationary electron beam, if we can scan
the b e a m and m a k e the auger electron detector accept electrons from only one kind of atom,
we get element distribution maps similar to Fig 10 However, since auger electrons c o m e from
only the outer 20 A or so of the surface, these element maps show what kinds of atoms are
sitting right on the surface and how they are distributed
A look at the energy levels o f electrons inside an a t o m will Illustrate where auger electrons
c o m e from and give us a review of other signals that can be used in microscopes (F~g 14) The
energy levels represented by horizontal lines are at particular locations for each kind of atom
T h e y are occupied by those little fellows shown m the figure that are electrons When we shoot
an external electron at such an atom, we are occasionally going to hit one of those electrons
sitting in the a t o m and knock him away Measure the energy of that fellow who used to be in
the a t o m and we have a t e c h m q u e called ESCA, electron spectroscopy for chemical analysis,
because measuring the energy of that level tells us what kind of element that was That electron
that caused the d a m a g e and bounces off~s one of those baekscattered electrons that we can use
to m a k e a picture
The atom, of course, does not like to have an electron missing, especmlly if, as in the picture,
~t is one of the m o r e t~ghtly b o u n d ones O n e way to get an electron back into the lower energy
level is to capture s o m e other electron sitting on an upper level W h e n one of ItS own electrons
(that electron pictured with the parachute) m o v e s down, the atom loses some energy H o w
does that a t o m get rid of that energy9 O n e thing it can do, and all atoms can do it, is emit an
FIG 12--Sketeh o! the ~trength of the signal coming from various areas of the sample and the corre-
sponding brightness on the vlewmg screen
FIG 13-- Two S E M mtcrographs of an etched ~urface The right photo ts the same a ~the left, but turned
up~tde down
X-ray quantum The X-ray has an energy equal to the energy difference between where the
parachuting electron was and where it ended up If we used an electron microprobe, for exam-
ple, to look at the energy of that X-ray, we could make an analys~s or store the information as
part of a picture Another way for that particular excited atom to decrease its energy, however,
is to put that energy into another electron, get nd of another one of its other electrons and put
all that energy into kinetic energy That ejected electron is the auger electron represented by
the fellow m the balloon
When we have a material with lots of atoms being bombarded by an electron beam, some
of them will be ejecting auger electrons and some of them will be e m m l n g X-rays Both signals
will be coming from the sample And some of the energy of the probing beam will bejosthng
low energy electrons out of the upper energy levels (hghtmg a match under them in Fig 14)
and producing secondary electrons Remember that any of these events can be used to make
a p~cture
Let us pause for a summary here Resolution--the finest of detail in an ~mage--depends on
where the sxgnal ~s coming from In instruments hke the auger, SEM, and m~croprobe, ~t is the
area from around the incident beam that emits those electrons or X-rays that determines the
fineness ofdetad that we can image (Table 1) So with X-rays, we have resolution of about 2
um, with auger electrons, considerably better than that Modern auger instruments use a
focused electron beam and they can get resolutions on the order o f h a l f a micron In a SEM,
TABLE l--Rewlutton of various mtcroscopes
Maximum
Finest Detad,/~m Magmlication
Microprobe (X-rays) 20 100

Auger
m depth 0 002 100 000
laterally 05 400
Scanning electron microscope 0 006 30 000
Light microscope 0 27 1 000
Transmission electron microscope 0 0002 1 000 000
100 METALLOGRAPHY:PAST, PRESENT,AND FUTURE
FIG. 14--Energy levels in an atom showing the source of backscattered, secondary, auger, and ESCA
electrons as well as the transition that produces X-rays.
about 60 A is typical resolution these days. The two instruments that use overall illumination
by electromagnetic radiation depend on wavelength for their resolution. The light microscope
gives us about a quarter of a micron resolution, and TEM gives us four ten-thousandths of a
micron resolution. When we take advantage of these resolutions by magnifying the detail to
the size that the h u m a n eye can see, the m a x i m u m useful magnifications that we can get are
indicated in the last column of Table 1.
ScanningTunnelingMicroscope
There are other kinds o f microscopes, o f course, s o m e of t h e m just being developed O n e o f
t h e m is the scanning t u n n e h n g microscope. It is a very simple microscope in principle There
is a pair o f translating devices to physically m o v e a needle m the X a n d Ydlrectlons The point
o f that needle, hopefully sharp to a t o m i c dimensions, is maintained at a constant distance
above the surface o f the sample by maintaining a constant tunneling electrical current or
a t o m i c force Meanwhile, the data collection system is recording the input needed to maintain
the separation In other words, we have a surface roughness m e a s u n n g device of atomic
dimensions where we get pictures reconstructed through a c o m p u t e r Distances are measured
in n a n o m e t e r s In ideal cases, we can detect the ups and downs as the needle moves over indi-
vidual a t o m s
Image Analysis
As soon as s o m e o n e gives a scientist a picture, the first thing he or she wants to know Is, how
big is that thing there or how m a n y of these things do I have here Getting quantitative infor-
mation from a microscope or mlcrograph is called image analysis Along the way, we often
c o m p u t e i m p r o v e m e n t s to the image as well That is called image e n h a n c e m e n t
The secret to getting an image into a form that a c o m p u t e r can deal with it is to dlgmze it,
break it up into picture points (plxels) T h i n k back to m y cloud-piercing telescope I had light
bulbs arranged m a grid pattern, the picture was broken up in a series o f points close enough
together so that the h u m a n eye could not see that they were not continuous A digitizing T V
c a m e r a on a hght microscope or a similar device on a SEM can break the image into a series
o f picture points each o f which has an associated n u m b e r that represents the brightness at that
particular point (Fig 15) O n c e the data are m a form that a c o m p u t e r can read, all sorts of
c o m p u t a t i o n s are possible
004 025 036 121 163 226 178 152 102 089
124 078 023 133 187 204 172 144 085
255 174 033 167 199 210 189 132
231 189 042 196 174 186 145 172
203 187 078 098 127 173 131
196 163 064 045 103 147 122
154 112 038 053 089 093
128 130 042 028 064
085 086 044 027 057
062 075 038 026

FIG 15--Data representmg a dtgtttzed ptcture The numbers are brtghtness levels These are the num-
bers producmg ~ontrast as m Ftg 12
For example, the top left photo in Fig 16 is an original picture presented to a c o m p u t e r We
can see that the illumination was not uniform The left side area is darker than the right side
Since we are dealing with numbers, it is easy for a c o m p u t e r to i m p r o v e the p~cture It just
measures the average brightness in one locaUon and adjusts it to s o m e standard level that has
been set, and measures the average brightness m another area and brings everything to the
same average to wipe out that illumination difference (top rtght o f Fig 16)
A n d the c o m p u t e r can do things like fill In little gaps m the grain boundaries, change the
overall contrast, and so forth It can emphasize some things, de-emphasize some other things,
and completely get rid o f features that it does not hke because of size considerations or other
criteria Eventually, we end up m a r k i n g the things that we want to measure by creating a
binary picture where everything is either white or black, leaving bright the things that we want
to measure (lower left, Fig 16)
Since the whole picture IS broken up into an array o f picture points, measuring these is now
fairly simple T o measure the area o f a particle, we just c o u n t the n u m b e r of picture points in
FIG 16--Dtgltlzed mlcr(~Traphs The upper le[t is the orlgmal tmage The uppet rtght Is aper shading
corre~tton, and the lower left ts a binary (black-)4har tmage ready[or measurement
the particle To measure a chord, we just count the number of picture points along the chord
To measure the perimeter, we measure the number of picture points all the way around the
outside of a feature
Local Orientation Measurement

Crystallographic oraentatlon Is not something that makes an image, but xt is something that
can be measured in a m~croscope Since gram orientation is important, we have attachments
on our SEM and T EM to make rapid evaluation ofbackscattered electron diffraction patterns
(KJkuchl lines) The patterns have always been there if we wanted to look at them What is
new is that a computer assists us m rapidly reconstructing the crystallographic radices for the
orientation of that particle crystal
Stereo Micrographs
The third dimension, the height dimension, is often important We can get a qualitative
impression of height on almost any of these microscopes by taking two pictures at an angle to
each other, one for each eye These can be put into a stereo viewer to visualize the third dimen-
sion or even measure the elevation of a few points But we are still tookmg for easy ways to
characterize the ups and downs of a rough surface quant~tatwely and m detail, not just a few
points, but all over so we can, for example, analyze fracture surfaces to estabhsh failure
mechanisms
The Future
Now we are beginning to estabhsh a wish list for the future What do we want9 Back in 1976,
I good-humoredly perpetrated a hoax about supposed late-breaking developments around two
new microscopes, the flashdark microscope and the temporal scanning microscope When I
sent the article in for publication, I intended it for a column called "Light Metallurgy," light
in the sense of not heavy, even frivolous But even back there in 1976, microscopes were com-
plex enough that nobody could really keep up-to-date, nobody could quite dare to say, "There
ain't no such t h i n g " Today things are so complex that people are almost sure to believe if we
tell them it is so
The supposed flashdark microscope worked on the premise that if there is something called
a flashlight, it is reasonable that there is a flashdark as well Now, we can not see the particles
inside a piece of aluminum, for example, because the light bounces off of the surface--and it
is left dark down in there But If we use a collimated beam of darkness, the dark can penetrate
down inside the metal and we can see those particles
An even more important concept is the temporal scanning microscope (Notice my empha-
sis back then on the concept of scanning ) A time machine on a microscope would be useful
for things like failure analysis, allowing us to see what conditions were dunng the actual failure
Although the Instrument Itself IS a hoax, temporal scanning has been done and I have done
it Figure 17, for example, out of one of my early papers, shows a fatigue crack at increasing
numbers of cycles You might ask the question, " H o w did I know that something interesting
was going to happen to the tip of this crack so that I took this series of mlcrographsg" And the
answer is, I did not know that something interesting was going to happen I waited until I saw
that something did happen and then scanned backwards in time I took the last micrograph
first and then the next-to-the-last, etc That was possible because I had replicas of what the
material looked like at those previous stages I had frozen time
FIG. 17--The same fatigue crack seen at successive times in its Ire. The numbers are millions o f cycles
(light microscope).
Another example of time scanning, this one in the transmission microscope, shows a frac-
ture surface made by a stress-corrosion crack (Fig. 18). I managed to mark where it was at one
time before I was able to look at the sample at a later time when the crack had grown further.
Again this was through replicas, but there is no question about how the crack had looked in
the past.
Now we are starting to get serious about what is going to happen in the future of microscopy.
Although it is always dangerous to make predictions, some directions seem evident.
New objective lenses for the light microscope are coming on the market that allow us to back
the microscope away from the specimen. We can get 1-#m resolution, for example, at a work-
ing distance of 152.4 m m (6 in.). This allows us to put windows, environment, furnaces, etc.,
in the gap. It also allows us to look at rougher surfaces without much loss of resolution.
I think we are going to see a lot more of computers. I think there will be a lot of image storage,
the digitized pictures going into rather permanent files, so that microscopists can call up an
image of what typical material looks like, to compare to their present specimens. They will not
have to go digging through the files and trying to find a micrograph of something they have
done before. The images will be accessed by other people in other groups and other buildings.
I think we will be seeing scanning pictures using novel signals. After all, any signal that
comes offthe sample that makes changes in a detector can, in principle, be put into a picture.
Ultrasound--we are already into ultrasonic microscopes--infrared, sonic emission, or per-
haps, a microscope built on, say, smell. If we had a detector for smell, and the smell varied
across the specimen, we could get a smell picture. Who knows?
Let us get philosophical. Who does microscopy? Who should do microscopy?
FIG 18--A s'tre~s-corroston crack m a r k e d / o r where tt was at one ttme /or vtewmg at a later ttme
Microscopes are powerful instruments and I think microscopy has to be done on two levels
The ordinary researcher, somebody whose main interest is in precipitation or recrystallizatlon
or some metallurgical phenomenon, should not be afraid to use a microscope In fact, he or
she has to use a microscope to see in his head what is happening That does not mean just
looking at mlcrographs that somebody else takes He has to be there looking at the sample,
moving around and seeing the overall process He has to get the mental picture
But we also need experts, those whose profession is microscopy, those trained, those who
will guide the other fellow and do some of the work for him or her
And that raises the question of where the microscopes should be It is not an easy question
to answer There is something to be said for the microscopes being where the research is being
done The individual investigators are more likely to use the microscopes if they are close by
The microscopes become more involved in the projects The response time for work tends to
be short
But we can also make a good case for having all the microscopes and all of the microscopists
in one central location and require that the investigators and samples come to the central
microscopy laboratory That way, because of proximity, there is communication between
microscopists They stimulate each other, profit from past experience They share reczpes,
avoid blind alleys Equipment is better utilized and expensive duplication avoided The
approach is more professional ! tend to favor this approach
But I suggest that there is a test for determining if the microscopist m your area is justified
It is through the word "exult " I f your microscopist is good and knows he or she is good, if you
have challenged him or her with Interesting work, if he or she contributes to projects and prob-
lem solving, if he or she is eager to come to work each day, m short, if he or she "exults" m his
or her work, you have a valuable and necessary individual
I've exulted m my work for 37 years
Metallographic PreparationTechniques
Gerald S. Cole, ~Leslie Bartosiewlcz, ~a n d F l o y d E. Alberts ~
Automotive Materials and Their

Characterization: 1916 to 1991
REFERENCE" Cole, G S, Bartoslewlcz, L, and Alberts, F E, "Automotive Materials and
Their Characterization. 1916 to 1991," Metallography Past, Present, and Future (75th Anmver-
sary Volume), ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szir-
mae, Eds, American Society for Testing and Materials, Philadelphia, 1993, pp 109-138
ABSTRACT" The automotive industry has been altered enormously since the era of the Model
T This paper describes some of the reasons for the changes in terms of technological drivers,
especmlly in terms of how new materials and processes ~mprovecomponent functmnahty Sev-
eral materials used in the Model T, such as cast iron, steel, glass, and ceramics wdl be compared
to modern materials used in a vanety ofautomotwe components The key systems of the vehicle
represented include electncal, exhaust, powertraln, chmate control, and body
KEY WORDS. automotive materials, metallography, metallurgacalspectmens, mlcrostructure,

metallographlc techniques
Automobiles have changed enormously since the early 1900s in almost every detail of mate-
rials and manufacturing With respect to material changes, vehicle bo&es were based on con-
ventlonal cold-rolled steel and have evolved into new high-strength, galvanized, bake harden-
able, dent, crash, and corrosion resistant steels, aluminum, magnesium, polymeric, and metal
matrix composites make up a growing list of lightweight materials, cast irons now include
spheroidal and compacted graphites along with the more common flake form, new ceramic
materials have been developed for catalysts and turbine blades whde semiconductors are now
used m electronic devices, complex glass/polymer laminates have replaced the dangerous sin-
gle panes of glass, high-strength steels have been developed for lighter weight, high-tempera-
ture materials, such as titanium alloys, have been developed for exhaust valves, and so on
With regard to components powertrams are low-polluting, lower weight, lower friction, and
more responsive, new sealed-beam halogen designs have changed our hghtmg concepts, com-
puterized slhcon-based digital controls have replaced analog circuitry, seat belts and air bags,
coupled with anti-lock brakes provide considerable more safety to the driver, and so forth
New design, fabrication, and assembly techniques have had to be developed to produce the
new components from these new materials
Material analysis in the Model T era used classic metallography, based only on light micros-
copy The matenals and components m modern vehicles require materials characterization
methodology based on a much broader range of sophisticated instrumentation scanning and
transmission electron microscopy (SEM and TEM), electron microprobe analysis (EMPA),
and electron and X-ray spectroscopies
Since the authors collectively have worked over 75 years in the automotive industry, we
dec~ded to commemorate thin seventy-fifth anmversary of the ASTM Committee E4 on Met-
allography by reflecting on the auto lndustry's 75 years of metallography and materials expe-
SoentlfiC research staff, Ford Motor Company, Dearborn, M148121
109
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
hence Because of our association with Ford Motor Company, we will &rect our presentation
to comparing differences between some of the materials used in the Model T and in present
Ford vehicles
The Ford Model T was introduced a httle more than 75 years ago (in 1908 to be exact) but
really reached its stride by 1916 when over 500 000 umts were produced Figures 1 through 5
show sections of this vehicle that revolutionized the personal transportation industry of the
world Figures 1 and 2 show right and left sides of a conventional four-passenger Model T,
Figs 3 and 4 show the components of a "Touring Model T," and Fig 5 depicts the powertraxn.
It is interesting to note that by 1916 the overall functlonahty of the automobile had been fairly
well defined with the major components--powertraln, dnvetraln, body, chassis, exhaust, inte-
rior, electncal, and fuel systems--not &ffenng much from modern vehicles (see Appendix I)
Upon examining the literature of circa 1916, we realized that there was not too much dif-
ference between the metallographlC techmques used then and those used today Metallo-
graphic samples were cut, mounted (albeit with Canada balsam rather than with polymeric
materials), ground, polished (using many of the presently used materials except diamond), and
etched (with nitric, pacrlc, hydrochloric, and sulphunc acids) as today Microscopy was begin-
nmg to be developed and there were even metallographs to take photomicrographs, see Fig 6
[ 1] Other authors in this conference will discuss these developments m more detail Our paper
will focus more on the applications of microscopy for materials characterization, particularly
with respect to the materials and components used m the automotive industry
Because of space constraints, it is Impossible to examine all the components, and their con-
stltuent materials, used in the Ford Model T Rather, we wdl analyze the material makeup of
some e~ght components that we were fortunate to obtain from a local Model T restorer The
Model T used many materials that are still employed to this day (see Appendix II) examples
FIG l--Ford Model T, right sld~
COLE ET AL. ON AUTOMOTIVE MATERIALS 111
FIG. 2--k~)rd Model T, left side.
have been selected (and are starred*) from cast iron, steel, aluminum, copper, glass, ceramics,
and paint.
Modern vehicles are very different in design (compare Figs. 7 through 9 with Figs. I through
5). The overall view of a 1990 Ford Probe is seen in Fig. 7, the body and chassis in Fig. 8, and
the powerplant in Fig. 9. However, the major materials used in today's cars are not altogether
different from those used in the Model T (see, for example, Table 1).
Materials trends from 1975 to 1985 (Table 2) demonstrate continuing reduction in total
vehicle weight achieved by a marked reduction in the amount of steel.
The Evolution of New Materials and Components

On examining the changes between the Model T and the present generation of vehicles, it
is interesting to surmise how and why the materials and components have evolved. The many
driving forces for technological change are exceedingly complex. They can be cataloged in
TABLE 1--Materials" used in Model T and modern cars.

Material Model T, % Modern, %
Rubber 3 4
Wood 14 9 (polymers)
Glass 4 3
Aluminum 6 5
Iron 10 13
Steel 47 60
112 METALLOGRAPHY PAST, PRESENT,AND FUTURE
TABLE 2--Materials m the automobtle (rounded weights and percentages) a

1975 Car 1985 Car
Matenal Weight, lb % Dry Weight, lb % Dry
Steel
Cold Rolled 530 20
Other 2300 850 30
HSS 100 270 10
2400 65 1650 60
Grey ~ron 600 15 370 13
Aluminum
Wrought 40 1
Cast 110 4
100 3 150 5
Magnesium
Copper/brass 40 25 1
Lead 30 3 30 1
Zinc die castings 30 10
Glass 90 2 75 3
Plastics 160 4 235 9
Rubber 180 5 125 4
Sound deadener 90 2 60 2
Miscellaneous (paint, adheswes, 50 2
textiles, etc )
Average dry weight 3800 2800
a 1 lb = 0 029 kg
terms of technological change pushed by product (that ~s, vehicle) considerations, changes in
manufactunng technology, and governmental pressures (acting as a catalyst) A bnefdescnp-
Uon of the pressures for change are included m Appendix III(a) and (b) for the reader who
wishes to understand the pressures that drive evolutionary change in the automotive industry
The selection of materials and components that have been selected for analys~s include a
cross-sectmn of ~mportant components used m the automobile.
1 electrical system (spark plug),

2 exhaust system (catalyst and muffler),
3 powertram (valve, from gray cast iron and steel),
4 dnvetram (transmission axle and gear from alloy heat-treated steel),
5 chmate control (radiator from brass and aluminum),
6 body structures (stamped box from painted cold-rolled steel), and
7 windshield (glass)
A short description of each component wtll be presented including mlcrographs companng

the Model T and modern component, where possible The authors will try to consider some
of the crmcal product and materials features that differentiate component, materials, and pro-
cess development over the last 75 years
Electrical System
The spark plug lgmtes the fuel charge by taking the electrical impulse from the ignition sys-
tem and discharging it across the gap between the plug electrode to produce a spark to ignite
COLE ET AL ON AUTOMOTIVE MATERIALS 113
FIG 3--Ford Model T, schemattc of body structure
the gasohne/alr mixture The cnUcal ~ssue ~s that there ,s no eas~er path for the electrical dis-
charge than across the gap to form a combusUon-promotmg spark Historically, ceramic insu-
lating materials have predominated, but at various t~mes, glass, quartz, mica, and even wood
have been employed The Model T used a porcelain, clay-based ceramic These materials were
excellent electrically at room temperature when unstressed, but of poor strength when sub-
jected to mechanical pressure and thermal shock Figure 10 shows the design of the modern
and Model T plugs Figure 11 shows the structure of a modern plug m more detail
I
L~
COLE ET AL ON AUTOMOTIVE MATERIALS 1 15
I
L~
116 METALLOGRAPHY:PAST, PRESENT, AND FUTURE
FIG 7--1 otd Probe
Charactert s'ltcs o/ the ( eramlc

The heart of the spark plug is the insulator The demands on this ceramic component are
very. severe, and according to Owens et al [2], has the following properties
1 High strength to withstand the severe mechanical stresses of the assembly and installa-
tion and the large thermomechanlcal stresses associated with operating for most of its life
at a red heat with one end under high pressure and the other at atmospheric (and may
even at times be sprayed with water)
2 High hardness to resist abrasion
FIG 8--Ford Tempo, body structure
FIG. 9--Cutaway view ~?/t')~rd 12 valve 2.2 L, turhocharged I-4.
3. Electrical resistance: to prevent power loss by electrical leakage over a broad range of
operating temperatures (a resistance of 105 mcgohms or greater is typical).
4. Dielectric strength: to prevent electrical breakdown at potentials that can reach 20 kV or
greater.
5. Thermal conductivity: as the temperature is raised, thermal conductivity increases (as
with most ceramics). When the temperature is <350~ excessive combustion deposits
occur leading to engine misfiring. At temperatures between 500 and 600~ combustion
deposits burn away, but at temperatures >950~ too high a conductivity can lead to
preignition problems. Note that too low a conductivity can reduce thermal shock
resistance.
6. Thermal shock resistance: since spark plugs have to operate at temperatures between
cold incoming fuel air mixtures at subzero temperatures, greater than 800"C temperature
of the exhaust gases, and in approximately 1 min.
7. Chemical inertness: to fuel mixtures and lubricating oil additives.
FIG. 10--(a)Model T sparkplug, and (b)modern spark plug (original magnification, X 1.5).
Electrode Materials
The metals selected for the electrode are important because of the extreme environmental
and chemical conditions operating at the spark plug gap. Electrodes tend to erode in the com-
plex environment of the electrical volatization, high temperatures, and the corrosive nature of
the oxygen and sulfur present in the gasoline. The earliest electrodes were platinum or copper;
later, nickel was used, but was further alloyed with manganese and silicon to increase resist-
ance to sulfur and oxygen attack. The classic manganese-silicon-nickel alloy plug material now
contains titanium, zirconium, barium, thorium, cobalt, and chromium. Some alloy additions
improve the corrosion resistance, either directly or by grain refining; others reduce the work
function in an attempt to influence breakdown voltage. Modern materials use high chromium-
content alloys, but chromium's low electrical and thermal conductivity affects functioning.
Higher heat transfer is desirable, and copper cores are present in the electrodes so that heat can
be more easily removed from the central firing system and back to the engine cooling system
via the plug insulator, body shell, thread, and gasket.
Seal Between Plug and Head

Early components used copper-containing asbestos string; gaskets of rolled copper and steel
were also used. Since smooth gaskets fall offwhen the plug is removed, a locking design is now
used.
FIG 1l--Schematl~ o/ modern spark plug ( l ) flash over rzbs, (2) termmal post, (3) ceramtc m~ulator,
(4) ~teel shell, (5) hm pre~s groow,, (6) mckel/glars seal, (7) carbon suppresor, (8) shell teat, (9) lower seal,
( 1O) ~hell thread~, ( 11 ) ~opper core center ~lectrode, (12) msulator ttp,(13) ground electrode, and (14) pro-
le~tton mto ~ombu~ton chamber
M o d e l T versus M o d e r n Destgn
As shown m Figs 10 and 11, modern plug materials are composed of an Inconel (trademark
o f INCO Alloys International) sheathed copper electrode, a cold-rolled steel terminal post, a
90% A1203 plus clay porcelain ceramic, and a copper glass seal The Model T materials
included a brass-threaded connector onto the steel base electrode and a carbon-conducting
path between the two electrodes
Exhaust System
The exhaust system for the Model T used a gray cast iron exhaust manifold coupled to a
steel muffler, to reduce the sound of the exhaust. Modern vehicles now require a very sophis-
ticated exhaust catalyst capability. Every car presently built in or imported into the United
States has a catalytic converter to reduce the unwanted pollutants from the combusted and
unburned gasoline vapors emitted from the tailpipe. The catalytic converter increases the con-
version of unwanted exhaust gases such as hydrocarbons water and carbon monoxide (CO)
into nitrogen (N,), carbon dioxide (CO,), and water (H20). The complete exhaust converter is
shown in Fig. 12. The ceramic monoliths, shown below the assembly, are hard ceramics, usu-
ally cordierite [Mg2 (Ai4SisO~0)], having thousands of axial channel openings (approximately
1 m m wide) running from end to end. Each channel is lined with a thin coating o f stabilized
gamma A1203 to promote a large specific area and thermally stable component. The catalyst
itself is either platinum, palladium, or rhodium; Fig. 13 shows the details of the washcoat that
contains the precious metal catalyst. The size and distribution of precious metal is critical,
since a uniformly large catalyst surface area is required to contact and react with the exhaust
gases. The large surface area is accomplished by having the catalyst distributed in small par-
ticles of typically 5 nm or so diameter.
Valvetrain (Valve)
Valves continue to undergo significant design and materials changes since the initial Model
T design was developed. The dual material seen in the Model T valve (Figs. 14 through 16)
results from a cast iron valve body that is friction-welded to the cold-rolled steel stem. The
overall view is shown in Fig. 14. Figure 15 shows the interesting structure of the weld zone
region. The structure of the cold-rolled steel stem is shown in Fig. 16(a) while the typical gray
cast iron structure of the valve head is seen in Fig. 16(b). Much of the materials' developments
in valves has been due to increasing demand for higher and higher engine operating temper-
atures over the past 75 years. This has necessitated more corrosion resistance and higher hot
FIG. 12--Cutaway view o['modern catalytic converter showing ceramic element.

FIG. 13--Detailed view o f ceramic monolith with wash coat.
strength. Coupled with the removal of leaded fuels, the requirements for higher power and
improved durability have necessitated that there be reduced wear between the valve, valve
stem, and the head. In the 25-hp Model T engines, both intake and exhaust valves were the
same design and material. This is not true in modern vehicles where both the design and mate-
rials parameters for the intake and exhaust are different. The modern intake valve is composed
FIG 14--Model T ~@aust valve (X 3)
FIG 15--Structure at welded regton of valve s'tem and head (• 100)
FIG 16--(a) Structure o! cold-rolled s'teel stem o f valve and (b) ~'tru~ture of grey ~ast m m head ~ectton
o! Model T valve (ortgmal magmfi~atlon, • 100)
of a one-piece cold-rolled steel shaft, heat treated at the upper retainer end for wear resistance
Figure 17(a) shows the complexity of the modern valve Both the valve seat configuration and
the valve surface have changed considerably versus the Model T In addition, the steel used in
the modern intake valve is of much higher quality, and this is shown in Fig 17(b) Because of
the higher operating temperatures, the exhaust valve materials are even more comphcated, the
FIG 17--(a) Overall shape o[ modern retake valve (X 3), and (b) structure of heat treated ~teel used m
modern retake valve body (X 500)
valve body is comprised of a hollow (sometimes sodium-filled) high-temperature Inconel alloy

stem that in turn is welded to a heat-treatable steel tip
Transmission (Axle Shaft, Transmission Gear)

The transmission gear and shaft steels used in the Model T were fairly high quality Two
examples are shown in Figs 18 and 19, the axle shaft and a transmission gear The modern
and Model T axle shafts are shown in Figs. 18(a) and (b), at )< 100 While the austenlte grains
are almost identical in the two steels (the Model T has a slightly larger grain size), the carbide
proportion is quite different and the modern steels are correspondingly stronger The modern
and Model T transmission gears are shown at • 10 in Figs 19(a) and (b), respectively. In addi-
tion to the different tooth design, the modern version has a case-hardened layer of about 400
#m thick The Model T structure, shown in Fig 19c, has approximately one-tenth as much
hardening depth (to 50 #m) The large difference in microstructure is associated with the dif-
ferent processing available with the Model T Seventy-five years ago, case hardening was either
a salt bath or flame treatment, this was slow, poorly controlled, and produced a shallow surface
treatment. Modern case hardening is performed by induction heating, this takes place in sec-
onds and has a greater effect on the structure The improved properties allow the modern com-
ponent to withstand much higher abrasion and compression loads
Climate Control (Radiator)

It was not until quite recently (the past ten years) that the copper-brass radiator began to be
replaced by other materials Ford Motor Company has been a leader in using lighter weight,
less costly processing in this area Figure 20 shows the vacuum brazed aluminum radiator that
has been the result of many years of metallurgical and process research and development [3]
The new process required that a braze be developed that (a) would not corrode during service
(that is, did not require a flux) and (b) could be applied in such a manner that it would flow at
the processing (brazing) temperature tOjOln the fins and headers without melting through and
destroying the assembly There are many issues that have to be controlled in a brazing oper-
ation the heat source and temperature, vacuum environment, fixturlng, alloy brazes used,
brazing application methodology, etc Figure 21 illustrates the kind of problems that had to
be overcome The photograph on the right shows a void resulting from incomplete brazing of
fins to a header When the temperature became too high (in this case, the control temperature
was only 2~ above the set point), the braze flowed away from the junction and left the
observed void failure The typical brass structure of a Model T radiator component is shown
m Fig 22, it is not different from modern brass microstructures
Body Structures (Stamped Box)

The demands on the steels that formed the body structures of the Model T were obviously
different from those required for the modern vehicle designs The typical mlcrostructure of
ingot-cast cold-rolled steel used in the Model T is shown in Fig 23, there are a sufficient num-
ber ofnonmetalhc inclusions that this matenal could not be used to form the skins of the pres-
ent vehicles Modern body steels are considerably more drawable and are produced by contin-
uously cast low-carbon, low-sulfur steels that often are mlcroalloyed to develop hardening
during paint baking operations There is insufficient space in this presentation to document
the considerable research and development efforts by the steel industry that have resulted m
highly drawable, reduced gage thickness (yet dent resistant), automotive steels developed over
the past 75 years
FIG 19--Transmls~ton gear (• 6) (a) M o d o n gear, and (b) Model T, and (c) Model T transmls ston
gear (ortgmal magmjl~atum, • 100)
FIG 20--Modern vacuum-brazed radiator
FIG 2 l--Structure oHm~header region (ortgmal magndl~atton, X 100)
FIG 22--Structure o! conventional brass sectton of Model T radtator (X 100)
FIG 23--Structure of cold-rolled steel box (X250)

FIG 24--Pamled surlace o/Mode/T body component (~<750)
Corrosion protechon is an ~mportant characterlsnc of body structures In the era of the

Model T, there was httle problem with rusting of car bodies, smce there was no salt used on
the roads Thus, the pamt system employed was simply several layers of enamel over the
primed steel component, as m Fig 24(a) Modern auto bodies are now exposed to an entire
range of corrosive med~a, which produces generahzed corrosion, as seen in the characteristic
scratch test of Fig 25 In order to reduce this corrosion, the steel and auto industries have
developed an entire range of protective coatings, m addition to paint (It should be noted that
paint systems have undergone considerable change over the past few years as a result of pres-
sures for reduced hydrocarbon emissions ) Zinc-based coatings (electrogalvanlzed and hot
dtpped) are the first protectwe layer This is followed by a phosphate electrocoat and a primer,
then by a base coat, a top coat, and finally by a clear outer coating
Body Structure (Windshield)

The original developments m glass technology have followed pressures for increased pas-
senger safety Whereas the Model T used plam plate glass, modern vehicles began using tem-
pered and laminated glass many decades ago Recent developments have focussed on ad&-
tional customer-desirable features The modern Ford "Instaclear" glass contains sophtsttcated
Z n O / A g / Z n O layers that, while maintaining perfect vlslbthty, can be heated by the apphcat~on
of a low voltage (Fig 26). Such products allow the wmdshleid to be deiced in several seconds
Conclusion
The Model T was an exciting revolution m motor transport But, over the past 75 years,
there has been a continual evolution to the modern automobile In contrast to 1916, when
Ford Motor Company sold 501 000 vehicles, the company now sells seven Umes or 3 5 mflhon
FIG 25--Corrosion m modern steel panel
vehicles in the U S and Canada and over 5 8 million worldwide The automotive industry
has grown considerably over the past 75 years and now consumes some one-sixth of America's
Gross National Product
It is unfair to attempt to understand the Model T by examining only a small slice of seven
or so components and develop a complete description of how and why the materials, com-
ponents, and processes evolved from the Model T era The goal of the authors was to outline
some of the materials and processing changes that have led to the present vehicles For each
material and component, material structural analysis and characterization and physical/prop-
erty standards have been developed by the industry Without materials structure characteriza-
tion, automotive developments could not have proceeded as rapidly as they have, and It IS for
this reason that the seventy-fifth anniversary o f ASTM Committee E4 requires recognition
Modern materials characterization includes more than just light microscopy Since the
Model T era, new technologies have been invented for mlcrostructural examination, analysis,
and evaluation Electron microscopy (SEM, TEM, AEM) and spectroscoples (Auger, XPS,
SIMS), X-ray, and acoustical techniques, all coupled with computer methodologies, are now
being employed to analyze the performance and behavior of materials and their fabncatlon
As the automotive industry employs more complex materials and processing, and as safety
requirements increase, more sophisticated materials characterization techniques will continue
to be developed With the members of ASTM Committee E4 ensunng continual standardiza-
tion of these methods, the quality of the automotive industry will be able to advance in an
orderly fashion
FIG 26--StJu6ture o/modern Ford "lnslaclear"glass wmds'hleld (• 100 000)
Acknowledgments
We would like to thank the staff of Greenfield Village/Henry Ford Museum for access to
their records and files, Mr Bill Barth of Troy, Michigan, a restorer of Model T cars, for all of
the Model T components described in this paper, Ms Darlene Flaherty for access to Ford
Motor Company Archives, and Dr W Wlnterbottom for supplying photographs of the alu-
minum radiator
APPENDIX I Major Components in the Automobile
Powertraln (dependent on design) Chassis

Head Frame
Valvetraln Suspension
Valves (Intake/exhaust) Arms
Retainers Springs
Springs Brackets/crossmembers
Camshaft Steering
Tappets Wheel
Rocker arms Kruckle
Intake mamfold Shaft, locks
Block Air bag

Power conversion Brakes
Connecting rod Fraction matenals
Piston Rotors
Piston rings Drums
Wrist pin Calipers
Crankshaft Master cyhnder
Miscellaneous Wheels
Covers Rims, spiders
Brackets Tires
Pumps Exhaust System
Belts/chains Exhaust manifold
Hoses Emission control
Drivetraln Muffler, pipes
Transmlsslon Climate Control
Housing Heater, A/C
Torque converter Radiator
Clutch Fluids
Housing Fan
Rear axle Belts/hoses
Gears Fuel System
Drlveshaft Gas tank
Clutches Pumps
Housings Valves
Differential Fuel
Body Interior
Bumpers Seats
Fenders Belts
Trunk (deck lid) Instrument panel, switches
Hood (inner/outer) Electronics
Doors (inner/outer) Miscellaneous
Hinges Lubricants
Fasteners Bushings, insulation
Glass Adhesives
Moldings, grill Sealers and fillers
Rocker panel Corrosion protection
Floor pan
Paint
APPENDIX II Materials and Components in the Ford

Model T circa 1916
Powertraln
Head Gray iron (GI)
Valvetram
Tappets GI head, cold-rolled (CR) steel stem
Valves* Heat-treated steel
Push Rods
Camshaft Drop-forged, heat-treated steel
Gear Malleable iron
Beanngs GI bushing, babbit beanng
NOTE Starred components (*) are those experienced m this paper
Intake mamfold GI (aluminum prior to 1915)

Block Steel frame, cast GI combustion, Welsh plug
Power Conversion GI (hardened steel pro/bronze bushing/beveled after 1914)
Piston Drop-forged steel
Connecting rod GI
P~ston nngs Machined seamless steel tubing
Wrist pm Drop-forged V-steela
Crankshaft Babbitt
Beanngs GI
Hywheel Bronze, (GI b in 1919)
Carburetor*
Dnvetraln
Transmission
Housing GI (aluminum prior to 1916)
Brakes Steel on steel (GI housing)
F/R Axle* Drop-forged V-steel, paper gasket, fiber thrust washer
Gears Drop-forged, heat-treated V-steel
Dnveshaft* Drop-forged, heat-treated V-steel
Clutches Steel d~sk in oll
Housings GI
Differential GI
Body Body structure (pressed sheet steel over wooden frame)
Bumpers None
Fenders* CR steel (form, roll, hammer, press)
Trunk, hood CR steel (hood was aluminum prior to 1915)
Hinges/fasteners CR steel
Glass* Untempered glass
Corrosion Protection Paint
Paint* Four coats 450~ baked enamel on primer
Flrewall Wood
Exhaust system
Mamfold GI, with flanged steel p~pes connected by brass nuts
Emission control None
Muffler/pipes GI ends, steel tubes (asbestos wrapped before 1916)
Chassis
Frame Wood
Suspension V-steel
Spnngs Steel (six leaf m front, eight m rear)
Steenng wheel Wood w~th GI spider
Shaft Steel
Gears Planetary
Knuckles/spindles V-steel
Hand brake Steel/asbestos on GI expanding with spnngs on rear wheels
Wheels Wood (ball beanngs m front)
Hub caps Brass
Tires Rubber (rear treaded m 1915)
Lubricants, sealers
Electrical
Commutator* Cast aluminum
Starting motor (1917)
Generator
Ignmon Magneto with 16 magnets
Spark plugs* Porcelain and steel
Battery
Wrong Copper
Lighting Sealed beam (gas until 1915)

Horn Electrical (after 1915)
Climate Control
Heater None
A/C None
Radiator Brass fins soldered to copper tubes
Fluids Water
Fan blades Steel, GI hub, leather belt driven
Hoses
Fuel System
Gas tank Soldered terne plate, brass sediment bulb
Pumps None" gravity feed, brass tubing
Valves
Fuel Unleaded gasoline
Intenor
Seats Imitation leather and burlap
Belts None
Switches Light switch/ignition switch attached to dash (firewall)
Instrument panel None
Electronics None
Miscellaneous
Lubricants
Bushmgs GI, steel or babblt (69)
Insulation Paper products
Mats Rubber
Descnptlon Engine 14. 176.7 m 3, 22.5 hp, 4 0 compression raUo
Maximum speed 35 mph
aHeat, quench, anneal, forge, tumble, snag, straighten, machine, polish
b41 lbs as-cast, 35 lbs fimshed, in 16 operations
APPENDIX IIIA--Product-Based Technological Change

Most changes m the automobile have been customer-driven They occurred as a result of a
new material, component, or design that enhanced the vehicle's functlonahty or reduced its
cost or both. A list of the important attributes could include
1 enhanced drlveablllty and performance (in terms of power, pickup and feel),
2 enhanced vehicle dynamics (reduced noise, vibration and harshness, improved handling
and braking, and greater comfort),
3 improved duraNhty, quality, and reliability,
4 enhanced appearance (including corrosion);
5 reduced cost and effort for maintenance and repairability,
6 increased fuel economy,
7 safety considerations (improved passenger protection and reduced vehicle dam-
ageabihty),
8 product/component/materials interactions that reduced cost to manufacturer and to
customer and reduced timing of product to market;
9 design considerations (interior and exterior styhng),

l0 enhanced instrumentation,
11 product/process interactions to reduce fixed and variable costs, and
12 because a competitor had introduced a similar feature
Each category may have many different subsets that helped "push" the particular improve-
ment to market For example, a product that improves a vehicle's appearance (4) will achieve
market acceptance if it is a paint or protecting layer that reduces surface damage from envi-
ronmental corrosion or impact or both with road dust and stones.
The attributes, enhanced vehicle dnveablhty/performance (1) and fuel economy (6), are
driven by reducing component weight, improving aerodynamics, and increasing powertram/
dnvetraln efficiency In turn, this latter attribute is affected by reducing friction, use of elec-
tromc controls, etc Additional subsets for weight reduction might include Increasing a com-
ponent's mechamcal properties, so that the component can have the same rigidity, fracture
toughness, creep, and be thinner and therefore hghter The additional improvement in prop-
ertles by materials that have higher temperature and humidity resistance can be additional
drivers for change in under-the-hood components
Government can influence product design by leglslatmn. For example, emission reductions,
better material recycleabfllty, use of alternate fuels, enhanced fuel economy, and improved
safety (say by increasing capaoty to absorb energy in a crash) will promote new materials
technology
APPENDIX IIIB Process-Based Technological Change
Advances m manufacturing technology have been major drivers for materials and compo-
nents changes m the automotive industry Several important attributes include
1 enhanced manufactureablllty (the material or component can be designed more readily

for lower-cost manufactunng),
2 the new material/component has higher quality (and quality that is more easily
verifiable),
3 the process is more rehable and reproducible,
4 the components are more machinable;
5 the component can be more easily joined (by adhesives, welding, etc.);
6 the c~176 are m~ c~ f~ van~ types ~ c~
7 the product can be produced to near net shape,
8 the product can be produced in comphcated one-piece components with thin walls/
close dlmens~onal tolerances and nonuniform wall thickness,
9 the design is more suitable for mass production,
10 the process has shorter cycle times,
11 the process can increase the speed of getting the products to market, and
12 the process has reduced variable and fixed manufacturing costs.
Government can influence manufacturing processing by mandating emission reductions

and safety Improvements at the workplace through the Occupational Safety and Health
Administration (OSHA) and the National Institute for Occupational Safety and Health
(NIOSH)
References
[ 1] Pusch, R , "Hxstory of Metallography," Pracncal Metallography, Vol 16, 1979, p 294
[2] Owens, J S, Hmton, J W , Insley, R H, and Polan, M E, "Development of Ceramic Insulators for
Spark Plugs," Ceramtc Bulletm, Vol 56, No 4, 1977, p 437
[3] Wlnterbottom, W , Ford Motor Company, private commumcatlon
Robert L. Benne?
New Diamond Grinding Disks for Specimen

Surface Preparation
REFERENCE" Benner, R L , "New Diamond Grinding Disks for Specimen Surface Prepara-
tion," Metallography Past, Present, and Future (75th Anniversary Volume), ASTM STP 1165,
G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amencan Society for
Testing and Materials, Philadelphia, 1993, pp 139-154
ABSTRACT: A new multflayer abrasive gnndmg disk has been developed to overcome the
grinding and pohshmg problems associated with metallographlc speomen preparation These
problems are discussed in detail The dlscussmn focuses on the contnbutlng factors of poor spec-
imen preparation, how they affect the surface, and how they are allewated The difficulties of
surface deformation, edge rounding, soft-phase undercutting, pullout, and chipping of brittle
specimens are reviewed together w~th their root causes Th~s foundatmn was used to design a
supenor gnndlng system employing the benefits of dmmond
Micrographs of speomens prepared using conventmnal techniques are compared to that of
the new grinding system The mlcrographs illustrate that edge rounding and soft-phase under-
cutting can be Chmlnated with chipping and pullout greatly reduced Other examples show that
the new grinding system greatly improves the specimen surface fimsh and that three gnndmg
&sks of the new design can replace five or six conventmnal gnndmg and pohshmg steps
KEY WORDS: specimen gnndmg, specimen polishing, specimen undercutting, edge rounding,
surface deformation, chipping, diamond abrasives, cubic boron nitnde, metaUography, metal-
lurglcal specimens, mlcrostructure, metallographlc techniques
Surface damage of metallographlc specimens and its affect on interpretation has always
plagued metallographers T h e three m a r e contributors are
(a) dull or deteriorated abrasive particles,

(b) heat from gnndlng, which can be significant (calculations indicate temperatures of
2200~ are possible on a mlcroscale [1], and,
(c) swarf or debris that c o m e s off the specimen and the abrasive, eroding the softer phases
o f the specimen and the m o u n t i n g material This swarf ts also a prime cause of edge
rounding
With this as a background let us review s o m e typical procedures
Specimen Preparation Techniques

Conventional Preparatton
I f a typical steel specimen ~s considered, the procedure generally starts out w~th a small seg-
m e n t being cut out w~th an abraswe cut-offwheel This segment ts then m o u n t e d m a plastic
material If edge e x a m i n a t i o n is required, additmnal precauuons m a y be required such as plat-
President, TBW Industries, Inc, Furlong, PA 18925
139
Copyright
Copyright*by1993
ASTMbyInt'l
mg the surface of the piece before mounting so that the surface edge of the specimen is encap-
sulated m another metal
Once the specimen is mounted, gnnding can begin If the abrasive cut-off saw was used for
sectioning, gnndlng generally starts with a 180 (70 ~zm) grit aluminum oxide (A1203) or silicon
carbide (SIC) paper then proceeds through the 240 (54 #m), 320 (35 #m), 400 (23 #m), and
600 (17 um) grits If the s p e o m e n was cut with a hacksaw or sheared, gnnding generally starts
with an 80 (190 ~m) or 120 (115 um) grit paper and then moves on to the gnnding steps
described earlier What these finishes look like microscopically is shown in Fig 1 It shows a
progressively finer scratch pattern through the five gnndlng steps prior to polishing Evidence
of particle deterioration can be noted on the figure by the random staggered scratch patterns
in the specimen, especially for the coarser grit sizes. Th~s random scratch pattern ~s more prev-
alent when the paper is new, It subsides as the paper becomes dull. On the other hand, dull
paper causes more heat and surface deformation than new paper
In th~s example, an epoxy mount material was used and no special precautions were taken
to preserve the edge Figure 2 illustrates how the edge was affected by the gnndlng process
Figure 2a shows a scanning electron microscope (SEM) mlcrograph of the edge of the speci-
men and the adjacent mounting material Considerable undercutting of the mounting mate-
rlal and extensive edge rounding of the steel can be observed This undercutting and edge
rounding IS promoted by the turbulence of swarf and loose particles collecting at the leading
edge of the specimen As the particles travel over the surface they leave deep gouges and
grooves m the rounded edge and top surface of the s p e o m e n These grooves extend for a con-
siderable distance Figure 2b shows a mlcrograph of this rounded edge area The staggered
random pattern of the loose abrasive particles can be observed.
S~mflar scratch patterns are observed with other materials, such as the bronze spray coating
on a steel plate shown in Fig 3 In general, the softer the material, the deeper the scratch pat-
tern for a given grit size
The coarser grit sizes have reduced considerable tearing and damage in the fragile bronze
coating. This gives the appearance of a larger pore size than really exists Not all of this damage
is removed m subsequent fine grinding steps as shown in the photomicrographs of Fig 3
New System
Fundamentals--In order to understand some of the problems with conventional abrasives,
~t would be well to understand some of the fundamentals of gnndlng As previously men-
tloned, there are three major contributors to poor specimen preparation, namely, particle
deterioration, heat flow, and swarf. The first two can be alleviated by using a particle that has
good thermal conductivity and does not dull easily. In this instance, diamond and cubic boron
nltrlde (CBN) are natural selections. Figure 4 shows that the hardness of diamond and CBN
are superior to those of other abrasives. They also have a much higher thermal conductivity
than other abrasives, even metals, so that the heat flows into the abrasive particle rather than
the specimen, see F~g 5
Fixed abraswes, diamond and CBN gnndlng disks, have another property that is not shared
by other fixed abrasives This property yields an added bonus in specimen preparation Recent
studtes have shown [2,3] that the more diamond or CBN particles m contact with the speomen
the better the surface fimsh This phenomenon was noted in grinding metals and nonmetals
over a wide range of grit sizes, from 300 ~m down to 45 #m, and using a wide range of bond
types including resin, metal, and wtreous bonds F~gure 6 shows that increasing the volume
percent of d m m o n d particles m an impregnated resin bond, improves the surface finish of
material. Part of this improvement is because the greater the number particles m contact w~th
the surface, the less pressure exerted by any one particle Naturally, as the volume of diamond
BENNER ON DIAMOND GRINDING DISKS 141
i
rT
L~
4~
FIG. 4--Knoop hardness ~f diamond and CBN compared to that of other abrasives.
FIG. 5 - - l'hermal conductivity ~f varimts materials and the effect on heat[low in diamond as compared
to aluminum
Copyright by ASTMoxide.Int'l (all rights reserved); Thu Dec 29 00:42:12 EST 2011
BENNER ON DIAMOND GRINDINGDISKS 145
cO
ill
2533
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tL. 0.7 ................................................................ .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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0.4 5.0% 10.0% 12.5% 15.0% 20.0% 25.0%

VOLUME PERCENT DIAMOND IN DISK
FIG. 6--Surlktce.[inish versus volume percent diamond in a resin bond and calculated number of par-
ticles per unit area protruding from the bond Surface.
FIG. 7--Development of particle protrusion during grinding.
increases m the bond, the number of dmmond parhcles m contact with the surface increases
As the particles get closer together, there is less chance for bond erosion m between the particles
and they do not protrude from the bond as much This is dlustrated schematically m Fzg 7
Consider a row of diamond particles m a metal or resin bond as shown m Fig 7a As the bond
~s worn away by the swarf coming off the specimen, a long support or "tall" develops in the
back, or trading edge, of the abrasive particle At the same time, the front and sides of the
particle protrude from the bond more as shown in Fig 7b This protrusion (E), the number
of particles, and the pressure apphed to the specimen, control the depth of the cut or scratch
pattern in the specimen The diamond particles that are far apart develop extensive protrusion
on the front and sides as shown m Fig 8 Here the sides and front are well protruded and with
httle effort the particle can pull out of the bond leaving a hole s~mdar to that shown in Fig 9
This pullout shortens the life of the grinding disk
If the number of particles is increased, as shown in F~g 7c, the undercutting and protrusion
(e) ~s decreased With the decreased protrusion and greater number of particles, the particles
do not cut as deep and the surface finish is better.
It would be very expensive to increase the volume of dmmond m a gnndmg &sk that has
slgmficant depth of diamond If however, the particles are consohdated into a three-&men-
s~onal honeycomb network, such as dlustrated in F~g 10, the effectiveness of the particles can
be maximized This type of structure offers a continuing supply of diamond for grinding As
FIG 8 - - S E M photo,graph o / d i a m o n d protru ston m metal bond
F I G 9 - - S E M pholoy(raph o{ empt~ socket/e/t by dlamond pullout /rom a metal bond
FIG 1O--Method o[ ~on~ entratmg dtamond
one layer is worn away other layers come to the surface to continue the grinding Unhke abra-
sive papers, the third dimension of diamond depth increases the hfe of the product slgmficantly
so that ~t can replace thousands of paper disks
This type of consohdatlon has other advantages The empty spaces within the honeycomb
offer a place for the s p e o m e n swarfto collect This addresses the last major source of specimen
preparation problems The holes also carry coolant across the entire surface of the s p e o m e n
at all times The absence of mterfenng swarfallows the hard d~amond parhcles to do all of the
gnndmg, thus reducing the undercutting of soft phases It also offers full-time cooling to the
speomen, reducing still further the potentml for thermal damage
Results
If the same steel specimen is prepared using the new technique, the sectioning procedure is
the same as for the abrasive paper technique At this point, the new system is simpler No
speoal edge preservatxon techniques are required because undercutting does not occur The
grinding begins with a 200-grit (68-urn) gnndlng disk of the new configuration This is then
followed by a 30-um disk and a 12-em disk, both of the new configuration This is illustrated
in the photomicrographs as shown in Fig 11 When Fig 11 is compared with Fig 1 at equiv-
alent abrasive particle size, a dramatic difference is noted It will be shown later that the final
step in the new system is equivalent to a polish step
Figure 12 shows a scanning electron microscope mlcrograph of the edge of the specimen
and the adjacent epoxy mounting material, using the new system and an equivalent grit size
to the SiC grit used m Fig 2a A dramatic difference is noted between the two fgures. With
the new method, virtually no undercutting is observed The scratch pattern is much finer and
the gouging has been virtually ehmlnated Figure 12b shows that the edge is fiat with virtually
no edge rounding
Figure 13 shows a comparison of scratch patterns produced by 17-um SIC papers, a 12-um
diamond disk o f the new system and a 3-~m diamond paste on a medium nap c o t t o n cloth
In this case, the steel specimens show marked differences in the depth and width of the
scratches produced by the different abrasives
Figure 13 illustrates that the surface fimsh from a 12-~m dmmond gnndmg disk of the new
system gives a finer scratch pattern than other S~C fixed abrasive disks of comparable particle
size as well as 3-urn pohshmg pastes on cotton cloth. The printed orcult (PC) board, shown in
Fig. 13, illustrates that the new diamond grinding disk yields excellent definmon of the glass
fibers encapsulated by the copper plate The 3-~m d m m o n d pohshmg cloth, on the other hand,
seemed to undercut the soft phases of the solder A comparison of the bronze spray-coated
specimens, pohshed with 3-#m diamond paste on cloth, shows areas where bronze particles
were removed in prior grinding steps, whereas, the new 12-um diamond disk shows almost
none of this
Figure 13 illustrates that the new system is apphcable to a wide range of materials from
bronze coatings to steel or PC boards In this instance, the specimens were not rotated so that
the scratch pattern would be unidirectional In each case, the observed pattern from the new
system is better than a 3-urn diamond pohsh paste on cotton cloth
When the results of Fig 1, 11, and 13 are compared, it is obvious that the three disks of the
new system can replace easily five S1C grinding disks and the rough pohshmg step of the stan-
dard procedure, as shown in Fig. 14 Speomens were flatter, with no edge rounding, as shown
in Fig 12 Comparing Figs 3 and t3 also shows that they do not cause pore distortion in
porous materials such as the spray-coated bronze
BENNER ON DIAMOND GRINDING DISKS 1 51
FIG. 13--Comparison o f scratch patterns made with 17-#m SiC papers, 3-#m diamond paste on cotton
cloth, and 12-um new diamond disk on printed circuit board, low-carbon steel, and bronze spray coating
(um;tched).
Special Problems of Ceramics and Mixed-Phase Specimens

Preparation of ceramic specimens presents a special set of problems. Because of their brittle
nature, chipping and spalling is often encountered. The reasons for this are many and varied.
Most chipping is a result of compressive stresses induced on the surface of the specimen by the
abrasive particles. In many cases, the particles act like a moving indenter that causes a stressed
area on the surface creating cracks parallel to the stress direction. As the particle moves by,
cracks perpendicular to the stress develop giving rise to a series of concoldal chips forming
behind the particle These chips leave a trench much wider than the abrasive particle From a
materials removal standpoint, this is good because the rate of removal is high From a surface
fimsh standpoint, however, it is detrimental because the surface becomes irregular and
chipped
If the n u m b e r of particles in contact with the specimen surface is increased, then the stress
induced by each particle Is reduced and chipping is reduced A good example of this is shown
in Fig 15 that compares a glass-to-metal seal, ground with a standard SIC paper disk and with
a honeycomb resin bond diamond disk with a comparable particle size Figure 15 shows the
FIG 15--SEMphotograph~ comparing a glass to rnetal seal ground wuh (a) StC papers and(b) a new
dtamond grmdmg dl~k o/ ~omparable grtt stze
specimen after grinding to a 17-um SIC The figure shows a relatively deep scratch pattern in
the metal and some ch~ppmg m the glass section The glass/metal interface presents a special
problem because of the large difference in thermal coefficients of expansion Figure 15a shows
that a considerable a m o u n t of chipping has occurred at the interface This is probably brought
about by the heat generated d u n n g the gnndmg process The heat causes the surface of the
metal to expand quicker than the glass The sudden expansion of the metal m relation to the
glass causes considerable strain m the glass, which in turn, fractures the glass at the interface
Figure 15b shows the same specimen after grinding with the new resin-bonded diamond disks
A much finer scratch pattern is apparent on the metal and less chipping is present in the glass
More importantly, there is no chipping at the interface With the new method, there is less
heat generated, less d~fference in thermal expansion, and less mterfaclal chipping
Summary
By consolidating closely packed diamond particles into a three-dimensional honeycomb
structure, one obtains an abraswe d~sk that yields a superior finish to conventional abrasives
This reduces speomen preparation time considerably Its unique design allows one to g n n d
and polish speomens flatter with reduced mechamcal and thermal damage and edge rounding
In many cases, it will produce a surface eqmvalent to a 3-#m diamond paste and cloth polish
that is ready for a final pohshmg ff required by the application
A patent [4] has been recently granted on the concept, and the disks have been used suc-
cessfully in s p e o m e n preparation of a variety of materials Including metal coatings, barium
titanate capacitors, turbine engine parts, and carbides
References
[1] Snoeys, R, Leuven, K U, Maris, M, Wo, N F, and Peters, J, "Thermally Induced Damage m
Grinding," Grmdmg Theory, Techntques, and Trouble~hootmg, R P Llndsay and C P Bhateja, Eds,
Society of Manufacturing Engineers, Dearborn, MI, 1982, pp 206-216
[2] Wapler, H and Juchem, H O, "Diamond Abrasives for Machining Glass," Industrial Dtamond
Revtew, Vol 47, No 521, April 1987, pp 159-162
[3] Cooley, B A and Wapler, H, "Surface Finish when Gnndlng with CBN Abrasives," Industrial Dta-
mondRevtew, Vol 44, No 502, March 1984, pp 147-150
[4] U S Patent No 4,882,878 Gnndmg Wheel, 28 Nov 1989
N a t a h o T. S a e n z ~
Advancements in Ultrathin Section

Techniques for the Characterization of Brittle
Materials
REFERENCE. Saenz, N T, "Advancements in Ultrathin Section Techniques for the Charac-
terization of Brittle Materials," Metallography Past, Present, and Future (75th Anmversary Vol-
ume),ASTMSTPlI65, G F VanderVoort, F J Warmuth, S M Purdy, andA Szlrmae, Eds,
American Society for Testing and Materials, Phdadelphla, 1993, pp 155-166
ABSTRACT The use of ultrathm sections, on the order of'/. to V.,the thickness ofconventmnal
30-um thin secUons, consmutes a slgmficant advancement m the charactenzanon of brittle
matermls At a t~mewhen greater emphas~s~sbeing placed on optimum resoluUonand mterfacml
characterization of brittle materials, this approach makes possible a whole new order of optical
access to m~crostructural detad W~ththe evolution of~mproved mounting medm and pohshlng
eqmpment, ultrathln sectmmng techmques have also improved to produce sectmns that reduce
preparation time and operator dependence Preparatmn methods and examples of matenals
exammatmn using th~stechmque will be discussed
KEY WORDS ultrathln sections, metallographlc techmques, ceramics, ceramic composites,

rock and minerals, transmitted light microscopy, metallurgical specimens, m~crostructure,
metallography
The geologist and the metallographer have long used dlffenng sample preparation methods
because of the differences between the materials they study The brittle, elastic nature of most
minerals has allowed the geologist to prepare secnons under conditions that would be unthink-
ably abusive to the metallographer However, as one goes substantially below the traditional
30-urn thin section or seeks artifact-free, highly polished surfaces for reflected light examlna-
non, the most careful methods of the metallographer are definitely required, and traditional
petrography techniques are no longer adequate
Since the entire technology of petrography has centered around the 30-urn thin section for
well over 100 years, basic thin secnon sample preparation techmques have changed little dur-
ing that time Basically, 30-um-thlck petrographic thin sections have been prepared by free
abrasive grinding on thick glass plates using mechanical or manual laps while the matenal is
secured to glass slides with transparent balsam Upon completion of the thin section, a cover
slip is placed on the upper surface of the section to reduce the scattenng of light during exam-
marion ofthe thin secUon [1] Mineral constituents are identifiable partly because ofthelr crys-
talhne morphology and by their behavior under transmitted polarized hght The characteristic
interference colors ofa gwen matenal in a standard 30-um thin secUon is an tmportant feature
m convennonal petrography These colors, and the way in which they shift with the insertion
of polarizing filters, constitute mineral identification for vanous materials The science of min-
eral identification with the use of conventional thin sections, including all training and all text
book resource materials, are budt on the 30-urn thin sectmn techmques
Senior techmcal speclahst, Pacific Northwest Laboratory, Rlchland, WA 99352
155
Copyright
Copyrightby1993
9 ASTM Int'l (all rights reserved); Thu Dec 29 00:42:12 EST 2011
by ASTM International www.astm.org
Optical petrography, as traditionally practiced, has suffered from two basic deficiencies the
unpolished surfaces are not suitable for study by reflective light techniques, which limit optical
methods, and the relatively great specimen thickness of 30 ~m leads to opacity and poor res-
olution Earlier efforts were made to produce thicknesses below the standard norm, but those
efforts have generally proven unsuccessful because of poor adhesive performance, inadequate
surface preparation techniques, excessive stresses causing material pullout during the prepa-
ration steps, or a combination of all these factors Since the mid 1940s, refinements have
occurred in the preparation of thin sections G C Kennedy [2] produced and reported pol-
ished sections of conventional thickness roughly 100 years after the beginning of petrography
Refinements in microscopy and improvements in abrasives and preparation equipment have
also occurred Improvements in adhesive materials, premlxed and graded diamond abrasives,
lapping materials, and the evolution of the universal microscope have all combined to produce
an Increasing interest in polished thin sections
The use of the pohshed sections, mixed-mode illumination, and other minor refinements
to the 30-um standard thin section are of increasing interest The next natural step in the evo-
lution of the thin section was to produce sections below the standard 30-t~m limit Within the
past 20 years, R H Beauchamp [3] pioneered ultrathln section techniques for application to
brittle materials, such as lunar basalts and brecclas The sections, on the order of ~,, to V~the
thickness of standard 30-t~m thin sections, make possible essentially new levels of sophistica-
tion in the examination of brittle materials The intent of this paper IS to describe ultrathln
section techmques and to illustrate the wealth of information obtained through microscopic
analysis of brittle materials using this technique
First-Side Preparation Techniques

Sample material is sectioned and mounted with resin The first side is prepared by planar
grinding and vibratory polishing
Secttomng and Cast-Mounting

Sectioning is the first critical step in prepanng brittle materials for ultrathln section tech-
niques Its main function is to reduce the parent material to a smaller workable piece with
m i n i m u m deformation When prepanng ultrathln sections of brittle and fragile materials, it
is important that the pores in the material be impregnated with a low-viscosity thermosetting
resin before the material is sectioned This encapsulation step ensures that no sample degra-
dation, such as fracturing or plucking, occurs during the wafer sectioning process, it also
enhances the ability to produce thinner wafers The smaller section of material is then
mounted in the same type of epoxy resin and vacuum impregnated After the resin 1s hard-
ened, thin wafers of less than 0 6 cm thickness are sectioned from the resin-mounted material
Whenever possible, sectioning of the material should be done using a slow speed (300 to 500
rpm) cut-offsaw with a diamond wafering blade, using oll as the lubricant The sides of the cut
wafer are ground down with the use of a belt surfacer, placing the square wafer into a specimen
casting mold, as shown in Fig l The smaller section or wafer of material is then remounted
in epoxy resin and vacuum impregnated, partially filling the casting mold with the resin While
the specimens are being vacuum Impregnated, an alumina powder is added to the remaining
epoxy resin and stirred until a homogeneous mixture is achieved.
When the epoxy resin in the specimen casting mold has a minimal amount of outgasslng,
the alumina-loaded resin is used to finish filling the specimen casting mold The reason alu-
mina filler is added to the casting mold is that it serves as a guide for any specimen wedging
(nonparallel planes) and a thickness indicator d u n n g the thinning process An example of a
metallographlc m o u n t is shown m Fig 2
SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 157
FIG. 1--Sectioned specimen wqfi,r in casting mount.
Planar Grinding
The mounted metallographic samples are rough ground on an oil-cooled 125-urn diamond
planar grinding disk until the surface of the material covered by resin is exposed. It is impor-
tant not to grind too deep into the specimen; the grinding should stay within the depth of the
resin impregnation zone of the material being polished. The thickness of the resin impregna-
tion zone is dependent on the amount of porosity present in the material being polished. Vac-
uum impregnation causes the resin to flow within the interconnecting pores of the material,
FIG. 2--Metallographic sample mounts with alumina filler.

helping to reduce any pullout or plucking of the matenal during this aggressive gnndlng step
The decision to use either water or oil as the coolant depends on the water reactivity of the
mlcrostructural constituents of the specimen being polished The mounted samples are then
hand-lapped using an oil-based coolant on a 30-#m diamond planar grmdlng disk with wheel
speed of approximately 300 rpm, malntmnlng medium-to-heavy uniform pressure until all
gnnding scratches from the previous step have been removed. After each grinding step, the
mounted samples should be thoroughly cleaned to prevent contamination from the previous
step The mounted samples are then placed in a pohshlng weight assembly, shown in Fig 3
Vibratory Pohshmg
The mounted samples are polished with vibratory polishing equipment using a combination
of polishing slurries and polishing cloths that maintain surface flatness and artifact-free sam-
ples The use of diamond polishing abrasives IS indispensable for the preparation of ultrathln
sections The polishing rates using diamond abrasives are equal to, or better than, other pol-
ishing abrasives The type ofpohshlng cloth used has an extremely important beanng on the
finished s p e o m e n Napless polishing cloths should be used when rehefbetween the microcon-
stltuents of varying hardness and sample mount interfaces are to be held to a minimum Some
examples of napless pohshmg cloths are nylon, pellon, stainless steel mesh, and silk
Vibratory polishing is an effective polishing technique for thinning brittle, fragile materials
Resin-mounted samples are placed in weight assemblies, face down on the pohshing cloth
Inertia from the sample weight produces movement, which induces polishing Since the
removal rate of material is low, several hours ofpohshlng may be reqmred With the selection
of all these elements, the combination ofpohshmg cloth, abrasive slurry, and vibratory motion
gently pohshes the sample surface, slowly removing material, creating very little thermal or
mechanical shear loading of the material being studied
The first vibratory pohshmg step involves the use of 1-#m diamond abrasives using an oil-
based carrier slurry on a stainless steel mesh polishing cloth This combination of polishing
m e d m m and cloth produces samples with excellent interfaclal flatness between the mlcrocon-
stltuents as well as excellent edge retention The amount o f time involved m this rough pol-
ishing or flattening step depends on the hardness vanatlons within the specimen being pol-
FIG 3--Ftr~t-~tdepohshmg wetghtassemblyfor vtbratorypohshlng
lshed, 4 h is typical The fine pohshmg step consists of using 1-um diamond abrasives in an
off-based slurry on a synthetic napless pohshmg cloth Again, the time depends on the removal
rate of the material being studied, approximately 12 h of polishing time is required to remove
any artifacts
After the examination of the mounted specimen for any type of surface defects, the mounted
specimen can be prepared for transfer to a petrographic slide for preparation of the second side
Second-Side Preparation Techniques

The second side of the specimen is prepared by mounting a 2 to 3-mm-thick wafer on a glass
shde and mechanically thinning the exposed side
M o u n t i n g on Glass Shde
Upon completion of the first side of the specimen and m~croscopic examination of the sam-
ple, the polished m o u n t is placed in an abrasive cutter and a thin wafer IS sectioned from the
mount, parallel to the polished surface The thickness of the cut wafer is very important and
should be on the order of 2 to 3 m m in thickness to ensure satisfactory gluing to the petro-
graphic well slide The polished thin disk m o u n t is then belt-surfaced into a rectangular-shaped
wafer with an alumina ring around the outer edge of the wafer so that the resultant polished
wafer will fit within the well area on the petrographic well slide
The rectangular-shaped wafer is then placed, polished side up, into a casting mold The pol-
ished wafer is recast using the same type of epoxy resin as used in earlier steps, again partially
filhng the casting m o u n t After the resin-filled wafer is heated and vacuum impregnated, the
resin-filled wafer is removed from the casting mold and is placed with the polished side of the
wafer down on the glass slide, contacting the glass well surface of the petrographic well slide
The wafer ~sworked around to remove any mr bubbles trapped between the wafer and the glass
shde because air trapped m the section, or m the wafer/glass interface would cause a debond
area at the glue line, which could cause plucking or pullout of material in later steps of the
process The mounted slide is oven-cured to allow the resin to set The glass mounting pro-
cedure is shown in Fig 4
FIG 4--Step~ [or se~ond-stde thmnmg pohshed wafer, waJer mounted on gla.s s shde, and )~mshed ultra-
lhgn ~er
Planar Grmdmg
Thin-section fixturing is not used by the author dunng the grinding process, the initial grind-
lng operation is done with the glass shde held d~rectly in the preparator's finger tips This tech-
tuque requires a good deal of dexterity to prevent grinding of the preparator's finger Ups along
with the section If more substantmi fixturing is desired, various metallographlc vendors pro-
vide different types of thin-section fixtures. Standard clamp-type slide holders should be
avoided because they impose undue stresses on the mounted glass shde
The first step m the grinding process is the use of a 125-urn diamond planar gnnding disk
using an od coolant, gnndmg until light can be seen through the alumina filler around the
sectnon Examination of the alumina filler can signal any wedging of the section The alumina
filler should have the same color thickness around the section (no hght or dark areas), so great
care must be taken d u n n g th~s aggresswe grinding step The thin section may be taken to a
thickness of 50 um on th~s first grinding step An additional 10 to 20 ~m can be removed with
the use of a thin-section grinder This step 1s optional, depending on the avadabihty of this
specmhzed piece o f e q m p m e n t Lapping continues by hand through 30-#m diamond wheels,
again with the use of an od coolant, until all scratches from the previous grinding step are
removed The alumina filler around the specimen is highly translucent at this point, again
looking at the color thickness of the alumina filler as an indicator for any wedging of the sam-
ple. After the grinding process is complete, and the thin section has been cleaned thoroughly,
the shde is placed into a pohshmg weight assembly for the vibratory pohshmg step, shown m
Fig 5
Vtbratory Pohshlng
The mechanical thinning process is continued with the use of vibratory polishing equip-
ment, again using an oil-dispersed diamond slurry of 1-urn particle size on a synthetic napless
polishing cloth The pohshmg time vanes, depending on the hardness of the material. During
this process, the ultrathin section must be respected periodically to ensure that the section
FIG 5--Second-~tdepohshlng wetghtassembly wtthmountedglassshdes
SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 1 61
is pohshlng evenly and has not been pohshed through The difference between an ultrathm
section (under lO um) and no sectmn is slight. The use of the Michel-Levy Interference
Color Chart is a valuable aid when examining polished ultrathln sections with the micro-
scope because it graphically relates thickness, blrefrlngence, and retardatmn of trans-
parent materials
Results
Characterization of brittle materials using ultrathm section techniques presents a new level
of clarity and resolution to the optical microscopist Since a section is pohshed on both sides
or surfaces of the material, it can be examined using a full range of reflected and transmitted
light methods
Figures 6 through 9 show examples of ultrathm section techniques using a wide variety of
materials.
Figure 6 is a direct comparison of a standard thin sectmn (Fig 6a) with an ultrathm section
(Fig 6b) of tin oxide electrode material. The photomicrograph shown m Fig 6a illustrates the
unsuitability of the standard 30-#m thin section for resolving needed mlcrostructural refor-
mation Figure 6b illustrates the resolution of individual grains, their boundary relationships,
and twinning habits of this material.
Figure 7 illustrates very clearly the fine detail and complex microstructure ofchondrules m
stony meteorites. The photomicrographs are from the Dhajala meteorite showing loosely
bound chondrules with well-preserved, cleary-uneqmhbrated mlcrostructures
Figure 8 shows the complex range of minerals, textures, and the scale of m~crostructural
details In terrestrial mineralogical studies The photomicrographs of the minerals aphte and
graphic schist demonstrate clear dehneatlon of individual grains and their characteristics mak-
ing mineral ~dentlficaUon an easier task
Figure 9 shows the mlcrostructural detail of silicon-carbon/silicon-carbon (SIC/SIC) fiber
composites prepared by the chemical vapor induction (CVI) process Growth of the SIC matnx
from the black SIC fibers dunng infiltration reveals impingement interfaces of this material
that can be seen only by transmission light microscopy
Conclusions
The advantages of ultrathin sections are that much greater resolution is avadable to the
microscopist, and that regions of the material that may be opaque m thicker 30-#m sections
can be illuminated and examined The gain m clarity is illustrated m Fig. 6 It is apparent that
the standard thin section of tin oxide electrode material provides very little information while
the ultrathln section reveals grain relationships, twinning, and a small amount of porosity The
improvement m clanty results from thinning the section of matenal to a monolayer of grains
This eliminates the overlapping diffraction patterns of stacked, small grams, which obscure
structure m the standard 30-#m thin section Because the ultrathln secUon ehmmates the scat-
terlng ofhght that occurs in a standard thin section, it is well suited for the application of newer
microscopic techniques, such as Nomarskl differential interference contrast (DIC) Such
methods are most powerful m providing apparent rehefbecause small refractive index differ-
ences build contrast m some difficult objects.
The ultrathln section technique described here is one of many analytical tools for the char-
actenzation of brittle matenals The technique given m this paper should help overcome major
obstacles m the preparation of bnttle matenals for m~croscopIc examination.
~3
I
L~
t~
Acknowledgment
The Pacific Northwest Laboratory ~soperated for the U S Department of Energy by Battelle
Memorial Institute under Contract DE-AC06-76RLO 1830
References
[1] Kerr, P F, OpttcalMmeralogy, McGraw-HallCo, New York, 1977
[2] Kennedy, G C, "The Preparation of Pohshed Thin Sections," Economw Geology and the Bulk,tin of
the Socwty ofEconontc Geologtsts, Vol 41, 1946, pp 353-360
[3] Beauchamp, R H and Wdhford, J F, "Metallograph~cMethods Apphed to Ultrathmnmgof Lunar
Rock, Meteorites, Fossds and Other Brittle Materials for Ophcal Microscopy," Metagographlc Spec-
Imen Preparation, Plenum Press, New York, 1974
M i c h a e l R. Notis, ~A r n o l d R. Marder, ~ a n d Ye T Chou ~
The Early Metallographic Studies of Chih-

Hung Chou on the Formation and Morphology
of Widmanstatten Structure and Martensite
REFERENCE" Notls, M R, Marder, A R., and Chou, Y T , "The Early Metallographic Stud-
les of Chih-Hung Chou on the Formation and Morphology of Widmanstatten Structure and Mar-
tensite," Metallography Past, Present, and Future (75th Anntversary Volume), ASTM STP
1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szwmae, Eds, American Society
for Testing and Materials, Phdadelphm, 1993, pp 167-173
ABSTRACT: One of the early studies concerning the detaded mtcrostructural aspects of phase
transformatmns m ~ron-carbon alloys was performed by Ch~h-Hung Chou (Ph D, Harvard,
1928), a student of Professor Albert Sauveur The research describes the formatmn of W~dman-
statten structure and martenslte m ~ron-carbon alloys possessing a broad range of carbon con-
tents and heat treated using a broad range ofcoohng rates A umque mercury quench method ~s
descnbed This research work was never fully pubhshed
The present paper shows original photomicrographs and portmns of the written text from the
dlssertatmn, and seeks to clanfy and reinterpret these m terms of our present understanding of
ferrous phase transformatmns Also included zs the background h~story of the introduction of
modern industry and science In China, and Chou's personal reminiscences of Professor Sauveur
KEY WORDS: metallography, history, won-carbon alloys, martenslte, Wldmanstatten struc-

tures, surface rehef, metallurgical specimens, mlcrostructure, metallograph~ctechmques
In 1872, the first yearly group of 30 students was sent from China to study science m the
Umted States With the establishment of the Chinese Repubhc in 1911, the Chinese reahzed
the importance of modern science and technology m nation building In 1914, the Chinese
Society of Science (Zhong Guo Ke Xue Sh0 was founded, with its inaugural meeting held in
1915 at Cornell University, members came predominantly from Andover, Carnegie Institute
of Technology (now Carnegie-Mellon Umverslty), Columbia, Cornell, Harvard, Lehigh,
Princeton, Wflhston, and Yale Among these students was a semor m Chemical Engmeenng
from Lehigh, Chin Wong, who was soon to return to China to set up the first laboratory for
modern quantitative analytmal chemistry m China, at the Nanking H~gher Normal School,
now Nanking Umverstty Among his research interests was the analys~s of ~mpunt~es m cast
bronze alloys used for coinage In the early 1920s, he was a founder and &rectlng e&tor of the
journal, K e X u e (Sctence), and in 1928 he became the first &rector of the Natmnal Institute of
Chemistry (Academ~ca Smlca) Chin Wong, known as the father of modern chemistry m
China, was therefore an lnfluentml figure m the Intellectual circles that promoted the idea of
saving China through the development of modern industry and science
Among the young men that Chin Wong in turn influenced to study in the Umted States was
Chlh-Hung Chou, who graduated m 1923 from the Metallurgy Department of Belyang Unl-
vers,ty m Tianjen Chou strongly beheved that ff people m China could master the field of
' Department of Martenals Science and Engmeenng, Lehigh Umvers~ty,Bethlehem, PA 18015-3195
167
Copyright
Copyrightby1993
metallurgical science, then China would give rise to a modern steel industry that would greatly
aid its industrial development As it turned out, Chou was the only member of his graduating
class of 16 (five in metallurgy, eleven in mining), who continued in his field He was helped by
Professor Edwin Sperry, an Amencan, who was his department head in Belyang University,
to obtain a two-year work-study position in the South Chicago Steel Works In 1925 he
enrolled in the Graduate School of Carnegie Institute of Technology where he received a mas-
ter's degree m metallurgy in 1926 His research thesis, on medium carbon manganese steel,
won h~m a dtploma "with distinction," and for which he received the attention of Albert Sau-
veur, a professor at Harvard who had come to Carnegie to give a seminar lecture Chou was
recrmted by Sauveur and was admitted to graduate school at Harvard In verbal reminiscence,
Chou remembers his advisor, Professor Sauveur, as a good teacher who was always cordial,
patient, and listened to his student's ideas. The graduate students in his group (R F Mehl, C
R. Wohman, R Luter, and D. C Lee) would meet each week and everyone would present
their work for discussion and suggestion He was also concerned with their personal life and
well being, especially of his foreign students.
After two years, by mid-1928, Chou had completed a two-volume dissertation [1]. In fact,
Sauveur had recommended him to receive his Ph.D. after one year (research on the effect of
different cooling rates on the formation of Widmanstatten structure in sub-eutectold steels),
but this was not granted, as no one had ever completed a Ph.D at Harvard in one year Chou
subsequently completed a second volume (research on Wldmanstatten-hke structure in rap-
idly quenched pure iron), which will be the focus of much of the remainder of this paper
J. Gordon Parr, in a paper entitled, "The Criterion of the Martenslte Transformation," pre-
sented at the Sorby Centennial Symposium on the History of Metallurgy [2], ascnbes the ear-
hest descnptlon of shape change in martensite to Dumas [3], who, in 1905, descnbed the sur-
face rehef that was observed when a polished sample of nickel steel was rapidly cooled The
portions that "have been transformed project above the onglnal surface, they are those which
have passed into the c o n d m o n of martensite." An earlier observation of such a surface effect
was recorded and illustrated by Osmund in a paper published in 1901 [4] Parr further points
out that, with the exception of the work of Sauveur and Chou [5] in 1929, the characteristic
of surface relief in martensite was apparently forgotten between its early mention up to more
recent studies near mid-century Parr also notes that although the observation of surface rum-
phng had been made by Sauveur and Chou, httle importance was attached to it We have had
the opportumty to examme Chou's onginal Ph D thesis, m addition to the pubhshed paper,
and would like to share some of the contents here
Dr C H Chou studied the allotropic transformation in pure Iron His objective was to
prove that his mentor and adviser at Harvard, Professor Albert Sauveur, was correct m describ-
ing that allotroplc transformation of iron as follows [6]
On coohng through the point A3, at about 900~ iron passes from the gamma condmon to a new
allotrop~c form generally desagnated as alpha Th~stransformation, however, ~s not instantaneous
There are good reasons for behewng that it begins at the gram boundanesalong the octahedral planes
of the crystals and that at progresses untd each gram of gamma iron ~schanged into a gram of alpha
aron, the resulting structure being s~mdar to that of gamma ~ron Were ~t possible to retam at room
temperature pure ~ron but partmlly transformed, at seems probable that a w~dmanstatten structure,
or rather, as later explained, a martensmc structure would be observed, consisting of alpha aron at
the gram boundaries and at the octahedral planes, and ofa groundmass of gamma iron
In order to confirm Sauveur's hypothesis, Chou developed several innovative experimental

techmques, combined with exceptional metallography, to document the transformation.
Using a vacuum etching technique, Chou placed polished samples of electrolytic iron in evac-
NOTIS ET AL. ON EARLY METALLOGRAPHIC STUDIES 169
uated quartz tubes heated to 1000*C for 2 h and quenched. The results (Fig. 1) show the prior
austenite grain structure that was attributed "to iron volatizing at the grain boundary" [5].
Convinced that iced brine and liquid air were not efficient quench media, he developed an
elaborate method to quench the quartz capsules in mercury. As a result, the quench severity
was vastly improved and what was referred to as the allotropic transformation was clearly
revealed (Fig. 2).
Although Sauveur and Chou left no doubt that they were observing a martensitic/Widman-
statten transformation, they nevertheless mistakenly referred to this transformation as being
allotropic. It was not until 1964, some 36 years later, that Bilby and Parr [ 7] were able to show
the effect of cooling rate on the transformation mode in pure iron.
Chou clearly revealed the surface relief accompanying the martensitic transformation (Fig.
3). He went on to study the effect of carbon on the ability to form martensite and was able to
conclude that increased carbon content and faster quench rate more easily produced the mar-
tensitic structure. On polishing from the surface inward, he was able to show that as the quench
rate decreased the martensite gave way to Widmanstatten and eventually to equiaxed alpha.
Chou was one of the first investigators to recognize that martensite was similar to Widman-
statten in that it formed along octahedral planes (Fig. 4). In the next decade, these results led
to the important crystallographic martensite studies of Kurdjumov and Sachs [8], Nishiyama
[9], and Greninger and Troiano [10].
Finally, recognizing that this low-carbon martensitic structure was unique, Chou labeled it
"Sauveurite," in honor of his mentor. Although the name did not catch on, it became part of
the long list of names for low-carbon martensite including: schiebung, self-accommodating,
cell, massive martensite, needlelike, dislocation, lath, unidirectional, Type I, and packet mar-
tensite [11]. Clearly, the advances made by Chou in 1928 on the study of martensite were great
FIG. 1--Vacuum etching of electrolytic iron.
FIG 2--Structure of ele6trolytlc iron alter mercury, quenching
and his efforts encouraged the numerous investigations on martenslte in the coming
generations
In the fall of 1929, at age 32, Dr Chlh-Hung Chou returned to the turmod of Kuomlntang,
China, to work at the Shanghal Steel Works where he rapidly moved up to become director.
Starting in 1949, he also simultaneously taught at both Datong Umverslty (where he became
professor and department head) and Shanghai Jlao Tong University (where he became pro-
fessor and vice president) He became associate chief advisor to the Baoshan Iron and Steel
Complex, a modern integrated basic oxygen furnace (BOF) steel plant that started operation
in 1985 In his teaching and research, Professor Chou always stressed the importance of the
study o f phase transformations and the use o f metallographlc techniques At Jiao Tong Uni-
versity, he organized a complete metallographlc laboratory using eqmpment bmlt almost
entirely by his students. For example, he had a graduate student, Longyuan Xu, and a young
teacher, Yongpel Xle, construct a h~gh-temperature metallographlc microscope In the very
late 1970s and early 1980s, when the first groups of American visitors were able to come to
Jlao Tong Umverslty, we all marveled at the mvenhveness demonstrated m this laboratory
Professor Chou realized that in the history of the development of science and technology, qmte
a number of critical invenUons and discoveries were made with the help of a specific experi-
mental instrument or apparatus It was because of this concept that Professor Chou had built
the first high-temperature metallographic microscope in China With it, he and subsequent
workers were able to study the growth rate of WIdmanstatten plates in hypoeutectold steels
and the kinetics of bainitic transformations This work led to the conclusion that the maxi-
m u m growth rate appears after austenltizmg at certain temperatures, and that there is a peak
growth rate corresponding to the incubation period These observations were among the ear-
NOTIS ET AL ON EARLY METALLOGRAPHIC STUDIES 171
FIG 3--Rehel ~flect of the martenslttc structure (a)fi~cus on valleys and (b) locus on ridges
hest international studies that demonstrated that the Wldmanstatten structure, being coherent
with the matrix, proceeds by dlffusional transformation
In 1985, m Its inaugural issue, the Journal ofChmese Htstory of Sctence and Technology of
Academlca Slmca honored Professor Chou's 70 years as a metallurgist with a rewew article
concerning his professional contributions [ 12] Professor Chou was regarded as the founder of
FIG. 4--Octahedral traces in martensite.
modern metallurgy in China, just as his Ph.D. advisor, Albert Sauveur, is considered one of
the fathers of modern metallurgy in the United States.
Chih-Hung Chou was born on 28 December 1897 in Yangzhou, Jiansu Province. Professor
Chou passed away peacefully on 13 February 1991, in Shanghai, at the age of 94. He was loved
by all who knew him; relatives, friends, students, and colleagues all around the world. As a
young student, Chih-Hung Chou must surely have studied the photomicrographs of Henry
Clifton Sorby. As his legacy, Dr. Chou produced one of the most beautiful and thorough
metallographic studies to be found. If a picture is worth a thousand words, and if metallogra-
phy is the metallurgist's universal language, then Chou's thesis is truly encyclopedic and his
metallographic research represents an enduring gift to materials science throughout the world.
As a post script, the special relationships between Lehigh University (started through Chin
Wong) and Jiao Tong University (through Chih-Hung Chou) still continues. His son, Ye T.
Chou, is a professor in the Department of Materials Science and Engineering at Lehigh~ Many
of the faculty at Lehigh, including the present authors, have had the opportunity to visit Jiao
Tong, or to meet Professor Chih-Hung Chou when he visited at Lehigh. A number of under-
graduate students from Jiao Tong University have been graduate students or visitors at Lehigh,
and a few have returned to become faculty members at Jiao Tong University, among them Yi
Cheng Lu, Bing Chu Cai, Ming Gao, and Ming Yuan Gu.
References
[1] Chou, C. H., "The Crystallization of Iron-Carbon Alloys With Special Reference to the Widman-
statten Structure," Parts I & II, Ph.D. thesis, Harvard University, Cambridge, MA, 1928.
[2] Parr, J. G., "The Criterion of the Martensite Transformation," The Sorby Centennial SympoJium
on the History of Metallurgy, C. S. Smith, Ed., Gordon and Breach, New York, 1964, pp. 235-243.
NOTIS ET AL ON EARLY METALLOGRAPHIC STUDIES 173
[3] Dumas, L, Journal oflron and Steel Instztute Vol 68, 1905, p 255
[4] Osmund, F, "Contribution ~ l'e'tude des alhages," Society d' Encouragement pour l'Industne
Natlonale, 1901, Pans
[5] Sauveur, A and Chou, C H, "The Gamma-alpha TransformaUon m Pure Iron," Transacttons,
American Institute of Mining, Metallurgical, and Petroleum Engineers, Vol 84, 1929, pp 350-369
[6] Sauveur, A, Proceedings, American Phdosophlcal Society, Vol 66, 1927, p 267
[ 7] Bdby, M J and Parr, J G , Journal of the Iron and Steel Instttute, Vol 202, 1964, p 100
[8] Kurdjumov, G V and Sachs, G , Zettschrtft~urPhyslk, Vol 64, 1934, p 325
[9] Nlshlyama, Z, Sctenufic Reports, Tohoku Umverslty, Vol 23, 1934, p 637
[10] Grenmger, B A and Trmano, A R, Transactions, Amertcan Institute ofMining, Metallurgwal, and
Petroleum Engineers, Vol 140, 1940, p 307
[11] Krauss, G and Marder, A R, Metallurgtcal Transactions, Vol 2, 1971, p 2343
[12] Chou, C-H, "Seventy Years A Metallur~st," Zhong Guo Yue Jm Sht Ltao (Journal ofChmese Hts-
tory ofSctence & Technology), Issue 1, 1985, pp 61-71, translated mto Enghsh by the Council of
Chou Chlh-Hung Foundation, 1988
X-Ray and Electron Metallography
K u r t F. J. H e m r l c h I
Those Magnificent Men on Their Scanning

Machines
REFERENCE: Heinnch, K F J, "Those Magnificent Men on Their Scanning Machines," Met-
allography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Van-
der Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amencan Society for Testing and
Materials, Philadelphia, 1993, pp 177-183
ABSTRACr: A handful of lngemous scientists and engineers, m developing scanning electron

beam instruments, have revolutmmzed the characterization of m~crostructures m material
research Like an adventure game, the development of the scanningelectron m~croscope(SEM),
the electron probe mlcroanalyzer, and the analyhcal transmlssmn m~croscope includes tales of
war and conquest, of genres and intrigue, of s~multaneous and (perhaps not so) independent
d~scovenes, and of strange and Nzarre failures The future perspectwes of this art would be wor-
thy of a science fictmn story
KEY WORDS: metallography, mlcrostructure, metallograph~ctechmques, electrons, ~magmg,

instrument manufacture, metallurgical specimens, m~croanalys~s, m~croscopy, quantitative
analysis, scanning, X-ray absorption, X-ray fluorescence, X-ray spectrometry
The electron was discovered by J J Thomson shortly before the end of the nineteenth cen-
tury [I]. In the decade of 1930, the science and technology of electron optics developed rap-
idly, particularly in Germany De Broghe, Busch, Ruska, and Knoll established the bases for
electron optics and electron microscopy, and a commercial transmission electron microscope
(TEM) built by Bomes and Ruska was available in 1939 (For reviews of the early history of
electron microscopy see Refs 2 and 3, for the development ofmlcroanalysls see Refs 4 through
6 ) Knoll demonstrated the feasibility of the scanning electron microscope (SEM) in 1935, and
scanning versions of the TEM were described by yon Ardenne in 1938 This budding tech-
nology was interrupted by the Second World War the German electron optical instruments
in part were 'liberated' by the victorious allies, and the rest divided between two antagonistic
regimes Where before the war much of the development had occurred, it would take years
until research in applied electron optics was restarted Von Ardenne, following his political
mchnaUons, established himself in Dresden, DDR, cooperating with colleagues in the USSR,
but his work performed there, surely under difficult circumstances, did not greatly influence
the further development of the SEM Smith and Oatley finally built a viable SEM in 1955, and
the first commercial model appeared in England as late as 1965 In the meantime, significant
breakthroughs in applied electron optics had been made in France, the United Kangdom, and
in the United States
In the United States, Radio Corporation of America (RCA) had developed a transmission
electron microscope that became commercially available in 1942, some of these instruments
went to Europe Several institutions in France, Canada, and the United Kingdom received
German instruments after the conclusmn of the war, and these sources of lnstrumentatmn
Retired, National Institute of Standards and Technology, Rockvdle, MD 20850
177
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
stimulated further developments in electron microscopy and related areas The main focus of
innovations m England wasthe Cavendlsh Laboratory in Cambridge, where Dr V E Cosslett
directed activities that enriched the field through his work and that of of his colleagues and
students, and through the stimulus it provided to investigators in other places The British
group would lmtlate and further the study of b~ologlcal and geological specimens, high-voltage
spectroscopy (an instrument of this type was developed in Cambridge), the first scanning elec-
tron m~croscope, significant contributions to practical electron optics and development of
electron lenses (Dr Mulvey), and the first prototypes of the analytical transmission electron
microscope (P Duncumb)
Compared with th~s massive effort, the activity in France was, at the beginning, essentially
a one-man show, performed, to be sure, by an extraordinary man, Raymond Castalng He was
at that time working at the Office National d'Etudes et de Recherches Aeronautlques
(ONERA) Castamg became fascinated with the electron microscopes he saw at his institute
Professor Gulmer from the University o f Paris, a d,stmgu~shed sclentzst in the field o f X-ray
optics and diffraction, suggested that he investigate the poss~bdmes of identifying the com-
posmon of small precipitates In steel by exciting them with a focused beam of electrons and
obserwng the emitted X-ray spectra Castamg first underesUmated the difficulty and the mher-
ent limitations of the proposed method, in fact, he thought that the task was too trivial for a
doctoral thesis But after some hesitation he agreed to develop such a mlcroanalytlcal method
(an account by Castalng of these events wdl soon appear m the proceedings of a workshop held
at the National Bureau of Standards (NBS) in 1988) [6]
The precipitates Castamg was planning to characterize were much smaller than 1 um m
diameter--usually they could not be ldenUfied by X-ray diffraction The mmal calculations
indicated that the X-ray lntensmes observable with crystal spectrometers would be a few
counts per minute Castalng and Gulmer considered the posslblhty ofenergy-d,sperslve anal-
ysis (which many years later would be a very widely used techmque in electron microscopes),
but after attaching a focusing (curved-crystal) X-ray spectrometer such as Gmmer used to
monochromatlze X-rays to a modified TEM, Castamg found that h~s forecast had been too
pess,m~sUc, due to the metficlency of curved-crystals for large X-ray sources For a point source
such as that produced on the specimen in his instrument, the count rates were sufficiently high
O N E R A then budt for Castamg a well-constructed spectrometer of h~gh resolution that gave
him the means for the development of the electron probe m~croanalyzer
Another difficulty Castamg ran into was basic, and thus less tractable to impart to the elec-
trons the energy reqmred to excite X-rays emitted by the elements of interest and observable
with the X-ray spectrometers at his dlsposmon, he had to operate at several ten thousands of
volts (his initial work was done at an effective electron energy of 29 keV) But electrons so
energized would penetrate into a microscopically thick specimen to a depth of several microns
The resolution of the classical electron probe m~croanalyzer was therefore considerably poorer
than Castamg had originally expected, nevertheless it was better by several powers often than
the available alternatives (spark source spectroscopy), and Castamg had to accept this physical
hmltatlon
The instrument that Castalng modified was an electrostatic microscope built by Campagme
Francame de Telegraphle Sans Fd (CSF), and its first commercml versions were also provided
w~th electrostatic lenses Later, these were replaced by electromagnetic optics, and Mulvey as
well as Wlttry in the United States contributed to the development of asymmetrical lenses that
allowed the observation of X-rays at h~gh ( > 2 0 ~ emergence angles A static-beam electron
probe was independently developed by I B Borovsky and N P II'ln m the USSR Their work
was published m 1956 The interesting illustration o f their instrument shows the electron col-
umn as a mere attachment mounted on the mowng arm of a large curved-crystal X-ray
spectrometer
HEINRICH ON SCANNING MACHINES 179
The thesis of Castalng is an admirable document that lays the foundations to the theory of
the instrument and its use for quantitative analysis It also contains examples of applications
in fields of importance, particularly in metallurgy Castalng's work, and the construction of
the first commercial microprobes by CAMECA (the first two Instruments were built at
ONERA), put the French in a leading posmon in microprobe analysis and provided the basis
for the development of a powerful group of investigators, including, among many others, Phi-
llbert, Descamps, Klnanenko, Tlxier, Henoc, Maurice, Galle (in biological applications), and
Pouchou
The development of quantitative analysis was also rapid, although the physics of electron-
target interaction was far from being known to a satisfactory degree X-ray physics and X-ray
generation had been explored by the physicists in the 1920s and 30s, and they had no need for
the quantitative accuracy later required for a microanalytlcal method However, Castamg
observed that many uncertainties in physical and instrument parameters canceled when the
compositional evaluation was based on companng the X-ray intensities from the unknown
s p e o m e n with that from a pure element, and that therefore some simple approximations
could be established We should recall that at that time the powerful computers that nowadays
dominate the processes of analysis and data evaluation did not as yet exist, hence, involved
calculations and particularly procedures for on-line data evaluation were not practical The
main limitation of accuracy was the absorption of X-rays produced within the specimen Its
estimation required the knowledge of the depth distribution of X-ray generation This prob-
lem was resolved by Castalng and his students with the aid of tracer experiments Phlhbert was
the first to provide a general algebraic model for calculating the absorption losses He and Tix-
ler then established the so-called Z A F method that contains three factors responding to atomic
number (Z), absorption (A), and X-ray fluorescence (F) effects
The developments in the United Kingdom covered a wide range of techniques With the
stimulus of the work across the Channel, contributions to electron probe mlcroanalysis came
quickly In Harwell, Poole and Thomas had demonstrated the existence of the atomic number
effect, Green performed important experiments on X-ray absorption by means of an instru-
ment with variable X-ray emergence angle, and introduced the use of Monte Carlo calcula-
tions for the determination of electron trajectories The Monte-Carlo technique was later used
and perfected by numerous scientists, particularly in Japan under the leadership of Professor
G Shlnoda D u n c u m b was the first to formulate algebraically the losses of X-ray production
due to backscatter, and Reed proposed a simple and effective correction for fluorescence But
perhaps the most important British contribution was the introduction of scanning techmques
Electron beam scanning was widely used at that time, for instance, in oscilloscopes The
French school did not, however, use such techniques for the construction of images of element
distributions in the microscopic domain Castaing, and later CAMECA, the French manufac-
turers of commercial instruments, used X-ray spectrometers of fairly high wavelength reso-
lution The X-ray intensities provided with these were too dependent on the position of the
X-ray source on the specimen to be of much use for obtaining X-ray images by electronic beam
scanning Scanning X-ray techniques were first developed at the Cavendlsh Laboratory in
Cambridge, United Kingdom, by Cosslett and Duncumb The latter was also the first to use
color images to simultaneously dlustrate the distribution of as many as three elements m one
image To allow the use of beam displacement necessary for scanning operations, the Cam-
bridge firm that produced the first commercial microprobe used a semifocusing spectrometer
Such devices did have unsatisfactory resolution for some wavelength regions, however, work
such as that performed by Melford clearly demonstrated the usefulness and importance of
scanning imaging for practical applications
Duncumb, who worked in ferrous metallurgy, was also concerned about the problem of
poor spatial resolution observed by Castalng To resolve this difficulty, he constructed the Elec-
tron Microscope Micro Analyzer (EMMA), in which a thinned metallurgical specimen was
exposed to an electron beam of submlcron width, and the X-rays were observed with energy-
dispersing gas detectors or with conventional crystal spectrometers The fact that the electrons
emerged from the thinned specimen at a short distance from the point of impact minimized
the effects of electron diffusion. Therefore, high acceleration potentials could be used without
penalty in spatial resolution Yet, the intensities observed with the aid of crystal spectrometers
were low, and the energy-dispersive devices were often lacking in the required resolution Dun-
cumb was, unfortunately, ahead of the technical developments only when sohd-state energy
dispersive detectors (SILl detectors) were introduced In microprobe analysis could his instru-
ment (which is now called the Analytical Electron Transmission Microscope) be used to full
advantage Modern instruments of this type also have scanning faclhties, their use has greatly
extended the potential of X-ray mlcroanalysls In metallurgy and biological sciences.
The use o f energy-dispersive detectors was not new in the field At the Stanford International
Conference on X-Ray Optics and Mlcroanalysls, R. M Dolby, a Callforman who was a stu-
dent of the Cosslett group, caused sensation by showing scanning images of the distribution of
low-atomic number elements such as carbon, oxygen, and boron The ultrasoft X-rays emitted
by these elements were detected by a gas proportional counter and separated electronically by
a complicated network of single-channel analyzers That this bnlhant investigator should later
have switched from microanalysls to the construction of novel sound amphficatlon devices
was a loss for m~croanalysls as well as a gain for music lovers
James Hllher, at RCA in Princeton, having made various significant contributions to elec-
tron optics, also became interested in the possibihtles of mlcroanalysls with electron beams
In 1942, he obtained a patent for a device in which a focusing electron column was used for
elemental analysis in the microscopic domain by the energy analysis of the electrons that had
passed through a thin specimen. He later dwected his attention to other problems, and, due to
Castamg's work, X-ray analysis became the preferred tool for this purpose
Before commercial instruments became available, many investigators m the United States,
such as Bwks, Wittry, Adler, J Brown, Ziebold and Ogllvie, Macres, and others, built their
instruments themselves. Microprobe research in this country did not proceed as much as a
team effort as in Europe, rather it was performed by metallurgists and geologists who wished
to apply this instrument to their field It was at that time that I began to make personal contact
with the field Being a chemist, I felt a strong interest in learning the physics on which micro-
analysis is based, and I found my wish more than fulfilled with my participation in an electron
probe summer school at Massachusetts Institute of Technology (MIT), with the partlopation
of Castalng, professor Norton (MIT), Mulvey, and several other experts The abundant display
of "laws" of electron-target interaction, with which I had been unfamlhar, was to me quite
overwhelming. To make up for my ignorance, I collected bibliography in all pertinent fields,
and then proceeded, with the help of some of my colleagues, to prove wrong what I had not
understood m the first place I dare say that m this task we were qmte successful
Of the many instruments that were individually constructed, that of LaVerne Bwks at the
Naval Research Laboratory stands out in my mind It was quite compact, as in most Instru-
ments of that generation, the X-rays exited the vacuum enclosure through a window The col-
umn was standing on a table covered by heavy paper or cardboard, on which mysterious draw-
lngs were traced. A circular curve turned out to be the focal circle along which the bent crystal
and the window of the detector were aligned by hand The device was, from a didactical view-
point, of utmost clarity
Another remarkable instrument had been built by B W Schumacher at the Ontario
Research Foundation The electron beam in his device left the vacuum enclosure through a
d~fferentlally pumped gate, and produced cathodoluminescence in interaction w~th the air I
do not think that many persons have seen, as I did, an electron beam entering a small beaker
HEINRICH ON SCANNINGMACHINES 1 81
filled with water And I do not believe that this Instrument would meet present safety criteria
any better than Birks'. Curiously, the idea of letting the electrons enter a gas (in this case at low
pressure) was recently revived for .use in a SEM for biological specimens because this technique
reduces at low beam energies the electrostatic charging of poor electrical conductors
The concept of an atmosphenc electron probe was of some interest to the students of mete-
orltes I recall a laboratory, m the area of Boston, where an investigator was building an instru-
ment that could analyze specimens weighing up to a ton To mlmmize vlbrat~ons, the entire
probe system was hung from the ceding on steel girders The design was based on the assump-
tion that meteontes are very precious and could not be cut into the small specimens that could
enter the ports leading to the vacuum enclosure of more conventional instruments Th~s
apprehension, fortunately for the meteorite analysts, turned out to be groundless. The con-
structor ofth~s unique instrument, who insisted m budding all sections of the instrument h~m-
self, apparently ran out of grant money shortly after having built the first spectrometer.
Another designer worked on an instrument to be built commercially m which space charges
w~thm the electron beam were to be avoided by the use of an optical system m which the beam
was gradually compressed without forming a crossover This design, to the chagnn of several
potential customers, never got offthe ground e~ther, although ~ts ongmator was able to pro-
duce the scanning p~cture of a dxme on which I could read the somewhat fuzzy lnscnpt~on:
"In God We Trust "
Although a few French microprobes were |mported into the Umted States, electron probe
microanalys~s only became w~despread with the introduction of a commercial instrument
built by Apphed Research Laboratories (ARL) in Santa Barbara, Cahfornia, designed by D
Wlttry This instrument was quite successful It had three curved-crystal spectrometers (each
with two exchangeable crystals) and efficient scanning facdmes An X-ray emergence angle of
52 5~ ensured an efficient and accurate measurement of X-rays of photon energy down to
about 1000 eV. This angle was obtained by means of a clever design in which the X-ray emis-
sion was observed through the center of the objectwe lens, the specimen had to be elevated
through the body of this lens to pass from the specimen chamber into the operating pos~t~on
The electron column and the spectrometers were inside a huge evacuated chamber that gave
this instrument its characteristic "pregnant" shape The readout electronics were rather simple
but could be upgraded w~thout difficulties This instrument was, I beheve, sold in greater num-
bers than any other electron probe Why this successful mltlal design was not upgraded or
replaced by the manufacturers to keep up with the developing technology ~s a sad story that
should be analyzed in more detad The competing American manufacturers of electron
probes, such as Macres, eventually stopped producing as well, at present, no electron probe is
manufactured in the United States
The motlvat~on for Castamg's work was to resolve a metallurgical problem, and it was m
metallurgy where the instrument was particularly helpful Many phase equdibnum dmgrams
were substantially improved w~th the md of electron probe analysis, and studies of mtergran-
ular diffusion and oxidation were of great practical usefulness The technique also became a
tool of ~mportance m mineralogy, where many new species were--and stall are--first docu-
mented w~th th~s instrument. But the most exciting aspect for many researchers was the study
of extraterrestrial objects In th~s respect, I should mention an interesting investigation, in
which huge hehum balloons were sent to stratospheric heights from a base in Australia, some
cwcled one or more times around the globe, and by means of a funnel-shaped feature at the
top of the balloon, they collected dust particles, presumably of extraterrestrial ongm Unfor-
tunately, ~t was not possible to ehmmate completely the dust contamination d u n n g the take-
off and landing, although a large number of particles were collected, characterized, and visu-
ahzed m scanning images, one could never be fully certain ofthew origin
The excitement reached its culmination with the arrival of the lunar specimens from the
Apollo flights We had several specimens at NBS, searching for unusual phases by means of
backscattered electron scans that revealed the mean atomic number of the phases under the
beam, and providing qualitative and quantitative analyses of phases of interest The word of
the arrival of the " m o o n stones" in our laboratory spread quickly, and everybody wanted to
see them Unfortunately, several visitors also tned to touch our delicate polished specimens
To avoid such profanation, we prepared a mock "lunar specimen" from one of the pebbles
found in the gravel outside the building We gave our visitors ample opportunities to put their
fingerprints on this artifact, while the real specimens were spared the rough treatment
We soon appreciated the great advantages of the scanning procedure, and Harvey Yakowltz
and myself developed a technique of representing up to three elements, in primary colors, as
well as topographic information on the brightness scale, in color composite images (A similar
procedure had previously been demonstrated by D u n c u m b ) These pictures were not only
informative but also very attractive However, the technique was never widely used because
of the lack of electronic data storage facilities and signal manipulation techniques Blrks had
performed early expenments on storage of scan data in a multlchannel pulse height analyzer
(which had only 500 channels), but the lack of on-line computers hampered the effective use
of the instrument, both for scans and for quantitatlon We were forced to use instant devel-
opment films for the recording of scans, if the result of the color addition procedure was unsat-
isfactory, the entire operation had to be repeated The defocuslng properties of the spectrom-
eter further affected the value and appearance of area scans over more than a few microns
In 1968, at the occasion of an electron probe meeting in California, my family and I toured
the United States by car, and this trap included a visit to the Scnpps Institute of Oceanography
in La Jolla, California There, Ray Fitzgerald showed me a lithium-drifted silicon detector that
he had brought from Oak Ridge, Tennessee, to La Jolla in his car, and installed in his electron
probe Although the energy resolution of this device was four to five times worse than that
available at present, and the observation of low-energy X-rays was hindered by the excessive
thickness of the beryllium detector window, it was very exciting to see the lines of the X-ray
spectrum develop simultaneously on the oscilloscope screen, rather than being revealed
through a lengthy spectrometer scanning operation Ray kindly invited me to stay for a few
days, and, with the cooperation o f K Kell from the University of Anzona (who was not in La
Jolla during my visit), we obtained data that resulted In the first publication demonstrating the
use of such detectors in mlcroanalyzers [ 7] The new X-ray detection device was of very great
impact It was not only very useful in the traditional electron probe mlcroanalyzer, where it
sped up enormously the quahtauve identicatlon process, but it could also be installed in a con-
ventional scanning electron microscope (and also in a TEM), virtually transforming it into an
electron probe mlcroanalyzer, at a relatively low cost The diffusion of this technique in SEMs
may, in fact, have contributed to the slackening in the demands for the more expensive elec-
tron probe
The new technique has some disadvantages the resolution of energy spectra is lnferaor to
that of crystal spectrometers, so that overlap problems anse, and, for the same reason, the
background due to c o n t i n u u m emission IS more pronounced and particularly disturbing in
the conventional scanning images Such problems were resolved when It became possible to
connect the scanning instruments to powerful and fast computers for on-line data evaluation
Excellent scanning pictures can now be obtained, both with crystal and silicon detectors, due
to the calibration and background corrections performed at high speeds Large numbers of
scans can be stored permanently on magnetic tapes and disks At the same time, the data
reduction schemes for quantitative analysis can be made more accurate since there is no longer
the need for mathematical shortcuts as before Because more involved calculations can be per-
formed, it is also possible to extend quantltatlon to layered specimens, to thin films, and to
small (submlcron) particles
HEINRICH ON SCANNING MACHINES 183
As to the SEM, investigations by many researchers such as Crewe, Wells, and Joy are push-
mg the limits of resolution into molecular dimensions, and this instrument is now a necessary
adjunct to research and quality control in many areas (such as semiconductor manufacture)
The remaining limitations of the X-ray mIcroanalyzer and the SEM have stimulated the
invention of other mlcroanalytlcal tools, such as the ion microprobe and microscope, the
Laser Raman probe, the atomic probe, and the energy loss spectroscope Instruments We now
possess an arsenal of microanalytlcal tools that has proven indispensable for modern science
and technology, thanks to those magnificent men on their scanning machines
References
[1] Thompson, J J, Phtlo~ophlcalMagazme, Vol 4, 1897, p 293
[2] Hall, C E, Introductton to Electron Mtcroscopy, 2nd ed, McGraw-Hall,New York, 1966
[3] Wells, O C, Scanmng Electron Mlcrogcopy, McGraw-Hill, New York, 1974
[4] Quantttatlve Electron Probe Mtcroanalysls, K F J Hemnch, Ed, National Bureau of Standards Spe-
cial PubhcaUon 298, 1968
[5] Helnnch, K F J, Electron Beam X-Ray Mlcroanalyszs, Van Nostrand Reinhold Co, New York,
1981
[6] Electron Probe Quantttatton, K F J Helnnch and D E Newbury, Eds, Plenum Pubhshmg Corp,
New York, in press
[7] Fitzgerald, R, Ked, K, and Helnnch, K F J, Sctence, Vol 159, 1968, p 528
Samuel M. P u t ' d y I and Leo Zwell 2
Seventy-Five Years of Activity in X-Ray

Methods by ASTM Subcommittee E4.06
REFERENCE" Purdy, S M and Zwell, L, "Seventy-Five Years of Activity in X-Ray Methods
by ASTM Subcommittee E4.06," Metallography Past, Present, and Future (75th Anniversary
Volume), ASTMSTPl165, G F Vander Voort, F J Warmuth, S M Purdy, andA Szlrmae,
Eds, American Sooety for Testing and Matenals, Philadelphia, 1993, pp 184-188
ABSTRACT: ASTM Subcommittee E4 06 on X-ray Metallography was orgamzed m 1925, nine

years after Committee E4 ~tselfwasformed The first standard on radmgraphy was pubhshed the
next year, 30 years after the dmcoveryof X-rays In 1938, Hanawalt et al developed their method
of identifying compounds by X-ray diffraction that became the basis of ASTM Standard E 43,
pubhshed m 1942 In 194 l, the Natmnal Research Councd and ASTM orgamzed the Joint Com-
mittee on Powder Dlffrachon Standards (JCPDS) to administrate the pubhcahon of the data
used m th~s method Since then, the JCPDS has grown to include twelve Cooperating Organl-
zatmns and over 100 contributing sooet~es It became independent of ASTM m 1969 Other
additional activities of Subcommittee E4 06 Have included developing standards on determin-
ing the onentatmn of single crystals, the preferred onentatmn of polycrystals, and retained aus-
tenlte m heat-treated steels
KEY WORDS. X-rays, X-ray diffraction, dlffracUon, standards, metallography, metallurgical

specimens, mlcrostructure, metaUographlc techniques
Sixteen to seventeen years elapsed after the discovery of X-rays by Roentgen in 1895 before
their nature was disclosed by the work of Laue and Bragg F n e d n c h and Kmpplng, at Laue's
suggestion, produced X-ray diffraction patterns of single crystals, which Laue was able to show
reflected the symmetryofthe crystal Thlsdevelopedlnto the famlhar Laue method orpattern
used to determine the orientation of a single crystal and appears as ASTM Method for Deter-
mining the Orientation of a Metal Crystal (E 82-63); and, it is still going strong after 80 years
(the method, not the standard; that's only 42 years old) W. L Bragg, at the same time, 1912,
made the first crystal structure analysis of potassium chloride (KC1) and sodium chloride
(NaCl) by application of his famous law, nX = 2d sm 0 [1] Following close upon these devel-
opments, Debye and Scherrer in Germany in 1916 [2] and A W Hull in the United States m
1917 [3] came up with the powder diffraction camera Hull has been neglected in the history
of X-ray diffraction but he developed a powder camera independently from Debye and
Scherer This was d u n n g World War I and communications between Germany and the United
States were intermittent at best From these developments arose new sciences, X-ray crystal-
lography itself, and the materials sciences
ASTM Committee E4 on Metallography was orgamzed in | 916 Nine years later in 1925,
Subcommittee 6 on X-ray Metallography was organized Its first activity was to publish a long
report [4] prepared by Zay Jeffrles with a section on radiography by H H Lester and another
Semor research associate, Technical Research Center, Detroit, National Steel Corporation, Trenton,
M148183
2Consultant, Swarthmore, PA 19081
184
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
PURDY AND ZWELL ON X-RAY METHODS 185
on diffraction by L W McKeehan and E C Baln Two well-known names in metallurgy,

Jeffnes and Baln, have shown up, and later on, other famous names m diffraction and met-
allurgy will appear In 1926, ASTM Tentative Recommended Practice for Radiographic Test-
ing of Metal Castings (E 15-26T) was published as well as defimtions of terms for both crys-
tallography and radiography Thirty years after the discovery of X-rays, ASTM had
standardized their practical use
In the custom of ASTM in those days, standards were published as Tentative for a few years
to obtain field experience in their application Communications were slow, mall traveled by
railroad, and people were reluctant to travel any distance because of the time involved Phil-
adelphia to New Orleans by train took two nights, New York to San Francisco nearly a week
A trip by airplane was an act of desperation, long distance telephoning was an exercise in frus-
tration To clarify a point in a standard required wntmg a letter and awaiting a reply, some-
thing that might take a few weeks, or if the reply was complicated, a few months Life was more
leisurely then You sent off your letter and went about your business until the reply came
In 1929, ASTM E 15 was advanced from a Tentative Practice to a Standard Practice and a
hst containing 20 establishments using radiography and 41 doing diffraction was prepared Of
these, 23 were universities, 12 were industrial laboratories, three were government laborato-
ries, and three were commencal laboratories Interestingly enough, ten of the industrial con-
cerns are still in business and still doing X-ray diffraction A glossary of terms was to be pub-
hshed jointly with the AIME (American Institute of Mining, Metallurgical, and Petroleum
Engineers) and ASST (American Society for Steel Treating, now ASM International) but
apparently was never finished
X-ray diffraction in the times between the World Wars was not easy First of all, you had to
build your own power supply, starting with a me&cal or radlologlcal power supply Second,
there was the problem of obtaining or building a tube A Coohdge tube required no cooling
but only tungsten or molybdenum targets could be used Water-cooled tubes were built but
maintaining the required vacuum was difficult Usually this Involved cracking open a valve
just enough to hold a vacuum low enough to keep the target clean without losing conductivity
through the vacuum Third, there was the matter of camera design and construction In the
second half of the 1930s these problems were alleviated General Electric X-ray Company and
Phflhps Metalhx both began manufactunng sealed-off, demountable X-ray tubes, allowing
production of commerlcal X-ray apparatus. In the same period of time, M J Burger devel-
oped the familiar cyhndncal camera using the Straumanis film mounting method [5] By using
camera diameters of 57 3 or 1 l 4 6 mm, the film could be read directly using a mllhmetre scale
General Electric came out with a 145.5 mm (5 73 in ) diameter camera that had the advantage
that the specimen was out in the open, however, you had to be careful not to stick your finger
through the a l u m i n u m foil shielding the film With these developments, X-ray diffraction
became relatively simple and uncomplicated
At the Annual Meeting of ASTM in 1935, a preliminary symposium was held with nine
talks on radiography and more than 20 on &ffractlon. Next year, 1936, these papers were sum-
marlzed m a formal symposium with six papers each on radiography and diffraction It
was published by ASTM m 1937 as the "Symposmm on Radiography and X-ray Diffrac-
tion" [6]
Back in 193 l, the name of the subcommittee had been changed to X-Ray Methods. Then,
in 1937, Committee E7 on Radiographic Testing (now titled Nondestructive Testing) spht off
from Committee E4 under the leadership of Horace Hardy Lester and Earnshaw Cook. The
remaining portion in Committee E4 took up X-ray diffraction as its main topic There were,
however, a few meetings with the American Society for Metals (ASM), AIME, and American
Physical Society (APS) devoted to considerations of the physical basis of metal properties, but
these went nowhere, as far as we know
In 1938, J D Hanawalt and coworkers at the Dow Chemical Co published their historical
paper "Chemical Analysis by X-ray Diffraction" [ 7,8]. This paper, which contained the dif-
fraction patterns of 1000 compounds and a method of comparing the three strongest lines
(remember, this was all done on film) of the unknown with the three strongest lines of the
known compounds, was immediately recognized as presenting a workable method of deter-
mining the compounds present in a sample. This is an important point Ordinary chemical
analysis will tell you what elements are present but not how they are combined with one
another Sometimes, a good guess will allow you to make a prediction, but there is no certainty
X-ray diffraction, on the other hand, will tell you what crystal structures are present, and, if
you have been careful, you can infer what chemical compounds are present With both chem-
ical analysis and X-ray diffraction, the chemical compounds in a sample usually can be
identified.
In pnnciple, the procedure is quite simple In the original Index, the " d " spacings o f the
strongest lines of the diffraction patterns, ranging from 0 8 to 20 A, were divided into 77
groups Within each group, the patterns were listed in order of the second strongest line The
third strongest line was also listed Additionally, the intensities of the three lines were also
listed In making a search, you opened the Index to the section containing the strongest line
in your unknown and looked down the list until you came to the second strongest line, then
confirmed the identification with the third strongest line and comparison with the listed inten-
sities A complete diffraction pattern was hsted in a card file The prudent searcher checked
his, or her, identification from the Index with the pattern on the card file Of course, if your
unknown contained several compounds, hfe became complicated It took time, experience,
intuition, and, it is to be hoped, the chemical composition of the unknown, to sort out the
compounds present in a mixed unknown
Subcommittee 6, under W L Fmk, using this method, issued ASTM E 43-42T, Recom-
mended Practice for Identification of Crystalhne Materials by the Hanawalt X-ray Diffraction
Method. Later on, m 1952, there was an argument over the narrowness ofASTM E 43 A small
task force, C L Christ, F W Matthews, and W Parnsh, took up the question of either revising
ASTM E 43 or writing a new procedure After several meetings, a comprehensive text was
written, to be published as a Special Technical PubhcatIon (STP) It never was released
Finally, in 1962, ASTM E 43 was withdrawn Following protracted discussion, if not argu-
ment, agreement that a Methods and Procedures Manual ought to be written was realized
Karl Beu became chairman of the Task Group and was lust getting things going when he died
suddenly After that, calls to authors were ineffective
Returning to 1941, the U S National Research Council (NRC) and ASTM orgamzed the
Joint Committee on Chemical Analysis by X-Ray Diffraction Methods The Joint Committee
pubhshed the first set of X R D cards, comprising the Dow Chemical Co data Each card con-
talned the complete diffraction pattern, ~dentificaUon of the material, its source, and a litera-
ture citation along with the Index book containing the the three strongest hnes and their mten-
slues As menUoned earher, Subcommittee 6 had ,lust promulgated the tentative standard
ASTM E 43-42T, that used these data sets Later, having felt that they had completed their
mission, the N R C dropped out of the Joint Committee and was replaced by the American
Sooety for X-Ray and Electron Diffraction (AXRED), which later combined with the Crys-
tallographic Society of America to form The American Crystallographic Assocmt~on
Meanwhile, the British Institute of Physics had been collecting their own set of cards They
,lomed the Joint Committee in 1944 and thew cards formed the first Supplementary Set of the
Powder Diffraction File (PDF) This Supplementary Set, along with an appropriate Alpha-
betlcai and Formula Index, was pubhshed m 1945 as Set No 2 of the P D F In this set, organic
and lnorgamc compounds were separated, which was not the case in the first set Set No 3
appeared in 1950, Set No 4 in 1952, Set No 5 in 1953, and Set No 6 in 1955 Since 1957, a
PURDY AND ZWELL ON X-RAY METHODS 187
new set, with about 2000 diffraction patterns, has come out every year Each contained mostly
new data, but some older cards were replaced as better data became available Each new Index
Book interleaved the old and new data, formulas, names, and strongest lines, so that the newest
Index could be used without having to go back to an older edition
Data from the National Association of Corrosion Englneenng (NACE) were incorporated
into the fifth set and NACE became the fourth cooperating society of the Joint Committee in
1953 In 1969, the Joint Committee was separated from ASTM and became an independent
organization--the Joint Committee on Powder Diffraction Standards (JCPDS) Other orga-
nizations from the United States, Canada, the United Kingdom, France, Germany, and Aus-
traha, twelve m all, now comprise the Cooperating Organizations of the JCPDS Finally, in
1977, the name was changed to JCPDS-International Centre for Diffraction Data (JCPDS-
ICDD) Some things, though, die hard, reference IS still made to the ASTM Card File
In the mid 1960s, with the development of modern electron microscopes, selected area elec-
tron diffraction became popular Observed intensities of electron diffraction patterns often dif-
fered from those found in X-ray diffraction of the same substance W C B~gelow and J V
Smnh developed a new index listing the patterns In order of decreasing " d " spacing but using
eight spacings for each pattern and leaving out intensity values The JCPDS called this the Flnk
Index, after Dr W L Flnk of ALCOA, then chairman of the JCPDS In recent times, when
space became available, intensities have been added and now there is so little difference
between the Hanawalt and Flnk Indices that the latter is pubhshed only occasionally
In more recent times, the card file and the index have been computenzed, making searching
easier New software allows better matching but still experience and intuition are required for
effioent searching
Since becoming independent, JCPDS-ICDD has grown m membership and activity
JCPDS-ICDD now publishes its data m several forms, book (three patterns to a page), micro-
fiche, tape, and CD-ROM Selected data sets are published for minerals, for metals and alloys,
for forensic materials, and for electron diffraction Returning to a project of Subcommittee 6,
they have published several sections of the Methods and Practices Manual m the quarterly
journal, Powder Dtffractton These include "Toward Improved Alignment of Powder Dlffrac-
tometers," "Methods of Producing Standard X-ray Diffraction Powder Patterns," "Sample
Preparation Methods in X-ray Powder Diffraction," and "Standard Reference Materials for
X-ray Diffraction," among others Round-robin tests have shown, as they always do, that
uncertainty or error is one to two orders o f magnitude greater than that claimed by individual
participants JCPDS-ICDD is also the publisher of Crystal Data, a compilation ordered on
lattice parameters, of references to structural articles
To be horticultural, the present JCPDS is the flowenng tree that grew from the seed planted
by Subcommittee 6
Other things occupied the subcommittee besides the Powder Diffraction File In 1967, a
Task Group was organized to work on quantitative measurement of retained austenlte in
steels After discussion with the Sooety of Automotive Engineers (SAE), the decision was
made not to duplicate their work However, when Leo Zwell, one of the authors of this paper,
became chairman of the Subcommittee, in 1973, dissatisfaction with the results obtained by
the SAE method was evident A round-robin test was conducted, w~th ten laboratories partic-
ipating As expected, without equipment to rotate and translate the s p e o m e n dunng the test,
the results in three directions were very different but the averages of the three directions were
surprisingly close Robert Hlnton of Bethlehem Steel (a determined man and he had to be)
started offa Task Group that prepared and validated by another round-robm test the ASTM
Practice for X-Ray Determination of Retained Austenlte in Steel with Near Random Crys-
tallographic Orientation (E 975), issued in 1984
Another determined man, Peter R Morns, then of Armco Steel, accepted the lob ofimprov-
mg ASTM E 81-49, Method for Prepanng Quantitative Pole Figure Diagrams which dated
back to 1949 X-ray diffraction techniques had improved since then He wrote letters to many
people that he thought were qualified but recewed less than ten acceptances Nevertheless, in
two years, he rewsed ASTM E 8 l, producing the document, ASTM E 81-77, with the same
Utle, about the only thing left untouched m the revision
In more recent years, Subcommittee 6 has faltered and lost its way The major achievement
of Subcommittee 6, creation and n u r t u n n g JCPDS, was done JCPDS grew into a strong and
self-sufficient orgamzat~on The present procedures work, although some date back 40 years
and others are as recent as 1984 There seems to be httle demand for new procedures in X-ray
analysis of metal, however, one subject that may offer an opportumty for work ~s the Orien-
tation DlsmbuUon Function, but this is an enormously comphcated subject Subcommittee
6 on X-ray Methods has been folded into Subcommittee I 1 to form a subcommittee on X-ray
and Electron Metallography
References
[1] Bragg, W L, Proceedings, Royal Sooety, London, Vol 89A, 1913, p 248
[2] Debye, P and Scherrer, P, Zetts~hrdt[urPhyslk, Vol 17, 1916, p 277, Vol 18, 1917, p 291
[3] Hull, A W, Phystcal Revw~, Vol 10, 1916, p 661, Journal, American Chemical Sooety, Vol 41,
1919, p 1169
[4] Jeffrles, Z, Proceedings, American Sooety for Testing and Materials, Vol 25, Pt 1, 1925, p 444
[5] Buerger, M J, Amertcan Mlneralologlst, Vol 21, 1936, p 11
[6] Proceedings, Symposmm on Radiography and X-ray Diffraction, American Sooety for Testing and
Materials, 1937
[7] Hanawalt, J D and Rmn, H W, lndustrlalandEngmeermg Chermstry, AnalyttcalEdmon, Vol 8,
1936, p 244
[8] Hanawalt, J D, Rmn, H W, and Frevel, L K, Industrial and Engineering Chemtstry, Analytwal
Edltlon, Vol 10, 1938, p 457
Atul S. Rarnanl ~and Paul R. H o w e l l I
Microstructural Studies of an Oxide-

Dispersion-Stabilized Niobium Composite
Using Transmission Electron Microscopy
REFERENCE: Ramani, A S and Howell, P R, "Microstructnral Studies of an Oxide-Disper-
sion-Stabilized Niobium Composite Using Transmission Electron Microscopy," Metallography
Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Vander Voort, F
J Warmuth, S M Purdy, and A Szirmae, Eds, American Society for Testing and Matenals,
PhdadelphIa, 1993, pp 189-198
ABSTRACT: Transmission electron microscopy (TEM) has been employed to examine the
effect of mechanical alloying and subsequent hot isostatlc pressing (HIPmg) on the mlcrostruc-
lure of a mechanically alloyed nioblum-yttrlacomposite It ~sshown that the mechanical alloy-
ing process severely cold-works the niobium matrix and an elongated cell structure develops
Partially recrystalhzed regions form dunng the HIP cycle From the TEM data, it is argued that
recrystallization proceeds by repeated nucleation of new strain-free grains m contact with the
"old" recrystalhzation front This process is facilitated by the yttna-denved dispersoids that are
efl~ctwe m mhlbmng the motion of the "old" recrystallizatlon front Hence, partial recrystalh-
zation produces a necklace of small (~0 5 to 5 urn) grains that surround the still highly deformed
matr, x
KEY WORDS: niobium, yttna, oxide d~sperslonstrengthening, metal matnx composite, creep,
recrystalhzatlon behavior, necklace mlcrostructure, transmission electron microscopy, mechan-
ical alloying, hot isostatlc pressing, metallography, metallurgical specimens, mlcrostructure,
metallograph~ctechniques
In this paper, we report results of microstructural studies of an as-hot lSOStatically pressed

(HIPed) m o b m m - 2 % by volume yttna (Nb-2Y) composite using transmission electron
microscopy (TEM) The metallographic studies have permitted the formulation of a model
for recrystalhzation m this composite
The invention of mechanical alloying by Benjamin [1] made it possible to produce a whole
new class of oxlde-dlspersion-stablhzed alloys with good high-temperature strength The
promise that oxide-dispersion-staNhzed alloys offer is their exceptional creep resistance and
good mlcrostructural stabihty at high homologous temperatures The refractory metal, nio-
bium, has the potential for being used m applications that require high strength-to-weight
ratios at elevated temperatures However, at high temperatures, creep processes become a
major concern and these have been extensively studied in both pure niobium and nlobmm-
based alloys [2-4] Creep strengthening by second-phase particles has been shown to be fairly
effective [3], however, the thermal stability of the precipitate distribution is a major concern,
since coarsening of the precipitate d~stnbutlon d u n n g prolonged aging at high temperatures
significantly affects the creep strength We have employed mechanical alloying to d~sperse fine
(_<0 5 ~m) high purity yttna particles, homogeneously into a niobium matrix as a means of
hGraduate student and professor of Metallurgy, respectively, Department of Materials Science and
Engmeenng, The Pennsylvama State Umverslty, Umverslty Park, PA 16802
189
Copyright
Copyright*by1993
ASTM byInt'l
www.astm.org
obtaining a creep resistant moblum composite with a stable second-phase distnbutlon Due
to the high-energy nature of the mechamcal alloying process, where repeated welding, frac-
tunng, and reweldmg of dry powder particles produces the final alloy, the deformation pro-
cesslng aspect of the mechanical alloying process is very important The mechamcally alloyed
powder particles have a considerable amount of cold-work stored in them Hot isostatlc (HIP-
rag) of the mechanically alloyed powder particles that is used to consohdate them into a com-
posite, brings thermally achvated processes such as recovery and recrystallIzatlon into play
Composite Processing
Feedstock of overall composmon, m o b m m - 2 % by volume yttria, was prepared by blending
elemental (~< 100 #m) niobium powders and ( < 10/~m) yttna powders of high starting pumty
Mechamcal alloying of this feedstock was camed out by charging it into a laboratory-scale
high-energy ball mill, known as a Szegvan attntor, that was filled with steel balls During the
entire mechamcal alloying process, the attntor was water cooled and an inert argon atmo-
sphere was maintained to prevent any major contamination of the powders The process was
considered complete when the composite powder particles had a finely layered and umform
structure as determined by hght microscopy It was assumed that at this stage the yttna dls-
persolds were randomly distributed within the m o b m m matrix. The mechanically alloyed
powders were sealed m mild steel tubes under a vacuum of 10 2 Pa at 673 K The sealed tubes
were HIPed at 1573 K for 4 h under a pressure of 210 MPa to obtain the final composite A
schematic dmgram of the processing schedule is shown in Fig 1
Preparation of Niobium Composite Specimens for TEM

Two major steps were involved in preparation of specimens for TEM (1) preparation of
thin disks from bulk material, and (2) final thinning of the disks to electron transparency
Preparation of Thm Dtsks from Bulk Matertal

A diamond wafering saw was used to section a cylindrical rod of the bulk composite into
thin slices about 1 m m thick These slices were mechanically thinned to 200 #m using succes-
swely finer silicon carbide (SIC) grit papers. The final mechanical thinning step was done using
a mechanical thinning fixture and 600-grit SIC paper, where the specimen thickness was con-
stantly monitored with a micrometer gage Since the resulting thin sheets of the composite
speomen were not ductile enough to be punched using a conventional mechamcal punch,
d~sks that were 3 m m in diameter were cut from these sheets using an ultrasomc disk cutter
The disks were further throned down to 100 #m using the throning fixture and 600-grit SIC
paper Finally, the disks were dimpled to yield a 10-um-thick section m the center of the disk
speomen using a digital dimpling gnnder and (--<6 um) dmmond paste as the pohshing
medmm
Fmal Thmnlng of the Dtsks to Electron Transparency

The dimpled disks were mounted on an ion-millingspecimen stage and thinned to electron
transparency using an argon ion-mill operating at a gun voltage of 3 75 kV and a gun current
of I mA The initial ion-milling angle was set to 20* Ion milling was periodically interrupted
in order to check for formation of thin area on the dimpled speomen using a low-power micro-
scope Ion milling was stopped when the formation of a small hole was first noticed after which
the ion-milling angle was reduced to 7* and ion milling continued for an hour The ion-milled
RAMANI AND HOWELL ON RECRYSTALLIZATION BEHAVIOR 191
START
[ Nb + Yttria : Blend ]
I Mechanical Alloying I
I Encapsulation of Alloyed Powders I
I Hot Isostatic Pressing I

1
FINISH : As - HIPed microcomposite
FIG l--Schematlc dlagram of composlteprocesslng schedule
speomens were then examined with a Phlhps EM420T TEM operating at 120 kV Figure 2 is
a schematic diagram of the specimen preparation procedure for TEM exammaUon
Results and Discussion

Mlcrostructure Due to Deformation Processing by Mechanical Alloyzng
In the as-HIPed condition, certam regions of the mlcrocomposlte show no evidence of
recovery and recrystalhzatlon Figure 3 is a bnght-field (BF) TEM mlcrograph from one such
[ Sectioning [
[ Mechanical Thinning[
] Ultrasonic Disk CuttingI
]Dimpling]
] lon'Milling I
ITEM Examination ]
FIG 2--Schematw diagram of specimen preparationprocedurefor TEM exammatlon
region Characteristic of such regions are the severely elongated subgralns (aspect ratio
l0 1) The subgraln size is exceedingly fine along the thin dimension, typically 0.05 #m.
The figure clearly reveals the deformation processing aspect of the mechanical alloying pro-
cess This intense deformation of powder particles is due to the repeated high-energy cold
welding processes that occur within the attritor during collisions between the steel balls and
the concurrent entrapment of powder between the colhdlng balls It is evident from Fig 3 that
a large fraction of the input cold work from the mechanical alloying process is retained by the
niobium matrix In addmon to the preceding, certain regions of the specimen had partially
recrystalllzed These regions are discussed later
Nucleatton o f R e c r y s t a l h z a t l o n
Figure 4a is a BF Image of a partially recrystalhzed region The recrystalhzed grain (R) is
virtually strain free as can be gaged from both the BF image and the indexed selected area
diffraction pattern (SADP) of Fig 4b; the latter showing no evidence for arcing of the reflec-
tions Figure 4a also shows evidence of recovery in the deformed regions ahead of the advanc-
ing recrystalhzatlon front (the latter is marked F in Fig 4a) The presence of large subgralns
(S) suggests that recrystalhzatlon is o c c u m n g by a subgraln coalescence mechanism [5] How-
ever, the virtually ubiquitous observation of well-developed recrystalllzatlon fronts (for exam-
ple, see Figs 4 and 5) argues strongly for a mechanism involving pre-existing high-angle grain
boundaries rather than random nucleation in the deformed matrix Hence, it is likely that
FIG 3--BHght-/leld T L M linage o / a n tmretrvstalhzed regton m the ~ompostte 6hara~terlzed bl a

~eveteh ehmgated ~ell slrlt~lltre
FIG. 4 - - ( a ) Bri~,hl:/ield 7"EM imu~,e ~?/a partially cowtallizcd re,~,ion. N~le lhe ,~lram li'cc nalurc ~!/ lhc
rccry~la/lizcd L,raipl (R) and lhc pre~ence ~ f /ar~,(, .~ut~g,rains (S) in lhe vicmily O/'lh(' r~'o'.l'.~l~l//i:~llio/1 I/'O/ll
(F). (b) Selecl~'d urea df/lraclion l~allc>rn ot~lained //om the re~,ion (R) i/t b'i~,. 4a. 771ere i.~ m~ cvideHce #~r
arcin~, ~t l/tc rc/leclio/t.~. B = [ 1 lO]xj,.
FIG 5--Brtght-BeM T E M trnage o[ a well-developed recrvsTa/hzatmn [ront (F) The re~ry~talhzed gt am

stze ts relattvelv smal[ (tvptcall)~ 0 5 to 5 urn) and eqmaxed
prior mobmm particle boundaries are the nucleation sites for recrystalllzatlon In ad&tlon,
the very infrequent observation of large subgralns, "in regions remote from the recrystalhza-
Uon front," (and see Fig 5) again argues against "random subgraln coalescence "
However, large subgrams were frequently observed "in contact with the recrystalhzatlon
front" and an example of this phenomenon is presented in Fig 6 Again, the coarsened
subgraln is labeled S and the recrystalllzaUon front is labeled F
T h e R o l e o f DIspersotd Parttcles in the D e v e l o p m e n t o f a " N e c k l a c e " Mtcrostructure

Figure 5 shows that the recrystalllzed grain size is relatively small (typically 0 5 to 5 um) and,
m general, the recrystalhzed grains are relatively equlaxed. To substantiate th~s claim, Fig 7
is included In this figure, the &spersold is labeled Y, and the band (or necklace) of recrystal-
hzed grains have dimensions that are similar to those in Fig. 5
It is considered that recrystalhzatlon in this composite ~s occurnng in a manner that is vir-
tually identical to that documented by Bee et al. [6] for the case of a powder-produced nickel-
base superalloy In c o m m o n with the present lnvestlgaUon, it was concluded m Ref 6 that
recrystalhzatlon was initiated at high-angle gram boundaries. Furthermore, the nickel-base
superalloy employed by Bee et al [6] contained relatively large ( ~ 0 5 um diameter) 3" parti-
cles and the present alloy also contains submlcrometer &spersold particles that derive from
the starting yttna powders. In the following, it is argued that repeated nucleation of recrystal-
hzed grains yields the so-called "necklace" structure
Figure 8 shows a recrystalhzatlon front In common with any second-phase particle, the
submlcrometer (--<0 5 #m) dispersold particle derived from yttrla is exerting a Zener-type [ 7]
FIG 6 - - B r t g h t - h e t d T E l 4 zmage sho~* m g a lars sub,g, ram (S) m conlacl atth the rer r~ slal/izallon
/ l o n t (F)
FIG 7-- Brl~hl-BeM T E ~1 t m a g e sho~ m g a l'ttrla-derl~ ed ch spot stud pat ire le ( Y ) art e s l m g t/~e ter t ~ s-
Copyright
t a l h z a t t o n by ASTM
lronl (F) Int'l
l \ o t e(all rights
al~o lhe reserved); Thu Dec
n e c k l a c e o/pec 29 00:42:12
p v~lalhzed EST
~,,ram~ ol 2011
SltHllal size 1o those in I~I~, 5
FIG 8--Br;ghl-held T E M ;rnage dlustratmg lhe Zener drag [or~e on the recrystalhzatlon ]ront e.~erted
by a vHrta-der;ved d;spersotd partt~ h, (Y) Note the large subgram (S) m ~onta~l w;th the reervstalhzatmn
[ront
drag force on the boundary This drag force locally pros the boundary, which is then forced to
bow around the particle Figure 7 shows similar features (At this point, it should be noted that,
as yet, we have been unable to determine the crystal structure of the dispersolds Somewhat
surprisingly, they are not yttrlat) Figure 8 also shows that there is a large, strain-free subgraln
(S) in contact with the recrystalhzation front It is considered that this large subgraln forms by
the accelerated loss of dislocations to the high angle reaction front (this point will be returned
to later) The formation of this large subgrain (a further example of which has already been
presented in Fig 6) reduces the local strain energy differential, needed to propagate the "orig-
inal" recrystalhzatlon front through the heavily deformed regions that are immediately adja-
cent to the front Therefore, it is suggested that the formation of large subgralns, in contact
with the pinned reaction front, suppresses recrystalllzation from continuing from the original
position o f that front Rather, continued coarsening ofsubgrains such as (S) in Figs 6 and 8
will yield new recrystalhzation nuclei, and a necklace of small, equlaxed grams will result
The Model
The development of the necklace structure can be modeled with respect to Fig 9, which is
a schematic illustration of what we consider to be a sequence of events in the formation of the
"necklace" mlcrostructure. In Fig 9a, it is assumed that the recrystalhzation front has been
pinned by a dlspersoid particle (Y) (see also Figs 7 and 8) Because of the proximity of high
angle interfaces, subgraln coarsening (Areas C, D, and E in Fig 9a) will be accelerated m the
immediate vicinity of the recpystallized grains (see Figs 6 and 8) This will most probably occur
FIG. 9--Schematic illustration qf the sequence of events in the formation of the "'necklace" micro-
structure.
by dislocation loss to the high-angle grain boundanes During the process, the driving force
that maintains migration for Grams A and B will continually decrease and, eventually, this
driving force will be less than the drag force Migration will then cease Further recrystalhza-
tion will occur when the coarsened subgralns will have attained a sufficient mlsonentatlon and
size advantage A new recrystalhzation front will then form as shown in Fig 9b The processes
descnbed here then simply repeat as new pinning dlspersold particles are encountered and new
coarsened subgralns (F and G in Fig 9b) are formed
Conclusions
An oxide-dispersion-strengthenedniobium composite with a nominal StOlChlometry of nio-
b i u m - 2 % by volume yttna has been fabricated using mechanical alloying and hot isostattc
pressing A fine dispersion of dispersolds In a highly deformed niobium matnx charactenzed
by severely elongated subgralns is obtained by the high-energy mechanical alloying process
Partial recrytalhzation of the niobium m a t n x occurs upon subsequent hot isostatic pressing
Evidence obtained by transmission electron microscope studies of the niobium composite
argues against random subgraln coalescence as a recrystallizatlon mechanism In this compos-
ite A model that explains the formation of the "necklace" mIcrostructure observed in the
composite hasbeen formulated It involves repeated nucleation ofrecrystalhzedgralnsat pnor
recrystalhzatlon fronts that have been pinned by the dlspersold particles This process yields
the "necklace" mlcrostructure
References
[1] Benjamin, J S, Metallurgwal Transactions, Vol 1, 1970. p 2943
[2] Begley,R T , Harrod, D L, and Gold, R E m Refractory Metals andAlloys, Metallurgy and Tech-
nology, I Machm, R T Begley,and E D Welsert, Eds, Plenum Press, New York, 1968, p 41
[3] McAdam, G D, Journal of the lnstuute of Metals, Vol 96, 1968, p 13
[4] Klein. M J and Metcalfe, A G , Metallurgical Transactions, Vol 4, 1973, p 2441
[5] Hu, H, Acta Metallurgtca, Vol 10, 1962, p 1112
[6] Bee, J V, Jones, A R, and Howell, P R, JournalofMaterlalsScwnce, Vol 15, 1980, p 337
[7] Zener, C, pnvate commumcanon to C S Smith, Transacnons of the Amerwan Institute of Mmmg
andMetallurgt~alEngmeers, Vol 175, 1949, p 15
Rajan Varughese I and Paul R. H o w e l l I
The Application of Transmission Electron

Microscopy to the Study of a Low-Carbon
Steel: HSLA-100
REFERENCE: Varughese, R and Howell, P R , "The Application of Transmission Electron
Microscopy to the Study of a Low-Carbon Steel: HSLA-100," Metallography Past,Present, and
Future(75thAnmversary Volume),ASTMSTPI165, G F VanderVoort, F J Warmuth, S M
Purdy, and A Szlrmae, Eds, American Society for Testing and Matenals, Philadelphia, 1993,
pp 199-211
ABSTRACT: Transmission electron microscopy (TEM) together with scanning electron micros-
copy (SEM) and optical microscopy have been employed to analyze the microstructures that
develop in a copper-contalmng, low-carbon (0 04% by weight) HSLA- 100 alloy Specifically, the
martensmc mlcrostructures that develop in the simulated, coarse-grained heat-affected zones
(HAZs) have been examined and compared with those that develop in the base plate dunng con-
ventlonal quenching from the austemtlC phase field It has been shown that the lath martensltlC
packet size is increased dramatically in the HAZ as compared with the base plate In addition,
considerably more retamed austenite is found in the HAZ No ewdence for the so-called granular
balnite mlcroconstltuent has been found in either material However, for coohng rates somewhat
less than that experienced in the coarse-grained HAZ, a mlcroconstltuent that we term granular
fernte has been documented
Finally, the effect oftempenng on the martenslte in the base plate has been examined As soon
as they are observable, the copper (Cu) preopltates can be identified as face-centered cubic (fcc)
e-Cu
KEY WORDS: steels, martens~te, granular balnlte, granular ferrlte, copper precipitates, welding,
heat-affected zones, transmission electron microscopy, scanning electron microscopy, light
microscopy, metallography, metallurgmal specimens, microstructure, metallographlc
techniques
This paper is concerned with a metallographlc e x a m i n a t i o n of a new class o f steels that are
designated as H S L A - 1 0 0 Transmission electron microscopy (TEM), scanning electron
microscopy (SEM), and hght microscopy have been used to d o c u m e n t the p r e d o m i n a n t l y
martensltlC microstructures that develop in these alloys H S L A - 100 displays superior welda-
bihty and hence, as part o f an overall investigation o f the material, the coarse-grained heat-
affected zone ( H A Z ) has been simulated usmg a Gleeble and analyzed metallographlcally, pri-
marily by T E M In addition, the "base plate," which conventionally would be used in the
q u e n c h e d and t e m p e r e d condition, has been e x a m i n e d and c o m p a r e d with the H A Z
Previous studies [I,2] have indicated that "granular b a m l t e " might form In these steels
Smce the introduction of this terminology [3] to describe certain morphological features found
in hardenable steels, it has been often used in the literature, despite the lack o f a clear consensus
as to the strict nature of this transformation product In addition, there is no consensus con-
c e r n m g the phases, morphology, and the disposition of the phases that constitute granular
Research associate and professor of Metallurgy, respectively, Department of Materials Science and
Engmeenng, The Pennsylvania State University, University Park, PA 16802
199
Copyright9
Copyright by ASTM
1993 Int'l (all
by ASTM rights reserved);Www.astIII.OI'g
International Thu Dec 29 00:42:12 EST 2011
balnlte [4,5] Hence, one of the major goals of the study was to obtain unambiguous evidence
for the presence (or more likely, the absence) of this mlcrostructural entity To obtain this
"evidence," the present study has also employed cooling rates somewhat less than those expe-
rienced in either the HAZ or the quenched base plate
Experimental Approach
The composition of the expenmental material is given in Table 1 For the coarse-grained
HAZ studies, 6-mm-dlameter rods were machined and were weld s~mulated to a peak tem-
perature of 1320~ followed by cooling at a rate of 20~ through the 800 to 500~ temper-
ature range This simulation corresponds to a heat input of about 2 kJ/mm for the plate thick-
ness involved The simulation was performed on a Gleeble, courtesy of the David Taylor
Research Center, Annapolis, Maryland In addmon, continuous cooling transformation stud-
ies were performed on 5-mm-thlck samples by air cooling from 900~ at a rate of 7 5~ For
the present analysis on tempering of the HSLA-100 steel, 6-mm buttons (thickness = 6 mm)
were reaustenltlzed at 9000C for 15 m m and then water quenched at a rate of 40~ The
samples were then tempered at 600~ for times ranging from 30 rain to 48 h
Specimens for light microscopy and SEM were prepared through standard metallographlc
practices [6] and were etched in nltal or a mixture of nltal and plcral Thin foil specimens for
TEM analysis were prepared by first grinding 1-mm-thlck slices on a 400/600-grit silicon-car-
bide (SIC) paper to a thickness of 75 to 100 um Three-mllhmetre-dlameter disks were sub-
sequently punched, glued to a steel block, and further ground to a 35 to 50 #m thickness on
600-grit SIC paper After removing the disks from the block, they were then electropohshed to
electron transparency in a twin-jet electropohshlng unit using an electrolytic mixture consist-
ing of 95% acetic acid and 5% perchlorlc acid at room temperature TEM examinations were
carried out using a Phxhps EM420T at an accelerating voltage of 120 kV

The Mlcrostructure of the Coarse-Grained H A Z
The mlcrostructure of the simulated coarse-grained HAZ (peak temperature 1320~ and
coohng rate approximately 20~ consisted of very large packets ( ~ 50 um in diameter) of
lath martenslte as shown in F~gs 1a and b The laths are typically 0 2 to 0 4 um wide Reference
to Fig 1b shows that what might be termed "granular features" are present (arrowed)
TEM examination of the HAZ confirmed the presence of lath martenslte (for example, see
Fig. 2a) and it can also be seen that there are lnterlath films that appear dark in the bright field
(BF) image Centered dark field (CDF) images of the latter regions (for example, see Figs 2b
and c) show that these lnterlath films are retained austenlte (Figs 2b and c were imaged using
an 002 austemte reflection, see also Fig 8c) Reference to Figs 2b and c also shows that e-
copper (c-Cu) precipitation is absent m the CDF images (since both 7 and e-Cu are related to
the ferrlte by the Kurdjumov-Sachs OR [ 7,8], then a fraction of any e-Cu that might be present
should also be illuminated in the austenlte CDF image) This is not surprising, considering the
relatively rapid coohng rate However, the possibility of copper-rich Gurnler Preston (G P )
TABLE l--Chemtcal ~omposttton o/the HSLA-IO0 steel (percent by wetght)
C Mn P S SI Cu NI Cr Mo A1 Nb
004 082 0014 0002 032 1 59 345 058 051 003 003
VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 201
FIG 1--Ml~rostructure o/the coarse-gramed HA Z (stmulated /or a weld heat input of 2 kJ/mm) m the
ItSLA-IO0 alloy Coohng rate ~ 20~ (a) Ltght mt~rograph o/ the ba~l~ martemmc structure, and (b)
SEM mt~ rograph o/the lath ~tructure Narrow, elongated mterlath con~tttuent~ are also present
zones belng present cannot be discounted Finally, no evidence for granular bamlte was found,
and the occasional, large ferrltlC regions that were observed were found to be twinned as shown
In the BF-twln CDF image pair of Fig. 3 Hence, it can be concluded that the m~crostructure
in the HAZ is comprised of lath martenslte together with retained austenlte
The Ml~ro~tructure o f the Quenched Base Plate

Details of the material that has been reaustenltlzed at 900~ and quenched are to be pub-
llshed elsewhere However, for the sake of completeness and to facilitate a comparison with
the HAZ, a brief description follows Figures 4 and 5 are a hght mlcrograph and BF TEM
image, respectively, of the quenched material The quenched materml ~s fully martensltlC, con-
FIG 2--(a) TE~I b~l#llt held (Bk) mlaL,e o/the lath mlcrosmr (b and c) ('Dk lma~,es o/retained
altsfclll{~" (002 atl~{eHll~, r~,/le~lion ~)
FIG 3--(a) s Bk lmage of a lar,~e martensttlC ~t am that contam~ ~ne-s~ a/e t~ ms (b) r
twin CDb tmage
FIG 4 - - L i g h t mlcrograph o[ the quen6hed base plate
FIG 5--BF tmage o[ the lath rnartenstte Free ntobmrn-~arbMeprectpttates are pre;ent
SlStlng prlmardy of fine laths with widths of the order of 0 1 to 0 2 ~m and several microns In
length Generally, th~s length ~s hmlted either by the block &menslon or the packet s~ze At
th~s point, it can be noted that the laths m the HAZ could be as long as 50 um that was the
approximate packet size Now, reference to Fig 4 reveals a number of regions that are hghtly
etched and again could be IdenUfied as granular bmmte However, TEM analysis provided no
ewdence for such a m~crostructure and the only other m~croconst~tuent found m the quenched
material was retained austemte, located primarily at the mterlath boundaries as also noted in
other low-carbon steels containing mckel and chrommm [9] In contrast to the HAZ, the vol-
ume fraction of retained austemte was very small In common w~th the HAZ, some large inter-
nally twinned regions were observed occasionally These large internally twinned martensmc
units are occasionally observed m low-carbon steels [10]
The Effect o f Tempering on the Quenched Base Plate

Figures 6 and 7 are hght mlcrographs of samples that had been tempered for 2 h and 48 h,
respectively, at 600"C At these magnifications, there seems to be httle &fference in the two
materials However, TEM examinations reveal that substantial m~crostructural changes occur
during extended tempering treatments
After 3 h aging (Figs 8a and b), the lath structure is stdl preserved and a fine dispersion
( ~ 25 nm m diameter) ofe-Cu has developed both on the lath boundaries and within the laths
The C D F image of copper precipitates seen m Fig 8b has been formed by the combined (002)
3,/e-Cu reflection as shown in Fig. 8c (austemte and e-Cu both being fcc and have slmdar lattice
parameters, the 002 diffraction spots coincide) The C D F image m F~g 8b also reveals the
presence of stabilized austemte in the m~crostructure after aging After 10 h of aging, the lath
structure is replaced partially by eqmaxed fernte (Fig. 9a) although certain regions still retain
FIG 6--Light mlcrograph o/the ba~e plate after tempering/or 2 h at 600~
vestiges of the lath structure (Fig 10) C D F images of the precipitates formed by the (002)
copper reflection confirms their identity as e-Cu Comparison of Figs 9 and l0 with that of
Fig 8 shows that the copper precipitates have coarsened considerably after l0 h and many of
the larger lntragranular particles are assuming a rod-like morphology After 48 h aging, the
dominant femtlc morphology is equlaxed (Fig 1 l) although, in c o m m o n with the 10-h aged
material, certain regions still retain a lath-like morphology (Fig 12) Reference to Fig 11
shows a number of coarse e-Cu preopltates on the gram boundaries
FIG 7--Ltght mlcrograph o! the ba~e plate after tempering/or 48 h
FIG 8--(a) T L M B F linage o/the lath structure and ( opper preclpttates, (b) austemte/e~-Cu CDF image,
and(c) s'elected area dl/]ractmn pattep n (SADP) o[ Ftg~ 8 a and b The 002 rejle~twn wa~ u~ed to /orm Fig
8b
The Mlcro~truc ture o / A i r - C o o l e d Sample~ o f the Base Plate
Specimens that were reaustenmzed at 900~ and cooled at 7 5~ were examined m order
to (hopefully) develop ferrlte/martenslUc mlcrostructures that could correspond to what has
been termed "granular balnlte "Reference to Fig 13 shows that a dual-phase, ferrlte plus mar-
tens~te, m~crostructure develops The martenslte was found at the equlaxed fernte grain
FIG 9--(a) T I i ~1 B1~ m ~ a f e cd c oa~ ~ened coppcr prcc zptzazes a/let ] 0 h a~.n~~ (b a~ld c) ( ' D I ~ zrna~c
l o o m e d ~ zt h the 002 ~-( zl t e/lc,~11on
boundailes, and somewhat mtcrestlngb within the ferrlte grams (Figs 14a and b) This latter
mlcroconstltuent, fernte plus entrapped pools ot martenslte could be termed granular bamlte
However we would argue that granular fernte is a more appropriate designation since this
mlcroconsntuent, predominantly fernte plus martenslte, does not conform to either of the
current defimtlons of bamlte that are (for steels)
FIG I O--BF tmage o/the lath-hke mtcrostructure after lO h o! agmg
FIG 11 --Coarse prectpttate~ o[ copper on the gram boundartes after 48 h agmg
FIG 1 2 - - B F tmage oJ the 48-h aged material Remnants of a lath morphology are observed
FIG 13--(a) Ltght mlcrograph o/specimen ~ooled at 7 5~162 A granular morphology Is present (b)
T L M Bk linage the stru~lure is a dual phase, ~on.~Istmg o/equtaxed !errtle and marten site
FIG 14--1nlragranularpools o! marlenstte m the aw-( ooled material (7 5~ (a) Bb and (b) ~orre-
spondmg marten stte C D F t mage
1 A nonlamellar aggregate of fernte plus cementlte [11]

2 A lath or plate-hke ferrltlc product that forms by shear [12]
At th~s point, ~t should be pointed out that, in the present investigation, mlcrostructures slm-
dar to that presented in Figs 13 and 14 have not been found in either the HAZ or the quenched
base plate This again reinforces our claim that these latter regions are predominantly lath mar-
tensltlc together wxth retained austenlte as the second phase constituent
Conclusions
The major findings of the present investigations are as follows
1 The coarse-grained HAZ transforms to a coarse lath martenslte during coohng. Austen-
lte is retained as thin interlath films
2 The quenched base plate is also compnsed of lath martenslte, but on a finer scale L~ttle
retained austemte was observed
3 No granular balmte/fernte was found in either the HAZ or the quenched base plate
4 Tempering the quenched base plate led to the development of a dispersion ofe-Cu. The
lath structure was replaced generally by a more eqmaxed ferntlc structure.
5 Granular fernte was found m the air-cooled sample We suggest that the designation,
fernte, is far more appropriate than what has been used heretofore, bamlte
Acknowledgments
The authors gratefully acknowledge the support of The Office of Naval Research Grant
Number N00014-89-J 1958
References
[1] Wilson, A D, Hamburg, E G , Colvm, D J, Thompson, S W, and Krauss, G m Mlcroalloyed
HSLA Steels (Proceedmgs Mtcroalloymg "88), Amencan Society for Metals, Metals Park, OH, 1988,
p 259
[2] Thompson, S W, Colvm, D J, and Krauss, G , Scrlpta Metallurgtca, Vol 22, 1988, p 1069
[3] Habraken, L J and Economopoulos, M m Transformatton and Hardenablhty in Steels, Chmax
Molybdenum Company, Ann Arbor, MI, 1967, p 69
[4] Bramfitt, B L and Speer, J G , Metallurgtcal TransacttonsA, Vol 21A, 1990, p 817
[5] Ohtam, H, Okugach~, S, Fujlshlro, Y, and Ohmon, Y, Metallurgical TransacUons A, Vol 21A,
1990, p 877
[6] Vander Voort, G , Metallography-Prmctples and Pracltces, McGraw-HJll, New York, 1984
[7] Honeycombe, R W K in Phase Transformations m Ferrous Alloys, A R Marder and J I Gold-
stem, Eds, The Metallurgical Sooety of the American InsUtute of Mining, Metallurgical, and Petro-
leum Engineers, Warrendale, PA, 1984, p 259
[8] Howell, P R, Ricks, R A, and Honeycombe, R W K, Journal ofMaterlals Science, Vol 15, 1980,
p 376
[9] Thomas, G , Metallurgtcal TransacttonsA, Vol 9A, 1978, p 439
[10] Wayman, C M in Phase TransformaltonsmFerrousAlloys, A R MarderandJ I Goldsteln, Eds,
The Metallurgical Sooety of the Amencan Institute of Mining, Metallurgical, and Petroleum Engi-
neers, Warrendale, PA, 1984, p 49
[11] Aaronson, H I, Reynolds, W T, Jr, Shlflet, G J, and Spanos, G , Metallurgzcal TransacttonsA,
Vol, 21A, 1990, p 1343
[12] Olson, G B, Bhadeshla, H K D H, and Cohen, M, Metallurgwal Transacttons A, Vol 21A, 1990,
p 805
Lucille A. Giannuzzi, ~Paul R. Howell, l H o w a r d W. Pwkerlng, 1 and
William R. Bltler ~
Transmission Electron Microscopy of the

Interdiffusion Regions of Iron-Zinc Couples
REFERENCE: Glannuzzl, L A , Howell, P R , Plckenng, H W , and Bltler, W R , "Trans-
mission Electron Microscopy of the Interdiffusion Regions of Iron-Zinc Couples," Metallogra-
phy Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Vander
Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Sooety for Testing and
ABSTRACT The iron-zinc system has been studied frequently due to the fact that zinc inhibits
corrosion of the ~ron by cathodic protection However, there are discrepancies in the literature
concerning both the nature of the mtermetalhc phases that can form in Iron-zinc (Fe-Zn) alloys
and the detads of the Fe-Zn phase diagram Many of the problems that are associated with this
system can be attributed to the difficulty of prepanng homogeneous alloys of known composi-
tions because of the high vapor pressure of zinc relative to iron For many of the same reasons,
it has proved difficult to produce thin foils for examination in the transmission electron micro-
scope (TEM) from blmetalhc Fe-Zn matenals Transmission electron microscopy of the blme-
talhc Fe-Zn couple in cross sectmn ~s desirable because m~crostructural reformation by ~maglng
techniques, phase identification by dlffractmn techmques, and chemical analysis by energy &s-
perslve spectroscopy can be achieved w~th one instrument
In the present investigation, a sample preparation techmque for the production of cross-sec-
tion TEM foils of Fe-Zn couples is described in detail In an attempt to obvmte the problem
associated with the thinness of commercial Fe-Zn couples, pure Fe-Zn couples have been pro-
duced that are in excess of 3 mm m thickness These samples can be cut directly to the required
dlmensmns for thin foil preparation Electron transparency has been achieved by liquid nitrogen
ion mdllng with specimen dlmphng Prehmlnary results from the zinc side of the Fe-Zn couple
are presented The zeta (~) phase has been identzfied, and It xsbeheved that these are the first TEM
m~crographs and electron diffraction patterns ofth~s phase observed from cross-sectioned Fe-Zn
couples The mlcrostructural evolution of the n (Zn) ~ ~ + ~"~ ~"phase transitions within the
&ffUSlOn zone is discussed
KEY WORDS" transmission electron microscopy, selected area dlffractlon pattern, rt phase, ~"
phase, mn mdhng, ~ron-zme couple, metallography, metallurgical specimens, mlcrostructure,
metallographlc techmques
Recently, m u c h a t t e n t i o n has been given to the analysis o f zinc-based steel coating systems
by t r a n s m i s s i o n electron m i c r o s c o p y ( T E M ) (see for example, Refs 1 t h r o u g h 8) O b s e r v a t i o n
o f the zinc-coated steel c o u p l e in cross section by T E M (or m o r e specifically analytical electron
m i c r o s c o p y ( A E M ) ) c o u l d be a d v a n t a g e o u s because the m o r p h o l o g y , chemistry, a n d structure
o f the lnterdlffUSlOn region m a y be d e t e r m i n e d In a d d i t i o n , t h e n a t u r e o f any i n t e r m e d i a t e
phases c o u l d be d e t e r m i n e d T o f a o h t a t e later discussion, T a b l e 1 lists the i n t e r m e d i a t e phases
t h a t h a v e b e e n f o u n d to o c c u r in the i r o n - z i n c ( F e - Z n ) system [9]
Post doctoral research associate, Center for Advanced Materials and professors of Metallurgy, respec-
tively, Department of Materials Science and Engineering, The Pennsylvania State Umverslty, University
Park, PA 16802
212
Copyright
Copyright*by1993
ASTMbyInt'l
GIANNUZZl ET AL ON IRON-ZINC COUPLES 213
TABLE 1--lntermedtate phase3 m the Fe-Zn system
Approximate Composition Range

Phase Crystal Structure at 450~ (atomic % Zn)
F cubxc (bcc) 68 5 to 73 5
F~ cubic (fcc) 78 0 to 81 0
hexagonal 86 5 to 92 0
~" monochnlc 92 5 to 94 0 (FeZnj3)
However, preparation of the lnterdiffUSlOn region of an Fe-Zn couple for TEM analysis is
nontrivlal For example, a c o m m o n techmque for prepanng conventional alloys for TEM IS
twin-jet electropohshlng. However, the role of zinc is to inhibit corrosion of the iron by cath-
odic protection and, therefore, the great difference in chemical reactivity between the zinc and
iron has thus far precluded jet polishing as a viable technique. As a result, TEM sample prep-
aration of Fe-Zn couples in cross section have concentrated on the techniques of ion beam
milling [ 1-4] and ultramicrotomy [5,6]. The physical properties of zinc (for example, the high
vapor pressure of zinc relative to iron) add to the uniqueness and difficulty in preparing TEM
foils m this system For example, it has been shown that zinc is extremely sensitive to damage
induced by ion bombardment d u n n g Ion beam mllhng [1,4] In addition, previous studies in
this laboratory have suggested that Fe-Zn intermediate phases may form during ion beam mill-
ing, even when a liquid nitrogen cooling stage IS being used, due to the redeposition of sput-
tered zinc onto the iron-based substrate [2, 7,8]
A recent study in this laboratory has shown that the steel-zinc interface may be imaged by
TEM using the technique of mechanically polishing to electron transparency, however, the
steel substrate is damaged and the zinc coating is recrystalllzed [1] Subsequent 1on milling
using a hqmd nitrogen coohng stage was shown to remove the mechanically damaged region
and revealed a mlcrostructure that was consistent with the starting material Unfortunately,
the interface could not be imaged due to the faster ion milling rate of zinc with respect to iron
Therefore, it was concluded that optimum sample preparation conditions for cross-section
analysis of Fe-Zn couples must minimize the degree of mechanical polishing in order to avoid
specimen damage, and shorten ion mill times to avoid preferential thinning and ion beam
damage In the present study, the lnterdlffusion region of an Fe-Zn couple has been observed
successfully by TEM utilizing the dimpling-liquid nitrogen ion milling technique of sample
preparation
Experimental
Fe-Zn Btmetalhc Couple Producuon
In an attempt to obviate the problem associated with the thinness of commercial Fe-Zn cou-
ples, pure Fe-Zn couples have been produced that are in excess of 3 m m in thickness A thick
zinc coating was electroplated onto the iron substrate so that a sample may be cut directly to
the required dimensions for thin foil preparation
A specially prepared "pure" lron-electrogalvamzed zinc couple was prepared courtesy of C
Cheng of Inland Steel A 50-mm iron ingot was hot rolled to 12 5 mm, then to 2 54 m m The
2 54-mm sheet was then cold rolled over several passes to a final thickness of 0 75 mm. The
composition of the iron sheet is listed in Table 2 Prior to electroplatlng, the iron sheet was
degreased in acetone, followed by an alkaline electrocleaner and was then activated by a 10%
sulfuric acid (H2SO4) solution Thereafter, it was plated in a conventional zinconium sulfate
TABLE 2--1mpuray content of iron sheet (ppm)
C Mn P S SI Al As T~ Sn Cu
50 < 10 90 80 160 250 20 2000 100 20
(ZnSO4) bath at a current density of 4 8 A/dm 2 (the pH was controlled between 1 2 to l 8)

The plating process was carried out over a period of 24 h To avoid surface roughness due to
dendritic growth, the surface of the zinc coating and edge of the sample were mechanically
smoothed every 30 m m d u n n g electroplatmg The ZnSO4 was added to the bath every 30 rain
to maintain the bath composition The final thickness of the zinc-coating plated onto both
sides of the iron sheet was ~ I m m ( ~ 700 g/m 2 of zinc), thereby producing a couple thickness
of ~ 3 m m
Fe-Zn Heat Treatment

The as-received Fe-Zn sheet was sliced into strips of ~ 15 m m by 50 m m using a diamond
wafenng blade Each stnp was degreased in acetone and encapsulated in Vycor tubing Zinc
powder of 99 7% p u n t y was poured into the tubing until the Fe-Zn stnp was covered com-
pletely The assembly was topped with quartz wool that acted as a heat sink d u n n g necking of
the tubing. The assembly was then evacuated to 30/Lm Hg and sealed The encapsulated Fe-
Z n couple was annealed at 450 ~ _+ 2~ for l0 min and water quenched It should be appreci-
ated that the annealing temperature is above the melting point of pure zinc (419 58~ and
was chosen to reproduce the temperature in which hot-dip galvanizing of steels occur.
T E M Sample Preparation
A specimen for TEM analysis was prepared in the following manner The heat-treated Fe-
Z n couple was sliced m cross section to a thickness of ~ 1 m m using a diamond wafenng blade
The thickness was reduced further to ~ 100 um by grinding on sdicon-carbide (SIC) papers
with lapping od as a lubricant The specimen was dimpled in the vicinity of the interdiffuslon
region to < 5 ~m in thickness using 6-urn and 1-1zm diamond paste The specimen was
trimmed to a diameter suitable for TEM examination ( ~ 3 ram) Final TEM thinning was
achieved by ion milling with a liqmd nitrogen cooling stage until the Fe-Zn interface was per-
forated The couple was positioned inside the ion mill such that the argon beams were per-
pendicular to the interface for the majority of the milling time A light optical micrograph of
the perforated speomen is shown in Fig l Note that the thickness of the diffusion zone (DZ),
which is ~ 4 0 #m, is visible due to the ion milling procedure Note also that the perforation is
w~thm the diffusion zone on the zinc side of the couple, and, therefore, mlcrostructural infor-
mation by TEM on the iron side of the couple was not attainable The labels, a, b, c, and d,
around the perforation represent the approximate locations m which TEM analyses were per-
formed Position a is located in the zinc coating, and positions b, c, and d are points within the
diffusion zone that progress toward the iron-nch side Reference to these positions will be
made in the following section There is also evidence of pores (P) within the thick zinc coating
that may be due to the collapse of as-plated dendrites d u n n g the annealing operation. The
feature labeled T is a trench formed in the couple due to the direction of ion milling as
described earlier The specimen was examined in a Phlhps EM420T operating at 120 kV
FIG 1--4 ~ro.~~-~ectmn hght optical rm~ rograph o/an Fe-Zn couple annealed at 450~ ]or 10 mm a[ter
dimpling and ton mllhng with a hqmd mtrogen cooling ~mge (see text/or the lull de~ rlptlon)

Fzgure 2a is a bright field (BF) mlcrograph of the zinc-rich eta phase (~), and Fig 2b is a
[0001] selected area diffraction pattern (SADP) from the region shown in Fig 2a Confirma-
tion of the indexing scheme is provided m the computer-generated pattern obtained in Fig 2c
Note the extended dislocations in Fig 2a that may have formed as a result of sample prepa-
ration The diffusion zone width and locations of the TEM analyses shown in Fig 1 are
approximate Nevertheless, the relative positions of the TEM images within the diffusion zone
will be mentioned to emphasize phase boundary transitions Figure 2a was imaged from Loca-
tion a in Fig 1
Figures 3 through 5 present micrographs dlustratlng vanous features of second-phase par-
tlcles (Figs 3a, 4a, and 5a), corresponding SADPs (Figs 3b, 4b, and 5b) and computer-gen-
erated patterns (F~gs 3c, 4c, and 5c) taken from each region The diffraction patterns index
consistently with the monochnIc Fe-Zn zeta (~-)phase The SADPs were indexed by companng
d-spacings and diffraction patterns obtained by computer simulation. The complexity of cal-
culating electron diffraction patterns from the ~"phase (as well as other complex crystal struc-
tures) is greatly diminished by employing computer calculations The computer simulations
m F~gs 3c, 4c, and 5c were generated using a = 1 086 nm, b = 0 761 nm, c = 0.506 nm, and
fl = 100 53 ~ [10] A base-centered monochnlc lattice was defined (that is, atom locations at
(0,0,0) and (0 5,0 5,0)) to yield matching extinctions of reflections present between the actual
and computed SADPs The indexing scheme reported in h g s 3c, 4c, and 5c are therefore con-
Slstent with the preceding crystallographic data Ftgure 3c indexes to [101], F~g 4c to [010],
and Fig 5c to [ 121 ] Figures 3a and 5a were imaged from Location d, and Fig 4a was imaged
from Location c m Fig 1 To our knowledge, these are the first published TEM ~mages and
electron dlffracUon patterns of the ~"phase obtained from cross-sectioned Fe-Zn couples
The ~"phase may appear as a d~screte particle within the )7 matrix ( ~ 0 . 5 to 1 ~m) as shown
by the example given m Fig 6 (Location b, Fig 1), as particles that have coalesced (F~g 4a),
or as larger single-crystal grains (Fig 5a), depending on the location within the diffusion zone
Thus far, it has been shown that, in general, as the distance into the diffusion zone from the
zinc side of the Fe-Zn couple increases, the number density of the ~'phase increases The pres-
ence o f twins m the f phase has been confirmed by electron d~ffraction lndwidual ~"particles
FIG 2--(a) Brlght field (BF) T E M ml~rograph of the zm~-rtch ~ phas'e, (b) a [0001] selected area dtj-
fractwn pattern (SADP), and (c) computer generated pattern from the area m Ftg 2a
GIANNUZZI ET AL ON IRON-ZINC COUPLES 217
FIG 3--(a) Centered dark ~eld (CDF) mlcrograph of the ~ phase, (b) a [ 101] SADP and (c) computer-
generated pattern fiom the area in Fig 3a
FIG 4--(a) B F mlcrograph o f the ~ phase, (b) a [010] SADP, and (c) computer generatedpattern from
the area m Fig 4a
FIG 5--(a) BF mzcrograph of the ~phase, (b) a [121] SADP, and (c) computer-generated pattern from
the area tn Ftg 5a
and the coalesced ~"region may contain twins, however, addmonal analyses are needed to
determme whether the various features m F~gs 3a and 5a are possible twins, stacking faults,
or antlphase boundaries Figures 7a and b are a BF and centered dark field (CDF) mlcrograph
of the same region Centered dark field imaging is useful for determining regions that have
s~mllar orlentaUons The usefulness of the C D F image is illustrated m Fig 7b where the large-
grained r/matrix appears bright due to virtually ~denucal orientation The particles are con-
tanned within a smgle zinc-rich ~ gram as illustrated by the contrast m Figs 7a and b, and the
single crystal [2110] SADP from the ~ region The computer-generated indexed SADP for Fig
7c is shown m Fig 7d The lower magmficatlon C D F image of Fig 8 again illustrates the single
crystal nature of the zinc-rich 7/matrix, individual ~"particles, and the onset of ~"parhcle coales-
cence Note again that in the C D F mlcrograph of Fig 8 the single crystal orientation of the 7/
FIG 6 - - B P lrnage o/an isolated f phas'e parttde wtthm the o matrix
phase is emphasized by the relatively uniform image intensity Conversely, the particles m the
CDF mlcrographs appear dark Figures 7a, 7b, and 8 were imaged from Location b in Fig 1
A schematic diagram for the mlcrostructural evolution of the n ---"n + ~'~ ~'phase transition
Is illustrated in Fig 9 and described in the ensuing text Figure 9a begins with a large single
crystal zinc-rich n matrix (compare with Fig 2a) At the beginning of the diffusion zone (on
the zinc side of the Fe-Zn couple) isolated ~"particles probably nucleate within the liquid (L)
phase (which, upon coohng, transforms to the solid ~ phase see Fig 9b and Figs 6,7a,7b, and
8) As the distance into the diffusion zone increases, the volume fraction of the ~ phase in the
two-phase region (L + ~') increases by additional particle nucleation and pre-existing particle
growth Upon cooling, (L + ~') transforms to (n + ~) In addition, the onset of particle coales-
cence also takes place (compare Fig 9c with Figs 4a, 7a, 7b, and 8) Finally, complete particle
coalescence is attained (Fig 9 d a n d Fig 5a) and the single phase ~'reglon is produced contain-
ing defects that definitely include twins, and may contain stacking faults, and antlphase
boundaries Figures 9a through 9d can be correlated with positions within the diffusion zone
shown by Locations a through d m Fig 1
Conclusions
A successful TEM sample preparation techmque for the analysis of the mterdiffuslon region
of Fe-Zn couples, has been described. It is believed that the first TEM images and electron
diffraction patterns of the ~"phase from cross-sectioned Fe-Zn couples have been presented in
this paper Additional research is needed to fully characterize the defects present m the ~"phase
A schematic diagram for the mtcrostructural evolution of the reaction ~ ~ n + ~"~ ~"has been
provided
GIANNUZZI ET AL ON IRON-ZINC COUPLES 221
<b
T~
FIG 8--Lower magnlhca[mn BF tmage show'mgthe dlstrlbutmn of ~fparttdes wzthm the. matrix and
the on sel o/~ partl~le ~oale~scence
Acknowledgment
The Fe-Zn couple was prepared courtesy ofC Cheng, Inland Steel This research was sup-
ported by the American Electroplaters and Surface Finishers Society Research Project No 76
and Inland Steel Corporation
References
[1] Glannuzzl. L A, Howell, P R, Plckenng, H W, and B~tler, W R, Proceedings, SUR/FIN '91.
American Electroplaters and Surface Finishers Socwty, Toronto. 1991, to be pubhshed
[2] Glannuzzl. L A, Howell, P R, lhckermg, H W, and Bltler, W R m Zinc-Based Steel Coating
Systems Metallurgy and Performance, G Krauss and D K Matlock, Eds, The MetallurgacalSoci-
ety of the American InsUtute of Mining, Metallurgacal.and Petroleum Engineers, Warrendale. PA,
1990, p 121
[3] Chen. Y L and Snyder, D D m Zmc-Based Steel Coating Systems Metallurgy and Performance,
G Krauss and D K Matlock. Eds. The MetallurgacalSociety of the American Institute of Mining,
Metallurgical, and Petroleum Engineers, Warrendale, PA, 1990, p 95
[4] Lm, Y, Pak. S -W, and Meshn, M m Zmc-Based Steel Coating Systems Metallurgy and Perfor-
mance, G Krauss and D K Matlock, Eds. The Metallur~cal Society of the Amencan Institute of
Mining, Metallurgical. and Petroleum Engineers, Warrendale, PA, 1990, p 109
[5] Drewlen, C A, Ackland, D, and Marder, A R m Zinc-Based Steel Coatmg Systems Metallurgy
and Performance, G Krauss and D K Matlock, Eds. The Metallur~cal Society of the American
Institute of Mining, Metallurgical, and Petroleum Engineers, Warrendale. PA, 1990, p 31
[6] Takahashl, A, Mlyoshl, Y. and Hada. T m Zinc-Based Steel Coating Systems Metallurgy and
Performance, G Krauss and D K Matlock, Eds, The Metallurgical Society of the American Insti-
tute of Mining, Metallurgical, and Petroleum Engineers, Warrendale, PA, 1990, p 83
GIANNUZZI ET AL. ON IRON-ZINC COUPLES 223
FIG. 9---A schematic diagram of the microstructural evolution of the n ~ n + ~ ~ ~phase transition
(see text for full description).
[7] Giannuzzi, L. A., Howell, P. R., Picketing, H. W., and Bitler, W. R., Proceedings, SUR/FIN '90,
American Electroplaters and Surface Finishers Society, Boston, 1990, p. 381.
[8] Giannuzzi, L. A., Howell, P. R., Pickering, H. W., and Bitler, W. R., Microstructural Science, Vol.
19, to be published.
[9] Kubaschewski, O., Iron-Binary Phase Diagrams, Springer-Verlag, Berlin, 1982, p. 173.
[10] Gellings, P. J., de Blee, E. W., and Gierman, G., ZeitschrifteJfirMetallkunde, Vol. 70, 1979, p. 315.
James Hillier I
Some Reflections on the Early Development of

Electron Microscopy and Microanalysis
REFERENCE: Hllher, J, "Some Reflections on the Early Development of Electron Microscopy
and Microanalysis," Metallography Past, Present, and Future (75th Anntversary Volume),
ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amer-
ican Society for Testing and Matenals, Philadelphm, 1993, pp 224-232
ABSTRACT: Theoretical mathematscal physics estabhshed the posslblhty of an electron micro-

scope long before the discovery of the electron Much later, theoretical physics provided the
incentive for developing an electron microscope The reahzaUon of a working instrument had
to await the maturaUon ofa w~de spectrum of new technologies Recollections of the successes
and heartbreaks of the early days of this struggle, at the Umverslty of Toronto and then at RCA,
provide the background for some mterestmg thoughts on the importance of t~mmg and chance
in such developments In the middle 1930s, technologies were emerging that made the trans-
mission electron microscope possible By contrast, electron microprobe analys~s could not
become pracucal untd at least two decades later when the much more demanding technologies
reqmred had been developed
KEY WORDS" electron m~croscope, electron microprobe analysis, transmission, h~story, tech-
nological infrastructure, metallography, metallurgical speomens, mlcrostructure, metallo-
graphic techmques
In a s y m p o s m m celebrating the 75th Anniversary o f the formation o f the A S T M C o m m i t t e e

E4 on Metallography, it is very appropriate to have a discussion of the early days o f an instru-
m e n t as significant as the transmission electron microscope (TEM) It is also appropriate to
give s o m e thought as to the helpful impact our past experiences might have on the evolution
and d e v e l o p m e n t o f future instrumentation The period I shall be discussing will be the decade
from 1935 to 1945 T h a t is about two-thirds of the way back to the origin of C o m m i t t e e E4
and safely beyond the reach of most o f your m e m o r i e s
It was a most exciting, even spectacular, decade during which a remarkably small group of
researchers scattered around Europe and North America, took the magneuc T E M from a
rather quiescent, theorettcal concept to a reasonably rehable, practical instrument in senal
p r o d u c u o n . In the s a m e period, this group took the resolving power from a doubtful third of
a m~crometre to a routine resolving power o f ten n a n o m e t r e s and, in the hands of experts, to
an occasional one n a n o m e t r e In this decade, the fields of applicaUon o f the T E M were
expanded from essentially zero to almost the full range o f the hght microscope There was not
yet any way of cutting sufficiently thin sections o f biological specimens That occurred a year
or two later Color, as used so valuably in light microscopy, did not seem to have a counterpart
In electron microscopy
It ~s revealing to w o n d e r why the T E M c a m e into being in that particular decade The cor-
relaUon between the refraction o f hght rays and the action o f fields o f force on pamcles had
' Retired, RCA Corporation
224
Copyright
Copyright*by1993
ASTMbyInt'l
HtLLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 225
been elucidated by Hamilton m the middle of the nineteenth century, long before the forma-
tion of Committee E4 and long before the discovery of the electron The wave nature of the
electron and Its extremely small wavelength had been understood for more than the preceding
decade The theoretical posslbfi~ty that an electron microscope, that was the analog o f a hght
microscope could have much greater resolving power, had been qmte well accepted for several
years before the early 1930s when Knoll and Ruska attempted ~ts construcUon In my opimon,
the state of our technological infrastructure is a most sigmficant controlhng factor m the t~mmg
of the transition from a concept to a practical device. Certainly, with the TEM and m~croprobe
analys~s we have two contrasting examples of this point and, for which, my own expenences
prowde good support. (Incidentally, it IS interesting that none of the acUve workers m the field
ever claimed to have "invented" the electron microscope )
Our First Instrument

In early spnng, 1937, I was a senior about to graduate in mathematics and physics at the
University of Toronto In a discussion about my future with the assistant chairman of the
physics department, he happened to mention the electron microscope, m which, it appeared,
the chairman of the department had some interest. My curiosity was immediately aroused
That was the very first time I had encountered that particular combination of the words "elec-
tron" and "microscope." As a child, I had been very interested In microscopes and had even
made several crude light microscopes As a teenager, a high school geography teacher had
roused an interest in ham ra&o I was completely mystified as to how these two acUvltles could
be related I was intrigued and my career was launched I &d a lot of reading that summer. In
the fall, I was joined by A1 Prebus and we got some practical experience by rejuvenating a
couple of emission type microscopes that Cecd Hall had built before he left for Kodak By the
end of the year, we had reached the conclusion that the only way we could achieve resolving
powers better than a light microscope was to construct a h~gh-voltage, magnetic, transmisszon
instrument We spent the Christmas break designing our first instrument Looking back, I am
stdl amazed We designed the column and did all the critical drafting m a few eighteen-hour
days Although the general pattern of the design followed that of Knoll and Ruska, we were
on our own as far as any of the engmeenng details were concerned We made some mistakes,
but it is remarkable that the projection lens, the objecUve lens except for its polep~eces, the
specimen chamber, and the column support were never changed
Over the years, I have always been impressed by the wisdom of the chairman and the assis-
tant chmrman for allowing two very young, very brash, zealous graduates undertake such a
major project on their own Recall, at the beginning of 1938, the country was still m the throes
of the Great Depression and the physics department was seriously strapped for funds The
chairman and his assistant were faced with a Hobson's choice Should they try to support a
large project in an impossibly austere environment or should they risk deflating two enthusi-
asUc graduate students who just might make a breakthrough It is to their credit that they
approved the project even though it was rather clear that, for the most part, we were going to
have to shift for ourselves
The only assistance available to us was that of the part-time efforts of a glassblower and of
the most recent addition to the machine s h o p - - a fellow whose prior employment was In a
locomotive repair shop v That shook us up but, actually, became one of the more fortunate
things that happened to us Fred was a delight at precision machining of very large pieces, but
anything that needed more than one part per inch completely confounded him Prebus and I
quickly realized that If the more complicated, delicate parts of our instrument were going to
be made, we were going to have to learn to do the machining ourselves That we did In later
years, for me at least, that experience was invaluable The many late hours I had spent m the
machine shop paid offhandsomely, primarily through the great advantage It gave me m com-
mumcatmg with instrument makers and machlmsts
So much for setting the scene Let us take a quick look at the technology we had avadable
then
By today's standards, the most laughable was the vacuum technology Except, to us, It was
very serious business The hagh-vacuum pump was a hand-blown glass mercury diffusion
pump, the largest that our glassblower could make We never really knew how fast ~t pumped
We estimated it to be somewhat under one htre per second The d~ffus~on pump was backed
by a small mechamcal pump Then, there was a maze of glass tubing and ground glass stop-
cocks that enabled us to bypass the mercury pump for the anatlal pumping of the instrument
Our vacuum gage was a monstrosity called a McLeod gage that gave us lots of physical exercise
but not more than one measurement per minute
That first instrument was a stack of lenses, tubes, a camera, an object chamber, and an elec-
tron gun Each piece was ahgned by shdmg it transversely relative to the group of segments
below it These junctaons were made vacuum taght by painstakingly hand lapping the shdmg
surfaces and seahng them with a special grease that we concocted ourselves. We spent many
hours surnng pure gum rubber very slowly into a pot of melted Vasehne In addmon to the
plane surfaces between segments, there were a number of lapped comcal plugs that provaded
access to the inside of our instrument
Our electrical components were equally primitive. The current supply to our lenses was sam-
ply a well-charged group of automobde batteries connected through large laboratory shdmg
variable resistors We d~d have a carcmt that prowded coarse, fine, and very fine adjustments
We also, very fortunately, had designed water-cooling into our lens coil structures to reduce
the thermal vanataons. However, they still took long periods to stabdlze Our hagh-voltage sup-
ply was an unbehevable concoction of parts that we scrounged from various nooks and cran-
rues around the physics department. It consisted of a very large 50 kV transformer, a mercury
vapor rectifier tube, and a filter capacitor made of glass plates and a l u m i n u m foal The only
place where one could possibly see anything comparable today would be m a very old Frank-
enstem mowe. Miraculously, ~t worked, although not very well. It turned out that the most
sophisticated ptece ofeqmpment, the mercury vapor rectafier tube, had a finng voltage with a
mind of ats own with vanataons that could not be smoothed out by our low-capacaty filter
system
In the design of our instrument, our most spectacular fadure was our camera. Recogmzmg
the slowness of our vacuum system and unaware of what problems we were going to encoun-
ter, we opted for a multiple exposure film camera Unfortunately, ~t took forever for the film
to outgas and when we d~d get adequate vacuum, any attempt to roll the film caused it to
fragment into a bunch of plastac shvers in the bottom of the camera
Applications Expand
In spite of these and many other problems, the instrument began to show promise and, as
~t d~d, some support began to dribble m from various Interested organizations.
It seems incomprehensible m today's world that, m the maddle th~rtaes, a few lndlwduais
were exerting enormous individual effort to develop a hlgh-resolutaon electron macroscope,
when the only type of specimen they were sure they could examine was no more exotic than
the cutting edge of a razor blade It was generally assumed that the contrast m an electron
image would be produced by the absorption of electrons m the specimen and, therefore, the
intensity reqmred to make a highly magmfied amage useful would immediately destroy any
but the most refractory specamen. Obviously, our dedlcataon had to be related to the challenge
HILLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 227
of achieving increased resolving power, rather than the ultimate, general utdity of the instru-
ment In mid-1938, just as we were beginning to get some promising pictures, we became
aware of Marton's 1937 paper in which he demonstrated that a sufficiently thin, suspended
film of collodion was not destroyed by the electron beam and could be the counterpart o f the
hght microscope shde It became apparent that differential scattering of electrons without
absorpUon could provide adequate contrast for the formation of an image Immediately, the
entire field of very fine particles (paint pigments, colloids, bacteria, viruses, etc.) was opened
up and the future o f the TEM as a useful instrument was assured
On to Serial Production
As we refined the Toronto instrument and our useful pictures became more frequent, our
reputation began to spread and we had more and more requests for micrographs of materials
of interest to an ever-widening spectrum of organizations. It became obvious that a homemade
"stnng and sealing wax" instrument in a university laboratory could not possibly meet the
demand As a result, in February 1940, I found myself at RCA designing a commercial version
of the Toronto instrument I also became aware that the technological infrastructure m the
electromcs industry was coming together rapidly and was far ahead of the university
We now had 50-htre-per-second oil diffusion pumps and continuously reading vacuum
gages We could achieve rapid demountabihty with synthetic rubber gaskets and O-nngs
instead of ground grease joints We had vacuum-tight flexible metal bellows that gave us new
freedom in deslgmng a means of manipulating within a vacuum chamber I am sure some high
vacuum technologists are cringing as I list these developments I can appreciate your reaction
now, but please recognize that they were miracles to us in 1940
On the electrical side, we moved into the electronics age with the newly developed, preci-
sion, self-regulating, high-voltage supplies and regulated current supplies that completely elim-
inated the need for cooling the lens coils.
All these, and other developments, speeded our work by at least an order of magnitude,
possibly much more If you think about that for a moment, you begin to realize that such
numbers practically guarantee the historical coincidence of the development of enabling tech-
nology and the emergence of a major new development However, it is interesting to note some
other changes between 1940 and today
The group I had assisting me at RCA consisted of an electrical engineer, a mechanical engi-
neer, one electronic technician, and access to the development fabrication shop. In just four
months, we designed, built and debugged what became the RCA Model EMB instrument to
the point where we were getting a resolution of around ten nanometres The total cost to RCA
was slightly over l0 000 1940 dollars. That would be between one and two hundred thousand
1991 dollars. Given the bureaucratic, environmental, and safety requirements in today's
world, I suspect that today, it would take several times as long and at least an order of mag-
nitude more money
An interesting sidelight is that, when he hired me to do this job, Dr Zworykm did not tell
me that he did not have any budget to support my work He was gambling on my having the
Instrument built before the accountants caught up with him. He won They did catch up with
him, but not untd six months after I was hired and two months after the instrument was work-
mg quite well Typically, he balanced his budget by selling my developmental model to the
American Cyanamid laboratories. If this were happening today, I am sure that Dr. Zworykin
would find a way to bypass the llmltaUons of a computerized, short-term financial control
system One factor in Dr. Zworykln's greatness was his abdlty to remove irrelevant obstacles
from his workers' projects.
The Pattern of Progress

In 1940, the technological mfrastructure that supported the design and constructmn of
TEMs was becoming avadable, but we were stdl almost two orders of magmtude from the
theorettcal hmlt of our spectfic design Unfortunately, the mstrumentatton needed to analyze
the limits of performance of the then current TEMs did not exist Before 1940, few of us appre-
crated how many external and internal factors were capable of disturbing the TEM image, or
the h~gh sensitivity of the images to those factors Ulttmately, the instruments themselves,
being the only devices with sufficient sensmvlty, had to become the means for detecting and
measunng the effects of the many techmcal problems that existed in those early instruments
The read-out was, of course, the nature and degree o f b l u m n g of the recorded image Because
of the low intensity of the visual images m those days, the necessary sensmwty was achievable
only m the recorded image and not m real time Not only was the read-out very ambtguous,
but ~t related only to those dtsturbances that happened to occur dunng the exposure interval
and, for which, we had no independent means of sensing. For example, the effect of a thermal
drift of the specimen, which represented a real physical movement of the specimen dunng the
exposure, was mdJstmgmshable from the motion of the image caused by an insulating parhcle
of material situated near the beam path As scattered electrons collect on such a particle, ~ts
potentml ts slowly rinsed causing the beam to be deflected slowly dunng the exposure Slmt-
iarly, the effect of a transient mechamcal vibrat~on that happened to occur dunng the exposure
could be lndlstlngmshable from the effect of a small transverse a-c magnetic field that was leak-
mg into the path of the beam In addition, it even took a very experienced eye to d~stmgmsh
between the effects of these two sets of examples
Thus, the development and refinement of the TEM became an unending repetmve series of
proposed hypotheses followed by the design of experimental tests and then, by the actual tests
Because of the erratic vanablhty of many of the defects, their large number, and of the absence
of real time observations, the successful ~dentlficatlon and removal of one defect rarely gave
an unequivocal signal that anything had happened However, there is another side to th~s coin
As it turned out, it was the same erratic vanabihty that prevented the process from becoming
completely discouraging As we were making thousands of exposures, m our struggle to
achieve consistent results at, say ten nanometres, there was always the unexpected exposure
that showed a resolving power several times better These were the mtcrographs that were pub-
hshed but, more ~mportantly, they were the teasers that kept telling us that it could be done
and gave us the incentive to continue
It is interesting to note that by 1943 the number of defects stdl present had been whittled
down to the point where identifying and removing the remaining ones became relattvely sim-
ple As a result, some spectacular improvements m resolving power were made qmckly and
easdy. It was this phenomenon that allowed the ~mphcit astigmatism of our magnetic objec-
tives to emerge from the masking effects of other problems and successfully be corrected by
the development of the shgmator
Using very small round holes m a collodion membrane as our test objects, it became clear
that we had some astigmatism m our objectives and that ~t was a relatively constant charac-
teristic of each set of objechve pole-pteces. Our first assumption was that the alignment of the
two poles was ~mpreclse We tried lapping the openings m the assembled pole-p~eces with
interesting results Sometimes, the pole-piece tmproved and sometimes, it got worse Because
none o f the best pole-p~eces was perfect, we tried contmmng the lapping We were surprised
to find that continued lapping, ultimately, always made a pole-piece worse We began to reahze
that the astigmattsm was due to the relative coarseness of the gram structure of the tron and,
frequently, due to mclustons of nonmagnettc ~mpuntles We then went through the exercise
of searching for better iron and better anneahng processes We had no success and became
quite frustrated
Then came the " e u r e k a " Late one night, I suddenly realized that if some very small defect
in the iron could pull the magnetic field askew, I should be able to find a way of introducing a
compensating defect that would pull it back This concept was exactly analogous to correcting
the astigmatism in an eye by adding a compensating amount of astigmatism m a spectacle lens
but the practical approach was equivalent to correcting the shape of the lens m our eye by
applying pressure or tension at evenly-spaced points around its periphery Early the next
morning, I had my machinst make some soft iron screws from (believe it or not) ordinary
welding rod He then threaded eight of them into the pole-p~ece spacer so that they pointed at
the axis of the lens and could be adjusted in or out It took a few hours to learn how to adjust
the screws to remove the astigmatism Nevertheless, w~thln 24 hours from conceiving the idea,
we were getting consistent results at about one nanometre that represented approximately an
order of magnitude improvement in average performance from the day before
IfI have a message In this part of my paper, it is to note that the great bulk of the work that
brought the TEM into being as a most useful tool for science and technology, had little if any-
thing to do with the basic theory o f the electron microscope. This leads to the observation that,
through some form of accepted scientific snobbery, of which I was as guilty as anyone, only
positive end results were ever published Reports of the tedious background work that led to
the achievement and details of the blind alleys that were encountered, remained buned m lab-
oratory notebooks There was much word-of-mouth exchange of such Information among the
early workers However, [ feel that our behavior condemned many newcomers, particularly
internationally, to repeating most of our research and many, if not all, of our mistakes.
In spite of the problems, the TEM did become useful and started providing essential infor-
mation to an expanding universe of research disclphnes, sometimes m spectacular and unex-
pected ways. Without question, some of the more interesting developments were attempts to
apply the electron microscope to metallography Theory clearly indicated that the fundamen-
tal interactions between electrons and solid surfaces would prevent the electronic analog of a
light metallograph~c microscope from providing any useful results In view of the fact that the
main stream of the research at RCA was the development of television, it was quite natural
for us to consider a scanning system for metallurgical specimens. When we &d, it became clear
that a scanning system would circumvent most of the difficulties we expected In the &rect
imaging approach Thus, in 1941, we embarked on building a scanning electron microscope
We did succeed in building such an instrument and in obtaining a few pictures However, it
became painfully clear that the technology of the early forties was far from adequate for our
objectives. Even so, we probably would have continued to pursue the scanning approach if we
had not learned of Mahl's success m applying the TEM to metallography by his brilliant use
ofrephca techniques We concluded, probably correctly, that we could achieve more of value
by devoting all our efforts to the development of the TEM and its applications
The Value of the TEM in Research

Let us examine, in a little more detail, what the TEM can do for research even when
restricted to revealing only the geometry of structures. There is an i n o d e n t that sticks in my
memory as a particularly significant demonstration of this role of the TEM and as one of the
building blocks of my own understanding In the late summer in 1940, we had the first devel-
opmental model of the RCA model EMB working in my laboratory in Camden We received
a call from Dr Wendell Stanley asking if it would be possible to take a look at one of his
tobacco mosaic virus (TMV) preparations Dr Stanley had spent most of his professional
career, to that point, working on plant viruses at the Rockefeller Institute Laboratories that
were then located in Princeton, New Jersey Later, he received a Nobel Prize for his work on
the ~dentificatlon and characterization of plant viruses
We agreed to take a look and within an hour after he arrived we had a spectacular picture
of his wrus, clearly showing the characteristic rods with precisely the dimensions he had pre-
dicted In minutes we had "confirmed" what had taken Dr Stanley and his group many years
to determine by uhhzlng such indirect techniques as low-angle X-ray scattering, ultracentri-
fuglng, blrefrmgence optical studies, etc Please note that I used the word " c o n f i r m e d " This
spectacular confirmahon of Dr Stanley's work is only one indicator of the value of the TEM
It is more illuminating to consider what the scenario might have been if the TEM had been
available at the time Dr Stanley was just starting his work He had discovered that the infec-
tious agent that caused the tobacco mosaic disease could pass through an unbehevably fine
porcelain filter If he had had a TEM available, he undoubtedly would have examined speo-
mens of the filtered jmces from healthy and infected plants HIs attenUon would have been
attracted by the presence o f very uniform rods as the only ahen structures m the jmces from
the infected plants Note that the presence of the rods m only the infected speomens would
have been strongly suggestive but, by itself, would have proven nothing However, starting
with the TEM observation, showing that the rods were actually the infectious agent would have
been a rather straightforward and relatively simple procedure There is an important, but inad-
equately apprecmted aspect buried in this alternative scenario The enormous ~mprovement
that could have occurred in the effioency of Dr Stanley's research, if he had had a TEM at the
beginning, would have been the result of what the TEM did "not" show, as much as of what
it did show Without TEM lmages, all the possible slzes and shapes the virusmlght have, would
have to be investigated before the characterization of the virus could be narrowed
Th~s digression shows that the TEM had, and probably still has, two basic funcUons The
first is to make ws~ble "submicroscopic" geometrical structures that have significance in an
ongoing research project The second is to increase the efficiency of a research program greatly
by slgmficantly reducing the number of possible geometrical structures that might have rele-
vance to the research and for which appropriate hypotheses and tests would otherwise have to
be devised
On to Electron Microprobe Analysis

From the beginning of our understanding of the research role of the TEM, it was appreciated
that if we could, by some means, attach some point-by-point chemical information to the
geometries revealed, we would add a whole new dimension to the utility of the instrument
Staining with heavy metal compounds became useful for enhancing the contrast in images of
organic materials Unfortunately, these had very little of the specificity of the stares used m
light microscopy
There was a flurry ofachvlty in our laboratory to explore the potential of electron diffraction
as a means of ldenUfying the chemical composition of individual small particles and struc-
tures We built a probe-type electron diffraction camera that enabled us to obtain patterns
from selected particles in TEM specimens Although it was an Interesting project, it quickly
became clear that the approach had such limited application that it was not possible to justify
any development of the necessary instrumentation It was essentially worthless for very small
organic structures Very small inorganic particles tended to be single- or near single-crystal
structures with indeterminate orientation and rarely gave adequate information for identifi-
cation While the diffraction approach was not successful, the research did have a payoff" We
acquired invaluable experience in the design and operation of an electron probe type of
instrument
Some time around the beginning of 1943, I was browsing in the library and ran across an
article by G R u t h e m a n n in Naturwtssenschafien, the German counterpart of the British pub-
hcatlon, Nature R u t h e m a n n wanted to show experimentally that when an electron excited a
certain X-ray level in a target, it lost precisely the energy required for the excitation The exper-
iment required a target so thin that the transmitted electrons would experience not more than
one inelastic collision He chose a collodion film and showed that the discrete energy losses
caused by the excitation of the K-levels of carbon, nitrogen, and oxygen produced the pre-
dicted peaks in the velocity distribution of the electrons in the transmitted beam
Reading that article was an interesting experience in how the h u m a n mind works Even
though R u t h e m a n n was interested only In the basic physics, his article triggered recognition
that his experiment could be used for analysis and that, with the use of an electron microprobe,
might solve the chemical analysis problem in our TEM specimens Interestingly, the complete
design of our first instrument popped into my mind simultaneously with the recognition of
the possibdities I was also amused at my obvious stupidity when I realized that I had been
thoroughly familiar with all the physics involved since my undergraduate days
We quickly constructed a 180* magnetic electron spectrometer that we added to one of the
probe instruments used in our diffraction experiments We confirmed Ruthemann's results
using much higher voltage electrons and even extended them to some other light elements We
also did some work with a crystal X-ray spectrometer to detect the characteristic X-rays emit-
ted from a very small area of the specimen All of this was very good research that we pursued
very enthusiastically Unfortunately, our enthusiasm began to wane as we realized that, once
again, our concepts were running far ahead of the technologies needed for their routine
application
There were many problems, but three were particularly intractable The first and most
annoying was the very rapid build-up of contamination at the point where the probe was
focussed on the specimen As a result, when we tried to analyze a very minute particle, the
contamination caused the specimen to become opaque in less time than was required for an
adequate photographic exposure to record the spectrum The second was the cumbersome
nature of the state of the art of techniques for making quantitative measurements of X-ray or
electron intensities from photographic exposures If you have gone through the exercise of cal-
ibrating the exposure on a photographic emulsion, standardizing the development of the pho-
tographic material, and then running It through a recording mlcrophotometer, you will appre-
ciate what I am saying Moreover, all that technology was invalidated essentially by the rapidly
changing situation occurring during the exposure, as a result of the contamination problem
The third was the nature of our probe system, which could become very tedious in routine use
It was almost three decades before all the technologies required to make microprobe analysis
reasonably practical, came together These involved some major developments, such as very
high resolution scanning transmission electron microscopes, very small, fast, and Inexpensive
computers, a broad range of very sensitive sensors for direct detection and measurement of X-
ray or electron intensities, and, finally, the development of instruments with ultrahigh vacuum
systems The stories of those developments will have to be told by the individuals Involved
What we can say is that our dreams of the early forties are now being realized
Conclusion
In this very br~efblt of nostalgia, there are many pieces of information regarding the creative
process that lead to significant discoveries There is the important role of pure chance in the
creative process and the need to have one's mind prepared to recognize and take advantage of
opportunities when they happen to emerge There is the relationship between the state of the
technological infrastructure and what is necessary to transform a theoretical concept into a
successful practical system Finally, there is the obvious desirability, if not necessity, of broad-
ening one's experience as widely as possible outside the limited requirements of one's imme-
diate projects
Bibliography
Rather than overload this somewhat philosophical article with a very long list of only slightly
relevant references, the author concluded that the interested reader would be better served if
he or she were directed to two monographs that cover the technical developments of the period
m much greater detail and provide all the significant references with a much better indication
of what each contains. These are:
1. Zworykm, V K , Morton, G A , Ramberg, E G , Hilher, J., and Vance, A W , Electron

Optics and the Electron Microscope, Wiley, New York, 1945, and
2. Hall, C. E., Introduction to Electron Microscopy, McGraw-Hall, New York, 1953
Quantitative Metallography
Daniel B. Fowler 1
Quantitative Metallography in Test Method

Standards and Product Specifications
REFERENCE" Fowler, D B, "Quantitative Metallography in Test Method Standards and
Product Specifications," Metallography Past, Present, and Future (75th Anmversary Volume),
ASTMSTPl165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amer-
ican Society for Testing and Materials, Philadelphia, 1993, pp 235-242
ABSTRACT: Quantitative metallographlc and stereologlcal methods can be applied to micro-

structures observed with the light microscope These methods, however, are not presently
requested by product specifications, except in a few notable cases For the most part, manually
performed chart comparison methods, developed 50 to 60 years ago, are still specified
Most laboratories that rely upon chart methods utilize poorly controlled metallographlc pro-
cedures for specimen preparation Image analysis using specimens prepared by these processes
yield erratic, inaccurate and nonreproduclble test results Of course, this is attributed usually to
the measurement method and equipment rather than to the specimen preparation procedures
and their execution
Specimen preparation, however, can be performed in a controlled, efficient manner with
highly automated equipment Image analysis measurements using specimens prepared with such
equipment are accurate, precise, and reproducible However, product specifications have not
been updated to incorporate this new technology In our quest for greater product quality, these
methods are essential
KEY WORDS: quantitative metallography, stereologlcal methods, light microscope, testing,

product specifications, standards, metallography, metallurgmal specimens, microstructure,
metallographlc techniques
Although there are now a few test method standards that descnbe quantitative metallo-
graphic methods, performed manually or by automatic image analysis, few product standards
specify use of quantitative test methods These product standards still specify mlcrostructural
analysis, for the most part, according to s~mple comparison chart methods, performed man-
ually Many o f these methods have been used for 50 to 60 years.
Specification writers appear to be reluctant to adopt these new, more rigorous methods
Partly, this can be attnbuted to the natural resistance to change or to ignorance of these new
methods Some will state that the current methods are "good enough" and that these new
methods will be more costly The quality of image analysis results is influenced by the quality
of specimen preparation A c o m m o n misconception is that poorly controlled preparation pro-
cedures produce acceptable results using the existing chart methods However, if the same
poor preparation practices are applied to structures measured by image analysis, results are
imprecise and inconsistent O f course, this is incorrectly attributed to the measurement equip-
ment rather than the preparation methods
Substantial progress has been made over the past 20 years in gaining an understanding of
the specimen preparation process Moreover, this knowledge has been incorporated into
highly automated equipment This equipment consistently produces properly prepared spec-
J Analytical products manager, Struers, Inc, Westlake, OH 44145
235
Copyright
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ASTMby Int'l
imens and at a lower unit cost Many laboratories have obtained such equipment With prop-
erly prepared specimens, good quantitative test method standards and a properly programmed
image analyzer, accurate, precise, reproducible microstructural measurements can be made.
However, product standards must speofy the use of these methods Otherwise, they will not
be used
ASTM Committee E4 on Metallography has been introducing quantitative analysis tech-
niques into their test methods Of course, the chart methods still exist, but efforts are being
made to improve them However, product specifications have not kept pace with this new
technology. They are still specifying 50 to 60 year old technology Comparison methods are
highly subjective The problems associated with developing chart methods has been well doc-
umented, for example, for assessing inclusion content [1], grain size [2], and graphite type,
size, and amount [3,4]. Regardless of the quality of the specimen preparation, comparison
methods yield less precise data than image analysis Moreover, chart method use may be
biased by the operator's desire to produce certain results
Precision instruments for sample preparation and evaluation make possible the develop-
ment of sophisticated quantitative metallographic standards. Recent developments in equip-
ment technology for mlcrostructural specimen preparation and measurement permit the
application of process control concepts to specimen preparation as well as evaluation Perhaps
more importantly, materials scientists have been working to change metallography from a
qualitative art to a quantitative science
Many existing product standards rely on visual companson test methods to determine
microstructural quality. As an industry, we can greatly improve upon these subjective stan-
dards The methods and tools needed to perform quantitative metallography efficiently are
now available What blocks the path to more scientific standards is a reluctance to accept new
ideas and methods
Consider the typical specifications and standards that exist tbr controlling the external
dimensions of a manufactured component To gage the acceptability of a part, certain meth-
ods and tools are employed Beginning w~th the design, the external dimensions of the part are
specified in a very precise way using engineering drawings The exact required dimensions
along with their corresponding allowable tolerances are given Dunng production of the part,
forming and finishing processes, such as casting, machining, and others are performed in a
highly controlled manner To determine the quality of the part, or its adherence to the speci-
fications, instruments are used to actually measure the dimensions. Whether it be a simple
caliper or more sophisticated electronic devices, the actual measurements are made and com-
pared with the dimensions given on the engineering drawings.
The demand for consistency in product quality, and the ability to measure part dimensions,
IS the basis for statistical quality control. It is difficult to imagine that the quality control of
dimensional specifications of a manufactured part could be based upon visually comparing It
to a picture in a specification book, and judging by eye whether or not the part meets the spec-
ificaUons. Yet the comparison methodology is exactly the basis for many specifications per-
taining to mlcrostructure.
The rigorous performance and environmental requirements placed upon engineered mate-
rials demand precise control of mlcrostructures Sophisticated metallographic tools and meth-
ods are readily available to meet these demands. Metallographlc preparation and evaluation
can be conducted as a manufactunng process Metallography, the controlled process, wdl yield
results that can be the basis for the product specifications and standards that are of the same
quantitative nature as those for any other manufactunng process. To do this requires the use
of tools for the precise development and measurement of mlcrostructure. All metallographic
standards should be quantitative standards. All metallographlc specifications should be based
on actual measurements o f microstructure with assessment of their statistical precision. Esti-
FOWLER ON QUANTITATIVE METALLOGRAPHY 237
matlons and visual comparison methods are no longer needed because Instruments and meth-
ods exist that allow quantitative test methods and product specifications to be effectively
Implemented
Metallography
Metallography is based upon the long standing and continuously evolving body of evidence
that demonstrates that the internal structure of a material has a direct influence on the eng~-
neenng properties and behavior of that material In the more than 125 year history ofmetal-
lography, manual specimen preparation and visual observation techniques have been funda-
mental to the study of mlcrostrucutres of matenals In fact, one researcher has gone so far as
to state that, "optical examination of materials IS the foundation on which all of our present
understanding of the relationship between mlcrostructure and properties is based" [5] How-
ever, one of the problems in using mtcrostructure as an indicator of matenal properties is that
considerable effort is required to prepare specimens so that internal structures can be observed
Early practitioners of metallography invented and experimented with different techniques
to accomplish their goals of revealing mlcrostructure As In any new endeavor, there were no
established standard methods and the ploneenng individuals developed their own styles for
the solution of problems In tracing the history of technology, the early successes were based
upon the skills of individual artisans [6, 7] Similarly, the concept of metallographlc specimen
preparation as art can be traced to the association of individual talents with successful prepa-
ration methods [8] Today, there exists an enormous body of knowledge concerning applied
metallography There are many accomplished metallographers and several excellent text-
books covenng all aspects of specimen preparation [9,10] The concept of metallography as
only an art is no longer valid today Viewing metallography merely as an art is based on the
behefthat preparation of specimens requires an individual and qualitative approach that can-
not be described precisely or performed by the unskilled or by machines.
Traditional artisan preparation is based almost exclusively on manual methods. The hand
tools used for preparing specimens did not provide mechanisms for control The objective was
the creation o f a microstructural image that met subjective, visual criteria, established empir-
ically and, perhaps, arbitrarily Under the "metallography is art" philosophy, preparation pro-
cedures such as this result " the sample should be polished extensively on the silk cloth, by
hand, using the 0 3 Alumina/distilled water slurry mixture until the voids are filled in, or no
slgn~cant improvement is noticed" [11 ]
This procedure IS qualitative, relying upon the terms "polished extensively" and "no sig-
nificant improvement" that offer little hope ofreproduclblhty or agreement This sort of ambi-
guity inevitably leads to disagreements over the correct preparation method and the true
microstructure, making mIcrostructural specimen reproduction virtually impossible A major
problem m metallographlc preparation is the difficulty in achieving reproducibility
The limitations of art-based metallography are obvious The question of correctness is not
applicable to art and, as art, the possibility of measurement is illogical and impossible Qual-
ities attributable to good art, such as originality and unique individual style, are totally unde-
sirable m metallography Conducted merely as an art, metallography cannot possibly be the
basis for standards or specifications
Now, let us consider metallography as a controlled manufacturing process Seven basic
manufacturing processes have been defined [12] These are
casting or molding,
forming or sheanng,
machining (material removal),
heat treating,
finishing,
assembly, and
inspection
With these operations in mind, consider the steps in a typical metallographic specimen prep-
aratlon procedure
l sectioning (sawing, a basic machining process);

2 mounting (an example of fixtunng in order to allow for subsequent machining
operations),
3. gnndlng (abrasive machining),
4. pohshlng (abrasive machining); and
5 etching, tinting, interference layering, etc. (finishing).
It is easy to define each step in the microstructural specimen preparation sequence as a basic
manufactunng process. By defining preparation as a series of manufactunng processes, com-
posed mainly o f abrasive machining and finishing steps, then the application of manufacturing
control concepts becomes feasible Metallographlc specimen preparation now becomes eligi-
ble for control
A wide variety of tools and methods are available to control specimen preparation.
Machines capable of precise preparation of specimens can control the rate and amount of
material removal, the pressure o f specimen on abrasive, and other variables associated with
specimen preparation Several controllable preparation variables have been identified, as listed
in Table l
The significance of controllable specimen preparation is enormous It yields a product of
reliable quality Specific tolerances may be achieved. Preparations can be performed equally
from laboratory to laboratory At last, the varlabihty in microstructure can be assigned to
causes other than specimen preparation Mlcrostructure revealed via controlled preparation
procedures provides a basis for reliable evaluation, quantitative standards, and specification
limits It also permits development of microstructural databases for quality control purposes.
Evaluation
The process of mlcrostructural analysis begins with specimen preparation The output of
preparation is the mIcrostructural image that becomes the input to evaluation Once specimen
preparation has been brought into a controlled state, it is necessary to provide for controlled
evaluation to complete the foundation for quantitative standards and specifications
What has microstructural evaluation meant in the past and what form must evaluation take
TABLE 1 Metallographlc preparation variables a
Abraswe type Material removal

Abraswe format Force
Abrasive dozing RPM
Lubricant type Rotatmn
Lubricant dosing Consumable degradation
Predoslng Cleaning
Time
a Table developed by S Glancy, Struers, Inc
m the process of quantitative metallography9 Historically, inspection of mlcrostructures was

made for the purpose of e n s u n n g the presence of features associated with desirable perfor-
mance (that is, long fatigue life, high strength, etc ) or, the absence of structures associated with
poor performance In the past, materials were not speofically engineered for certain applica-
tions and the need to monitor mlcrostructure very precisely was low In the age of"low tech-
nology" and nonenglneered materials, subjective evaluations were satisfactory since the
demands placed upon the materials were not closely matched with the material properties The
general evaluations produced by visual Inspection provided adequate information to verify
acceptability Many traditional evaluation methods rely upon the comparison of observed
mlcrostructures with charts or photomicrographs and are often referred to as microstructure
"interpretation" or mlcrostructure "characterization "
The problem with this approach is summarized by George Vander Voort in his book, Met-
allography Prmctples andPractwe, "Since the method depends heavily on the grading of the
pictures, errors m the grading influence rating accuracy and the ratings become highly depen-
dent on subjective opinion The result is that reproducibility suffers" [13] The development
of engineered materials, and the increasing recogmtlon of the need for more soentlfiC meth-
ods, has created a demand for a more precise definition of the objectives of mlcrostructural
evaluation. By replacing mlcrostructure mterpretatlon and characterization with microstruc-
ture measurement, it is possible to do more than supply subjective "pass/fall" Information on
the quality of a product
The grain size of metals and alloys, for example, is well known to influence many properties.
For many years, metals have been classed as fine or coarse, based upon the ASTM grain size
scale If the grain size was No 5 or finer (higher numbers), it was judged to be suitable for most
engmeenng applications. A comparison chart rating to simply show that the grain size was
clearly finer than No 5 was considered adequate Greater precision was not demanded as, in
most cases, the grain size rating was used for no other purpose
However, over the past 20 years, there has been a strong drive to improve the quality of
many metals and alloys, that is, to get much better properties and behavior from basically the
same alloy Llneplpe steels are a good example. Researchers [14,15] have discovered that
extreme refinement of the femte grain size is required for optimum properties The No 5 or
finer requirement does not work Grain size must be measured with a high degree of precision,
without bias, and with exceptional reproduclblhty Chart methods are inadequate
Through quantitative methods, metallography can be used to develop new or better infor-
mation on known materials or to develop new materials. It can also be employed to obtain
accurate measures of fundamental physical constants. What exactly is quantitative metallog-
raphy9 It is based upon a group of mathematical/geometric techniques for the actual mea-
surementofmlcrostructure It~stheeqmvalentofgaglngofmlcrostructure I t p r o w d e s a p r e -
clse way for mlcrostructural components to be measured that is exact and reproduoble
Although quantitative microstructural concepts can be traced to the mineralogical work of
Delesse in 1848, the first comprehensive publication of methods can be attributed to S A
Saltykov at the end of World War II However, it was not until a translation of the second
edition (1958) of his book [16], StereometncMetallography, became available m the West that
interest m this area began to grow. This stimulated ploneenng pubhcatlons by DeHoff and
Rhmes [17], Underwood [18] and many others.
Although the techniques are based on geometrical probability concepts, there is nothing
mysterious about the methods They involve the counting of points, intercepts, tangents or
features, measurements of line sections or areas based on the relationship of some sort of test
grid or pattern with respect to the mlcrostructure The test grid may be a group of systemati-
cally arranged points or lines, circles or areas, depending upon the desired measurement From
these data, numerical values for the amount, size, spacing, density, distribution or shape of
mlcrostructural features can be calculated Further, because a n u m b e r of such measurements

are performed, the statistical quality of these data can be descnbed Depending upon the
nature of the mlcrostructure and the measurement conditions, these data taken from two-
dimensional cross sections through the structure can describe the three-dimensional charac-
tensUcs of the structure
The measurement ofmlcrostructual features can be performed manually, an approach that,
in many cases, can be quite tedious and time consuming However, tools and instruments are
now available that automatically acquire the necessary measurements Beginning m the early
1960s, video technology was introduced to the world of metallography Computer mathe-
matical power was also brought into the laboratory and the term "image analysis" infiltrated
the metallographer's vocabulary. There are a whole range of fully automatic and semmuto-
matlc instruments that have been designed to extract feature measurements from a digitized
video image These Instruments are relatively fast, and if we prepare the specimens consis-
tently, the results are preose and accurate
There is some confusion over the terms "image processing" and "image analysis "Process~
lng includes mathematical transformations of the video image that may be used to prepare the
image for analysis The result of image processing is another video image that attempts to dis-
play the microstructural features in a more distract way Metallographic specimen preparation
is designed to clearly reveal mlcrostructure Electromc video image processing cannot make
up for poor metallograph~c specimen preparation Image analysis describes the extraction of
measurement data from the wdeo image The output of image analysis ~sthe structural feature
data that quantitatively describes the mlcrostructure These measurements are the basis for
quantitatwe product specifications
Just as in specimen preparation, where automatic grinding and polishing tools provide con-
trol of the preparation process, automatic measurement tools can control the process of eval-
uation, ehmlnatlng the subjectwlty ofthe h u m a n eye It is no less important to consider micro-
structure measurement as a controllable process in establishing sound quantitative test
standards By consldenng the entire range of metallographlC functions, both preparation and
measurement, as part of the same process, and that each process is controllable, we can arrive
at an excellent basis for the formulation of quantitatwe metallographIc test standards and
product specifications
Specifications and Standards

Material mlcrostructure, with its proven correlation to engineering properties, is a suitable
measure for a product specification. If the strength of a material is influenced by the amount
of porosity in ItS structure, porosity can be measured in order to assess the quality of the mate-
hal The patterns of microstructure and performance correlation form the basis for material
standards Specifications are intended to be a statement of a standard of quality
Product specifications describe the chemical and mlcrostructural characteristics required to
produce a certain combination of mechanical properties deemed necessary for a particular
product Other product characteristics, such as product size and shape, are also important, but
are not related to mlcrostructural control or measurement The ideal product specification
would define uniquely the qualities necessary to serve most efficiently for a given use and they
can be approached if truly significant tests can be made to determine the presence of the
required qualities [19] Controlled preparation and measurement of mlcrostructure using
quantitative methods provide these significant tests There exist today many private and public
standards that incorporate metallographlc procedures Most manufacturing companies have
many volumes of raw material and component standards. There exist many other standards,
such as Military Specifications, and there are several standards writing organizations, such as
the American Society for Testing and Materials (ASTM) and the International Organization
for Standardization (ISO) [20]
Standards have evolved along with materials soence and metallographlc technology. Im-
tlally, the requirements of materials being rather general, the techmques of preparation and
evaluation being imprecise, the product standards themselves did not reqmre exactness. Many
metallographlc standards have made use of chart p~ctures or photographs for comparison to
the observed structures. The first appearance of chart rating methods for gram size and inclu-
sion content was m the 1930s These methods became popular and are still used today These
standards exist today and are used within all manufacturing industries These standards, how-
ever, are inadequate They are remnants of a time when neither the need for preose measure-
ment of materials, nor the abd~ty to make them, existed. Clearly that ttme has passed As Davis
[19] states m The Testmg of Matertals "The skdl and accuracy w~th which a thing can be
speofied depends on the state of knowledge concerning it and on the preoslon with which its
qualmes can be determined "W~th the increasing complexity of matenals, more adequate test
methods and product specifications have become necessary, w~th advances m soenhfic under-
standing of these materials, and the avadabd~ty of precision analytical instruments, more ade-
quate speoficat~ons have become possible.
Conclusions
Engineered materials designed for demanding apphcatlons reqmre a more soph~stlcated
approach to metallographlc speoficatlons Only a short time ago, the concept of automahc
specimen preparatton was rejected by many practmoners and there may still be those who
resist advanced methods However, that number is rapidly decreasing. There are now many
who understand the value and absolute necessity of controlled specimen preparaUon
The next step is controlled quantltatwe evaluation We must go beyond mere charactenza-
tlon to meaningful quantification This is possible through the use of soent~fic methods per-
formed by automatic measurmg instruments Mtcrostructure preparation and evaluation pro-
cedures can be developed using the same basic engmeenng p n n o p l e s apphed to any
manufactunng process These process speoficatlons become the basis for true quantitative
standards
Quanhtatlve test method standards are being developed. Within the Amencan Sooety for
Testing and Materials pubhcatlons, several mlcrostructural standards exist that incorporate
rigorous quanhtatlve methods. But, there are many poorly wntten quahtattve standards, par-
tlcularly those issued by industry as private standards It ~s the responslblhty of industry pro-
fesslonals, both suppliers and manufacturers, to provide the highest possible product quality
Th~s goal can only be achieved by employing the best methods and technology avadable m the
metallographlc process
References
[ 1] Vander Voort, G F, "Inclusion Measurement," Metallography as a Quahty Control Tool, Plenum
Press, New York, 1980, pp 1-88
[2] Vander Voort, G F "Gram Size Measurement," PractwalApphcattons of QuantltattveMetallog-
raphy, ASTM STP 839, J L McCall and J H Steele, Jr, Eds, American Society for Testing and
Materials, Phdadelphla, 1984, pp 85-131
[3] Wyman, L L and Moore, G A, "Quantaatwe Metallograph~c Evaluations of Graphmc M~cro-
structures," Transactions, AFS, Vol 71, 1963, pp 7-16
[4] Underwood, E E and Berry, J T, "Quantltatwe Measurements of Cast Iron M~crostructures,"
Transactions, AFS, Vol 89, 1981, pp 755-766
[5] Cochrane, R C, "Optxcal Microscopy," Charactenzatton of Htgh Temperature Materials 1, The
Institute of Metals, London, 1988, pp 43-93
[6] Smith, C S, A Search for Structure Selected Essays on Science, Art, and History, The MIT Press,
Cambridge, MA, 1982
[7] Smith, C S, From Art to Science Seventy-Two Objects Illustrating the Nature of Discovery, The
MIT Press, Cambndge, MA, 1980
[8] Smith, C S, A History of Metallography, The University of Chicago Press, Chicago, 1965
[9] Vander Voort, G F, Metallography Principles andPracttce, McGraw-Hill, New York, 1984
[10] "Metallography and Mlcrostructures," Metals Handbook, 9th ed, Vol 9, American Society for
Metals, Metals Park, OH, 1985
[I 1] "Metco Polishing Procedure for all Ceramic Type Coatings," MLPP 5, Metco
[12] DeGarmo, E P, Materials and Processes in Manufacturmg, 5th ed, MacMllhan, New York, 1979
[13] Vander Voort, G F, Metallography Prmctples andPracttce, McGraw Hill, New York, 1984,p 410
[14] Abrams, H and Shmmon, P R, "Development and Properties of BethStar 80, A New 80 ksl Yield
Strength HSLA Plate," SAE Technical Paper Series, No 820486, Society of Automotive Engineers,
Warrendale, PA, 1982
[15] Abrams, H and Mueller, G E, "Development of Commercial HSLA Plate Steels Using the 160
Mill Process Control Computer Model," 1987 Mechamcal Working and Steel Processmg Proce-
dures, Iron and Steel Society, Warrendale, PA, 1988, pp 343-352
[16] Saltykov, S A, Stereometrw Metallography, 2nd ed, Metallurglzdat, Moscow, 1958, (3rd ed,
1970)
[17] QuantttatlveMwroscopy, R T DeHoffand F N Rhlnes, Eds, McGraw-Hill, New York, 1968
[18] Underwood, E E, Quantitative Stereology, Addison-Wesley Publishing Co, Reading, MA, 1970
[ 19] Davis, H E, et al, The Testing of Englneermg Materials, 4th ed, McGraw-Hill, New York, 1982
[20] Batik, A L, A Guide to Standards, Parker, CO, 1989, pp 77-128
John J. F r i e l 1 and Eddle B. Prestridge 1
Artificial Intelligence for Twin Identification

REFERENCE: Fnel, J J and Prestndge, E B, "Artificial Intelligence for Twin Identification,"
Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F
and Materials, Philadelphia, 1993, pp 243-253
ABSTRACT: The presence of twin bands in some alloys makes grain mzmg by automatic image
analysis difficult Twin bands appear mmilar to grain boundaries, therefore, the measured grain
size is too small Although an experienced metallographer can ignore twins while measunng
gram size manually, it is often desirable to use automatic image analysis to save time and increase
reproducibility Because twin bands are so similar to grain boundaries, traditional image pro-
cesslng techniques cannot distinguish them However, the techniques of artificial intelligence
(AI) can be used to impart knowledge to a computer that enables it to distinguish among micro-
structural features This method was tested on standard gram size charts and on real specimens
The results showed that the use of artificial intelligence for twin identification and removal works
sufficiently well to lead to an accurate measure of grain size
KEY WORDS: twin bands, artificial intelligence, image processing, image analysis, gram bound-
ary, mlcrostructure, metallography, metallurgacal specimens, metallograph~c techniques
W h e n annealing twins are present in a mlcrostructure, grain sizing by automatic image anal-
ysis is difficult T w i n boundaries appear similar to gram boundaries, and thus the measured
gram size is too small It is s o m e t i m e s possible to eliminate some o f the twins on the basis of
their gray level, but not all o f them. An entirely different approach is to attempt to identify
those characteristics o f twins that are different from grain boundaries and impart this lntelh-
gence into the image analyzer The first attempt to do this was reported previously, but
advances have now been m a d e that c o n v i n c e us that the artificial mtelhgence (AI) approach
succeeds [ I ]
A S T M M e t h o d s for D e t e r m i n i n g G r a i n Size (E 112-88 and E 1382) specify that a crystal
and its twin bands shall be considered as one gram Accordingly, if grain sizing by automatic
image analysis is contemplated, twin boundaries must be found and r e m o v e d This identifi-
c a h o n is not too difficult for an experienced metallographer, but quite difficult for a c o m p u t e r
However, if the c o m p u t e r can be taught to recognize most twins, removal is easy and auto-
matlC image analysts can proceed. It is not necessary for the c o m p u t e r to be perfect, accurate
analysis is still possible Even an operator is not perfect O n c e twins have been identified, it ts
possible to perform the analysis with and without twins as suggested for structure-property
correlations [2].
Image Processing
General Processmgfor Gram S l z m g
Before a mlcrostructure can be measured with a completely automatic image analyzer, some
preprocesslng or editing or both o f the digital image is often necessary. Image processing is
1Technical director and product manager, respectively, Pnnceton Gamma-Tech, Pnnceton, NJ 08540
243
Copyright
Copyright*by1993
ASTMbyInt'l
computer mampulat~on of an image that returns a d~fferent image Examples include contrast
transformation, digital filters for noise reduction or edge enhancement, illumination equah-
zatlon, etc Image editing means insertion or deletion of groups of pixels in a binary image.
For example, ffan image has been made binary by thresholdmg so that grains are bright and
gram boundaries are black, parts of the image can be edited to change them from boundary to
grain, or vice versa Image editing can be done by the operator and may be time consuming,
If there is much to be done Or it can be done by the computer as m erosion and dilation oper-
ations After appropriate image processing or editing steps or both are defined, the sequence
can be automated Image processing operations should have enough flexibility so that the
operator can determine the appropriate seventy of each process the first Ume and then apply
the same operation to other images.
Some of the preprocessmg steps that may be necessary are (l) uneven illumination correc-
tion, (2) gram boundary detection, (3) bmarizatlon, (4) inclusion removal, (5) gram boundary
completion, and (6) boundary throning. Not all of these processes are necessary on every spec-
,men, and one should never use image processing in place of proper s p e o m e n preparation and
microscope alignment
Whether or not a microstructure contains twins, the boundaries around each gram must be
complete, or the image analyzer wdl fuse them into one large gram Even one non-black plxel
on a gram boundary will cause the analyzer to measure these adjacent grains as one Achlewng
this condition might be done by careful etching or by setting a binary threshold that renders
all boundaries black If this condition is not met, all area-based measurements will be wrong
Measurements based on intercept counts are less affected by this problem [1] The methods
avadable to complete grain boundaries include manual editing, skeletomzation [3], watershed
segmentaUon [3], and modified convex segmentation [1 ]
Twin Finding
When twins are present, they must be removed or ~gnored by the measuring routine in order
to measure the correct gram size Ifa twin boundary ~s present across an entire grain, the grain
is measured as two. If the twin merely extends partially into a grain, it is irrelevant to area-
based measurement but not to intercept methods Such a twin may also cause a grain bound-
ary reconstruction program to close ~t offand create a false grain. This condmon can be coun-
tered by restricting the gram boundary routine to m l n l m u n seventy, so that it only completes
short lengths of m~ssmg boundary and does not attempt to reconstruct entire missing
boundaries
One way ofehmmatmg interferences from twins is manual measurement, wherein the oper-
ator ignores the twins In fact, mlcrostructures containing many twins have been considered
unsmtable for automatic image analyszs Another approach ~s use of specmhzed etchants that
do not attack twin boundaries [4] Other possibilities include image editing or semmutomatlc
analysis using a digitizing tablet Also, when setting the binary threshold, if only some twins
are filled in, there ~sless edmng to be done or less chance for even an lntelhgent image processor
to make a m~stake
A rtdictal Intelhgence
Because twins look so much like grain boundaries, it is difficult to develop an algorithm that
can distinguish them However, inasmuch as metallographers have little difficulty recognizing
most twins, an mtelhgent computer should be able to do the same One of the first steps was
to identify some of the common forms that twin bands take A compilation of these canonical
forms Is shown in Fig 1 The grain in the lower right portion of the figure is merely a comb1-
FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 245
FIG 1--Comptlatton of some of the forms exhtbtted by twm bands
nation of types One can see that some of these forms divide the entire gram, yet others dis-
appear beneath the plane of the pohsh Some bend back on themselves, whereas others branch
in different d~rect~ons There are, of course, other forms, but if an mtelhgent processor can find
these, it may find others
The one thing that stands out most when looking at these forms is straightness In a first
attempt at twin finding, straightness was the main parameter that we considered. However, we
quickly found out that it was not enough, because gram boundaries may be strmght m parts
In the present approach, the computer examines the scale of the straightness Other factors are
considered such as whether ignoring the structure would make the gram more or less "grain-
hke "Specifically, the computer measures the straightness all along a twin-candidate structure
and follows it even if it bends through angles such as those in Fig 1 It also examines the struc-
ture of the grain containing the candidate to ascertain if identifying a structure as a twin and
removing it would increase the overall convexity of the grain or, conversely, if leaving the
structure would produce two well-shaped grains. In the artificial intelligence approach to
metallographlc image processing, parts of the microstructures are taken as structures, not just
plxels In other words, the computer examines the entire microstructure and breaks it into
structures such as grains, grain boundaries, and twins By doing this, it is then possible to make
intelligent decisions among hypothetical images, that is, ones with different structures
included or excluded These decisions are made by computing a "twlnness score" that IS eval-
uated locally and lteratively, assuming that structures with higher scores have already been
eliminated If ehmlnatlng a twin candidate under consideration results in a higher score, then
that candidate is eliminated and the process repeated for all structures If the score IS lower,
the candidate is put back for reevaluation after other candidates have been examined It is
much faster for a computer to deal only with structures rather than more than a quarter of a
million individual pixels in a 512 by 512 digital image. Nevertheless, the AI approach still
requires the power and memory of a workstation class of computer
In order to ascertain how well this method works, we digitized an ASTM standard grain size
chart with twins (E 112 Plate II) for G = 6 0 Figure 2 shows the portion of the chart that we
digitized Some image processing was done to complete grain boundaries and to reduce the
thickness of boundaries and twins to two pixels A binary threshold was set producing the
image in Fig 2b Some twins were lost in this process. In particular, those that do not extend
across the entire grain may be eliminated in the boundary thinning operation [1], and a few
are eliminated just by carefully setting the binary threshold
Confidence Level--Once the binary image is formed, the twin finder goes to work Although
it is possible to identify twins and to eliminate them all in one step, it is more informative to
merely identify them at first The program classifies structures on the basis of"twinness," and
this measure is called confidence level Each structure is set to a gray level on the basis of the
computer's confidence that it is a twin Those about which it is most confident are set to a
brighter level or color than those at lesser confidence The lowest confidence level is zero or
black, implying that these structures are grain boundaries, not twins There are actually 40
individual levels from 0 to 100%. Figure 2c shows those structures above confidence level 75
as faint white, those below that level as black, and the grains themselves as gray Figure 2d
shows the mlcrostructure after the computer removed the structures it identified as twins
At this point it is necessary to assess how accurately the computer identified a structure and
the consequences of the mistakes it made. To do this, a one-gray-level density slice was passed
through the image This means that a pseudocolor was chosen one level wide (out of 256), and
as it was moved to each of the 40 confidence levels, the authors counted how many structures
were twins and how many were grain boundaries using our best judgment A plot of the results
is shown in Fig 3 We counted 496 total structures in this image and identified 241 of them
as twins and 255 of them as boundaries Figure 3 plots the cumulative number of twins cor-
rectly identified and also the total n u m b e r of grain boundaries minus those it incorrectly iden-
tified as twins, all against confidence level At confidence level 100, six twins were correctly
found, and no incorrect identifications were made As the confidence level was lowered, some
mistakes were made, and the n u m b e r of correct grain boundaries fell from 255 Below about
level 60, few additional twins were identified correctly, and more boundaries were incorrectly
picked up as twins At confidence level zero, all structures are called twins, and the number of
correct grain boundaries drops to zero by definition
We also performed this tedious structure counting on an image of brass with annealing twins
and found the same behavior Figure 4 shows the results This time we found a total of 526
FIG 2 - - D i g i t a l tmagesjpom A S T M ~tandard gram ~tze Plate H, G = 6 Ftgure 2a s'hows the original
tmage Figure 2b shows the resuh o / s e t t m g a binary threshold Figure 2c ~how~ m whlte the ~tructure
l d e n t ~ e d a ~ t~ zn s Ftgure 2d ts the mt6t ()structure alter twin removal
structures, of which we labeled 263 as twins and, comcldentally, 263 as boundanes After com-
paring Figs 3 and 4, it appears that the computer finds twins as a function of confidence level
similarly between a standard grain sxze chart and an image of brass This pattern suggests that
the operator's setting of the confidence hmlt need not be exact Consequently, at the outset of
an analysis, one could have the computer show the various structures with each at its confi-
dence level Then, after becoming satisfied with the setting, run subsequent fields or specimens
at the same level and have the computer both identify and eliminate twins all m one step It is
still possible to manually edit the image, but it is normally not necessary--the intelligent ana-
lyzer ~dentlfies enough twins correctly to measure the nght gram size automatically
Image Analysis
Image analysis is the process of extracting data from images, that is, turning images into
numbers In the case of the standard grain size chart, the relevant question is how senslhve is
260
240 . .
200
180
i ii
160
~ 140
Q,) 120 "I'~ns
~) 100
Z 6o
40
20
0 I I I
100 90 80 70 60 50 40 30 20 10 0
Confidence Level
FIG 3--Plot o f twin confidence level m the A S T M standard gram stze chart versus (1) the number o f
structures correctly ldenttfed as twins and (2) the total number of gram boundary segments remus those
mlsMenttfied as twm~
the A S T M grain size n u m b e r to the confidence level setting A S T M G was measured auto-
matlcally after running the twin finder at three different confidence levels (75, 70, and 62) on
the standard gram size chart for G = 6 The P n n c e t o n G a m m a - T e c h (PGT) image analyzer
we used measures grain size by both the p l a n l m e t n c and intercept methods, so the results of
both are shown m Table 1
The data show that over this range o f confidence levels the A S T M G is no more than 0 5
umts off F r o m F~gs 3 and 4, one can see that most twins are ldenUfied somewhere m the range
o f 6 0 t o 75 Higher confidence levels do not identify enough twins, and lower levels do not find
m a n y m o r e The " n u m b e r of grams" c o l u m n m Table 1 shows how m a n y grams were found
by the ~mage analyzer In the case o f the original ~mage, m a n y grams were found because twin
bands split grains into two or m o r e Original ~mage here means the binary image w~th twins,
m o r e will be sa~d later on the effect o f setting the binary threshold
H a v i n g said that the choice of confidence level is not crucial, we can go on to make mea-
surements on various mlcrostructures both before and after twin removal The data for the
TABLE l--Effect o f confidence level settmg on A S T M G measurement
Confidence Level G (plammetnc) G (intercept) Number of Grains
Original image 72 73 403

75 63 64 218
70 60 62 174
62 55 58 117
280
260
240
Grain B o u n d a n e s ~
220
200
.+..a
r 180
160
O
(.) I40
120
100
80
Z 60
40
20
0
100 90 80 70 60 50 40 30 20 10 0
C o n f i d e n c e Level
FIG 4 Plot o f twin confidence level m a brass specimen contammg twins versus (1) the number o f
structures correctly tdenttfied as twms and (2) the total number o f gram boundary segments mmus those
mlsldenufied as twins
standard gram size chart example are compared with the results of manual analysis in Table
2. The authors each measured the image by the lineal intercept method In accordance with
A S T M (E 112-88) We did this by counting every intercept including twin bands and then
using our judgment to count only grain intercepts, ignoring twins The results in Table 2 show
a difference of a little more than one G unit owing to interferences from twins
The differences between the planlmetric and intercept measurements are interesting We
previously showed that the planlmetnc method is quite sensmve to incomplete grain bound-
aries [1] Just one nonblack pIxel on a boundary fuses two grains together and causes the ana-
lyzer to sum their area If this condition persists throughout the mlcrostructure, many discrete
grams are fused, and the measurement is meaningless Intercept methods are much less sen-
TABLE 2--Measurements o f A S T M G on standard gram size chart
Original Image Binary
Twins Yes No Yes No
ASTM G (manual) 72 60
ASTM G (intercept) 73 62
ASTM G (planlmetnc) 72 60
Number of grains 403 174
sitive to this problem Not surprisingly, however, the intercept method is sensitive to the pres-
ence of twins Twin bands that do not extend completely across a grain are irrelevant to area-
based measurements, but they produce an intercept that does not correspond to a discrete
grain The best approach is probably to make both measurements and, if the results differ, then
look for the reason
Mtcrostructures wtth Few Twms

The grain size of a specimen of a beryllium-copper alloy containing twins was measured
both manually and by automatic image analysis before and after twin removal Although the
grain size of copper alloys is traditionally reported as average grain diameter, we will continue
to use ASTM G for consistency The authors individually measured four fields by the lineal
intercept method (ASTM E 112) and calculated ASTM G Again, we did this by counting
every intercept including twin bands and then using our judgment to count only grain inter-
cepts, ignonng twins These measurements were made on the original gray-scale images before
converting them to binary for automatic image analysis By using the gray-scale image, we had
all the contrast and shading information normally available to a metallographer using manual
methods The microstructure at various stages of processing is shown in Fig 5 The original
gray-scale image is shown in Fig 5a, and the other three images in the figure correspond to the
twin identification and removal process performed on the binary image In this mlcrostruc-
ture, there are not many twins, and setting the binary threshold eliminated some and caused
others to be incomplete This effect can be seen in the results given in Table 3
In this instance, setting the binary threshold clearly eliminated some twins The G = 8 7
that we measured by counting every twin band intercepted is not rephcated in the automatic
analysis It is also evident that the planimetrlc measurement was more accurate, whereas the
intercept measurement was probably fooled by remaining and Incomplete twins But it 1s still
within 0 4 G units of the manual results The total number of grains found by the image ana-
lyzer decreased only from 127 to 108 after twin removal, probably reflecting the few twins that
actually divided grains The total number of grains In the image were not counted manually
Mtcrostructures with Many Twins

An image showing the mlcrostructure of a brass specimen with many annealing twins is
shown in Fig 6 This mlcrostructure, taken from the work ofVander Voort [2], is made com-
plicated by the contrast between twins and grains Contrast within and between grains is useful
for grain sizing by companson with similarly prepared specimens and for identifying twins by
eye However, it makes automatic analysis difficult, because grams, grain boundanes, and
twins have an overlapping dlstnbutlon of gray levels Even an intelligent analyzer that distin-
guishes among structures must first find the structures. Accordingly, we selected this image to
TABLE 3--Measurements of ASTM G on berylhum-copper alloy with few twms
Twins Yes No Yes No
ASTM G (plammetrlc) 74 71
Number of grams 127 108
FIG 5--Dtgltal lmages Jrom a berylhum-copper alloy contammg twtns Ftgure 5a shows the ortgmal
tmage Ftgure 5b shows the result of settmg a binary threshold Ftgure 5c shows m white the structures
zdenHfied as twins Figure 5d is the mtcrostructure after twm removal
see if there was any chance of identifying most of the twins and then accurately measunng
grain size
As one can see in Fig 6b, just setting a binary threshold eliminates many twins but certainly
not most of them The process of finding them by AI was largely successful but not perfect
Some twins remained, yet, lowering the confidence threshold would cause the mlsldentlfica-
tion of too many grain boundaries. Nevertheless, in an image with enough grains, the errors
in twin identification do not seem significant The results are given in Table 4
In like m a n n e r to the beryllium-copper alloy, manually counting every twin band produced
a grain size much too small The G = 6 9 that we measured was not replicated by the auto-
matxc image analyzer, it measured 6 4 and 6 3 before twin removal because twins were ehm-
mated by setting the binary threshold After twin removal, again at Confidence Level 70, the
analyzer found G = 5 3 by both methods, and this is in good agreement with G = 5 6 mea-
sured manually If we had selected Confidence Level 75 for twin removal by AI, the result
would be G = 5.5 by both intercept and planlmetnc methods, with a total of 212 grains
FIG 6--Digital zmages from a brass speezmen containing many twlm Flgwe 6a shows the original
image Figure 6b shows the result of setting a binary threshold Figure 6c shows m white the structures
identified as twins Figure 6d is the mlcrostructure after twin removal
TABLE 4--Measurements of A S T M G on brass with many twms
Twins Yes No Yes No
ASTM G (plammetnc) 63 53
Number of grams 418 181
remmnlng. The consequence of these results 1s that ASTM G is not a strong function of con-
fidence level, and it is possible to come within 0 5 G unit even on a d~fficult image In fact, it
is probably more important to set the binary threshold carefully than it is to select the exactly
right confidence level in the AI system
Summary and Conclusions

The presence of twin bands in a m~crostructure whose grain size is to be measured is at least
a complicating factor and an impediment to automatic image analysis The benefits of auto-
matic image analysis arise not from increased accuracy or speed over manual methods, but
from increased reproduclblhty both from specimen to specimen and from operator to opera-
tor Furthermore, skilled operators are free to perform other tasks while the analyzer measures
grain size Some image processing IS often necessary before image analysis, but it should never
be considered a substitute for proper specimen preparation and metallographic technique
Processing such as smoothing or crlspenlng can be accomplished by well-defined mathemat-
ical operations Grain boundary reconstruction and twin elimination, on the other hand, are
not easily accomplished by straightforward computer methods They are, however, amenable
to an artificial intelligence approach And the twin removal problem in particular requires a
computer with some of the knowledge ofa metallographer Another advantage of AI is that as
more knowledge becomes available it is easily taught to the computer
Once the images are suitable for analysis, measunng them is extremely rapid For example,
a field with several hundred grains can be analyzed in several seconds And in that time, 75
standard or user-defined measurements can be made on every grain Moreoever, not only are
field measurements such as ASTM G available, entire distributions of size and shape are also
available for structure/property correlations The accuracy of automatic Image analysis
depends on the quality of the image analyzed The measurements are virtually perfect if the
grains are delineated properly and the boundaries are in the right places Tests that we have
conducted previously [1], as well as those described in this paper, lead us to conclude that the
use of artificial intelligence for grain boundary reconstruction and twin identification works
sufficiently well to lead to an accurate measurement of grain size
Acknowledgment
The authors acknowledge discussions with Dr T Williams and his colleagues at Amennex
Artificial Intelligence, Inc Their collaboration in the basic area of knowledge englneenng
allowed us to develop the complex, competing strategies used in the AI method
References
[1] Fnel, J J, Prestndge, E B, and Glazer, F, "Gram Boundary Reconstruction for Gram Sizing,"
MtCon 90 Advances m Vtdeo Technologyfor Mwrostructural Control, ASTM STP 1094, G F Van-
der Voort, Ed, American Society for Testing and Materials, Philadelphia, 1990, pp 170-184
[2] Vander Voort, G F, "Grain Size Measurement," Practtcal Apphcatlons of Ouant~tattve Metallog-
raphy, ASTM STP 839, J L McCall and J H Steele, Jr, Eds, American Society for Testing and
[3] Serra, J, Image Analysts and Mathematlcal Morphology, Academic Press, London, 1982
[4] Vander Voort, G F, Metallography Prlnctples and Practwe, McGraw-Hill, New York, 1984
Scott T. Bluni, 1 Katherine M. Goggins, 1 Brian J. Smith, ~and
ArnoM R. Marder I
The Use of Quantitative Image Analysis for

the Characterization of Corrosion-Resistant
Coatings
REFERENCE: Blunl, S T , Gogglns, K M , Smith, B J , and Marder, A R , "The Use of Quan-
titative Image Analysis for the Characterization of Corrosion-Resistant Coatings, Metallogra-
phy Past, Present, and Future (75th Anniversary Volume), ASTM STP 1165, G F Vander
Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, Amencan Society for Testing and
ABSTRACT" Materials are subjected to corrosive environments in many engineering applica-

tions Among the most successful techniques employed to minimize matenal degradation in
such environments is the use of protective coatings, which may be non-reactive or serve as sac-
nficlal barriers to a particular corrosion process Coating deposition methods include hquld
sohdlfiCatlon deposition (hot-dip), vapor deposition (pack cementation), and hquld droplet con-
solldatlon (spray) processes Galvanneal, chromlzed, and electric arc spray are respective exam-
ples of these coating processes All of these coatings have been used extensively and have proven
successful at reducing substrate corrosion in various service environments
The coating structural charactenstlcs that may influence coating performance include coating
thickness and thickness vanatlon, volume percent porosity or voids or both, volume percent
flaking or cracking or both, and the presence and dlstnbutlon of different phases Such charac-
tenstlcs have been examined traditionally by direct inspection techniques that are not often accu-
rate, time-efficient, or reproducible The ability to gather more reliable measurements is neces-
sary to further enhance the understanding of these coatings and lead to the estabhshment of
structure-property relationships
The techniques of computer-automated image analysis permit materials scientists and engi-
neers to quickly evaluate a coating structure Relevant measurements that can be tailored to indi-
vidual coatings are readily obtained in an accurate and precise manner with the use of such quan-
titative systems This paper discusses critical mlcrostructural characteristics for galvanneal,
chromlze, and thermal spray coatings Measurement procedures for such charactenstlcs with the
use of an automated quantitative image analysis system are discussed
KEY WORDS: quantitative image analysis, hot-dip galvanneal, chromlze coatings, thermal
spray coatings, metallography, mlcrostructure, metallurgical specimens, metallographlc
techniques
C o r r o s i o n - r e s i s t a n t coatings are fast b e c o m i n g the preferred m e t h o d for e n g l n e e n n g c o m -

p o n e n t p r o t e c t i o n W h e r e a s s o m e c o a t i n g technologies h a v e existed for m a n y years, there h a v e
b e e n m a n y recent process modifications. A l t h o u g h the r a n g e o f corrosion-resistant coating
technologies a n d a p p h c a t l o n s is rapidly e x p a n d i n g , the research, quality control, a n d micro-
structural c h a r a c t e r i z a t i o n t e c h n i q u e s used to s u p p o r t this growth h a v e b e e n slow to c h a n g e
T h e n e e d for systematic, precise, a n d a c c u r a t e e v a l u a t i o n p r o c e d u r e s h a s forced b o t h research-
Research assistants and professor, respectively, Department of Materials Science and Englneenng,
Whltaker Lab No 5, Lehigh University, Bethlehem, PA 18015
254
Copyright
Copyright*by1993
ASTMbyInt'l
BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 255
ers and manufacturers to consider many options Quantitative image analysis (QIA) is one
technique that has proven to be well-suited for coanng mlcrostructural evaluanon
Automated image analysis techniques are amenable to vanous quality control, processing,
and research applications In comparison to traditional measurement methods, quantitative
image analysis procedures are fast, accurate, reproducible, and allow for the immediate storage
and manipulation of large quantlnes of data The objective of this work IS to illustrate the
advantages of image analysis processes by describing the methods used to charactenze micro-
structural features that influence performance for a number of corrosion-resistant coatings
Hot-Dip Galvannealed Coatings

Purpose of Coating
Zinc coated steel sheet is used extensively m automobile apphcatlons due to the stringent
corrosion resistance requirements placed on car manufacturers [1-3] When coupled with
steel, zinc acts as the sacrificial anode offering protection to the steel substrate Being the more
reactive metal, zinc will preferentially corrode [4]
Hot-d~p galvanneal is a strong competitor as a corrosion resistance coating because it offers
enhanced performance properties over similar corrosion resistant coatings at low producnvlty
costs These properties include superior weldabdlty, scab corrosion resistance, and good pamt-
abflxty[2,3,5] However, due to the formanon ofbrlttle iron-zinc (Fe-Zn) mtermetalhcs dunng
processing, the coating tends to crack or powder during subsequent press-forming operations
Presently, the United States and Japan combined produce 5 2 mdhon tons per year & h o t - d i p
products for automotive applications [6]
Coating Charactertsncs
For automobile applications, hot-dip galvannealed coatings weights are between 45 and 100
g/m 2 [2,5] and the coating thickness is approximately 10 um Figure l a illustrates a fully
alloyed Fe-Zn coating containing several mtermetalhc layers Coating propertms are influ-
enced by the coanng morphology, thickness, and phase dlstrlbunon The use of QIA aids m
companng and determining the formabfllty of different coatings that contain vaned phase
morphologies due to vaned processing parameters
Measurement of Crmcal Coating Parameters

Some of the mlcrostructural features used to evaluate coating performance are coating
thickness and thickness variation and powdering The techniques used to evaluate these prop-
ertles with quantitative image analysis (QIA) techniques are described below
Coating Tkwkness--Coatmg thickness and thickness variation are crlncal properties in
coating processing. Varlanons of thickness cause uneven alloying rates that produce different
forming properties throughout the coating QIA offers an efficient method for measuring these
properties This fully automated method is qmck and more accurate than the conventmnal
method of measuring scanning electron or light optical mlcrographs
QIA sample preparation is identical to light optical metallography preparahon The sample
is pohshed to a 0 25 micron finish and etched with a modified Rowland's solution [7] The
etchant not only bungs out the true mlcrostructure of the coating but it also changes the grey
level of the coating from that of the substrate material
In using QIA techniques, the coating ~s first thresholded by grey level, from Fig. 1a to b In
this case the coating consists of two grey levels Since the resulting red binary image corre-
FIG 1--Image analy~ l s procedures &r mea yurmg galvanneal coating t&ckness (a) typtcal galvanneal
coating, (b) thre~holded coatmg, (c) tmage appearance after feature hmtts, (d) superlmposed grtd used to
determine coating thickness', and (e,f) result display of typical measurement~
sponds to constituents also contained in the substrate, it is sized so that irrelevant substrate
matenals are discarded The two remaining binary images are combined, representing the
entire coating layer, Fig 2c A vertical grid IS superimposed on the coating and a new image is
created that marks the intersection of the coating with the grid lines Next, a feature limit is
set to ensure that any erroneous measurements due to damaged, cracked, or crushed coating
are not included in the measurement The length of the remaining lines shown in Fig 2d is
now measured to determine coating thickness From this particular image frame, 46 mea-
surements were taken and the average coating thickness was 11 6 ___ 1 5 ~m (note that where
data are written x _+ y, y denotes one standard deviation) The resulting histogram is illustrated
in Fig 2e With use of an automated stage, data from several fields are compiled into one his-
togram and better statistics can be obtained
P o w d e r l n g - - T y p I c a l l y , galvannealed coating performance is evaluated qualitatively Most
steel companies have individual test methods to evaluate the formation and adhesion prop-
erties of the galvannealed steel sheet These tests are quick, on-line methods for examining the
FIG 2--Slcp~ ~ e d to determine pe:~etTt p~,~tderm:~ m gal~annca/ ~oalmgs (a)/ormd u~almg, (b)
thre~holded zmage, (c) coalln,~., and background bmar) m~agc a/let ~ub~'irate ~cl)arafmn and (d) hacL-
ground and ~oaring la) er ~epat alzon
FIG 2 (r onzmued)--(e) Lnttre coaling layer, (f) hortzontal grld ~uperlmpo~ed onto tmage, (g) [eature
hmlt~ ate ~et on the bmar) gpld/backL, round tmage to include only cracked or powdered tegmns, and (h)
odahedta[ dt/auon enables ~racked and powdered Jegtons to be fEh'd Percent crackmg or powdering t~
no~4 measured
quality of the coating One method 1s the peel-offtest Adhesive tape is apphed to a sample
either before or after forming The sample is formed by one of two methods, a bend test or a
cyhndrlcal cup draw-test The tape is then compared visually to a qualltatlve standard rating
system Th~s test is not quantitative nor particularly accurate A more quantitative method ~s
performed by QIA
A formed coating IS Illustrated in Fig 2a The coating layer and the background material
are first thresholded by different grey levels Because the substrate material is of the same grey
level as part of the coating and the background materials as shown by the binary image in Fig
2b, steps to distinguish these features are needed A size limit is set on the coating to exclude
the substrate material, Fig 2c The background material, coating, and cracks are next sepa-
rated A vertical grid as superimposed onto the background and coating layer, Fig 2d, that acts
to fragment the image into small segments By means of aspect ratio limitations, the segments
that correspond to coating phases are added to the coating layer, Fig 2e A horizontal grid is
superimposed onto the screen and combmed with the thresholded regions to form a new image
shown m Fig 2 f A feature size limit is then set so that the glad only lies within the spaces and
gaps o f the coating, Fig 2g Next, a vertical grid Is superimposed on the remaining horizontal
lines, and the points of intersection form another binary image. These points are ddated to fill
the spaces where the coating does not exist. The parts of the dilated binary image that over-
lapped onto the coating layer are deleted As shown m Fig 2h, the resulting image Is the com-
bination of two binary images, one corresponding to the coating area, and the other to the
powdered or cracked area in the coating F r o m this, a plane fraction o f powdered or damaged
coating can be determined Results indicate that 25 80% of this coating is cracked or has pow-
dered from the substrate
Chromize Coatings
Purpose of Coating
Chromlzmg, the process of coating a substrate metal/alloy with chromium, is a popular
choice for high-temperature surface protection. The chromlzlng process is inexpensive, appli-
cable to a w~de range o f metals and alloys, and is amenable to various part configurations
[8] The coating is formed by diffusing chromium atoms into a metal substrate that produces
an alloy layer that is an integral part of the substrate The high chromium alloy layer develops
a slow growing, t e n a o o u s surface oxide, that protects the substrate component from acceler-
ated corrosive attack The coating is also i m m u n e to the flaking and spallatlon problems that
afflict plating, overlay, and spray coatings Chrom~ze coatings are presently used extensively
in fossil-fired power generation plants and are being considered for certain aerospace
apphcatlons
Coatlng Charactertsttcs
An as-received chromlze coating mlcrostructure is shown m Figs 3a and b at magmficatlons
of • 100 and • respectively The coating mlcrostructure consists of an outer layer that
appears featureless at low magnification, columnar grains, grain boundary and lntragraln car-
bides, a black void layer beneath the outer layer, and a distinct coatlng/substrate interface The
Murakaml's reagent used for etching these samples has been shown to etch M6Cand M2C type
carbides Investigators have determined that the chromlze coating carbides consist of both
chromium and molybdenum carbides [ 9,10] The void layer and the columnar grain structure
are caused by the chromlzlng process itself [11-13]. The coatlng/substrate interface is very
abrupt and has been attacked aggressively by the pzcral etch, indicating the presence of car-
bides at the interface This interface is thought to act as an lnterdlffUSlOn barrier restricting
continuous chromium migration during service A direct consequence of the Interface for-
marion is a large decarburlzed substrate layer, immediately adjacent to the interface
Measurement of Crmcal Coating Parameters

Research into chromlze coatings indicates that the two critical mlcrostructural features that
influence coating performance are its thickness and porosity content Measurement of each
will influence repair and replacement decisions.
Coating Thtckness--Because the coating is designed to act as a protective barrier for the
substrate, maintaining a specified coating thickness is essential to extending the service life of
a component Traditionally, coating thickness measurement is performed in two ways (1) in
SltU measurement of component dimensions using a nondestructive evaluation technique, or
260 METALLOGRAPHYPAST, PRESENT,ANDFUTURE
(2) removal of the component and metallographlcal analysis of coating thickness The latter
is the more accurate method Metallographlc thickness measurements are usually performed
manually or with an operator-interactive semiautomated image analysis system
In this example, the chromlze coating was ground and polished using tradmonal metallo-
graphic methods It was etched very deeply using Murakami's reagent, note the heavy attack
at the coating substrate interface, Fig 3a Measurement ofchromlze coating thickness by QIA
begins by removing the mount material and substrate material from the initial live image This
is done by first thresholdlng the image to highlight the darkest Image features, that is, m o u n t
material, porosity, and coatlng/substrate interface Image dilation of the thresholded regions
was required to enhance the lnterfaclal feature, Fig 3c The next step isolates the mount and
substrate from the coating by superimposing a horizontal grid upon the image and eliminating
all discontinuous lines, which correspond to the coating porosity The remaining grid lines are
combined with the previously thresholded regions resulting in a series of rectangular regions,
the largest being the coating, Fig 3d The m o u n t and substrate rectangles are then removed
by Imposing appropriate dimensional restrictions Since the coating region still possesses some
residual m o u n t and substrate material, an aspect ratio feature limit is introduced to eliminate
both The coating thickness is then measured by placing a vertical grid on the image, combin-
ing these lines with the coating Image, and measuring the length of the resulting lines, Fig 3e
The coating shown in Fig 3a was measured using this procedure and found to have a thickness
331 + 2 45 u m
Porosity Content--Porosity in chromlze coatings may act as initiation sites for coating fail-
ure This porosity is typically subsurface, but may also be in the outer coating layer depending
on the coating process parameters used These Internal free surfaces may act as crack initiation
sites or facilitate both thermal fatigue or corrosion fatigue crack growth The void content of
diffusion coatings is rarely quoted in the subject literature
Fully-automated image analysis is suited uniquely to measure porosity Porosity size, shape,
and area fraction can all be obtained quickly, accurately, and precisely The measurement
technique is similar to the one used m the coating thickness measurement, since the same step-
wise coating isolation is used for both First, the m o u n t material and the substrate matenal
features must be isolated and removed from the image (using the same thresholdmg and ehm-
inaUon techniques as described previously), Fig 3a In thresholdlng these two features, the
porosity is also included Therefore, a feature limit must be Imposed to exclude the porosity
and coating from the m o u n t material and substrate The coating and porosity are then placed
In another binary image, producing an image containing no m o u n t or substrate material The
image features (coating and porosity) are then thresholded again and placed on separate binary
images Residual m o u n t and substrate material are eliminated using an aspect ratio feature
limit leaving the true coating dimensions visible The coating and porosity are then brought
back together in the same binary image, Fig 3f The porosity area fraction, size, and shape can
now be measured The coating shown in Fig 3a was measured using this procedure and found
to possess 1 27 + 0 30% porosity
Thermal Spray Coatings

Purpose of Coatlng
Thermal spray coatings are used for a broad range of apphcatlons in which corrosion, wear,
or high-temperature protection is needed Such coatings provide a sacrificial bamer for a sub-
strate material, as they are either nonreactive or form a coherent, protective scale One advan-
tage of thermal spraying that makes it particularly attractive for some applications is the ability
to apply coatings in SltU Some of the industries that employ these coatings include aerospace,
BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSTS 261
FIG 3--Steps used to measure chromtzed coatmg thtcknes+ and porostty (a,b) as-received chromlzed
coating, (c) image thresholdmg and mterfacml dtlatlon reqmred to tsolate coating from other linage fea-
tures, (d) dtvtslon of the tmage into separate regtons, (e) grid superlmposed on the image that is used to
measure coating thwkness, and (f) f n a l tmage used to measure coatmg porosay content and morphology
electronics, paper, automobile, utdlhes, matenal extracnon and manufacturing, and gas
turbine.
Coatmg Characteristics
A typical thermal spray-coating mlcrostructure is shown m Fig 4a, which is an electric-arc
spray coating Thickness is usually on the order of several hundred m~crons for an apphcanon
such as power plant boiler tubes Porosity can result from poor "splat" flow or from gas entrap-
ment between droplets. The total porosity volume frachon may be I to 15%, depending on the
deposition process Omdes, which appear as dark mlcrostructural constituents, can form as
droplets and travel from the gun to the substrate In addition, some oxides may be contained
within the feed material p n o r to spraying
Measurement of Crtttcal Coating Parameters

Poroslty--Poroslty has been noted generally to degrade the mechamcal properties of ther-
mal spray coatings [14] Both the volume percent and morphology of pores will dictate the
extent of property degradation For example, a pore with a large aspect ratio and correspond-
mg "tips" will provide a larger stress concentration than an equlaxed pore and may be more
likely to propagate as a crack upon the application of stress
Unfortunately, pores, oxides, and mounting material possess similar grey levels when
observed with a light optical microscope, as can be seen by inspection of Fig 4b For porosity
detection, thermal spray coatings should be vacuum mounted m fluorescent epoxy [ 15] Sam-
ples are ground with 320-grit slhcon carbide (SIC) paper just until the surface epoxy layer has
been removed By using fluorescent lighting microscopy and a color camera in conjunction
with an image analysis system, porosity is easily detected (Fig. 4c) and differentiated from all
other coating constituents. As shown m Fig 4d, the mount material will also be detected, but
can be ehmmated with a size hm~tanon The size, shape, and dlstnbunon of pores can now be
easily measured It ~s necessary to separate the coating from the substrate and mount materials
m order to determine porosity volume percent, and this can be performed under bnghtfieid
dlummatlon m the same manner as descnbed for coating thickness measurement A typical
thermal spray coating contains a porosity content of 5.15 + 0 99%
OxMes--hke porosity, oxides can degrade the mechanical properties of thermal spray coat-
rags as they are often bnttle and fractured easily with the apphcat~on of stress Oxides can be
thresholded readily with bnghtfield Illumination, and that contnbunon from porosity can be
subtracted using the porosity detection techniques described earher As an example of
acquired results, an oxide content of 25 97 + 0 52% was found for an electnc-arc spray
coating
Coatmg Thickness--Coating thickness is one cnncal mlcrostructural parameter that influ-
ences performance The effect of thickness is twofold as thickness increases, ( 1) substrate pro-
techon is enhanced as there is additional sacnficml matenal available, and (2) stresses that
develop upon heatlng/coohng of the coating system Increase due to thermal expansion m~s-
match. There should be an optimum coating thickness for each apphcahon and coating system
m particular
The task of thickness detection by fully-automated image analys~s procedures can be diffi-
cult because the substrate and mount matenals are often of the same grey level as many of the
coating components (refer to Fig 4a) and therefore cannot be easily dlfferennated The solu-
non to this problem lies within mlcroconsntuent contmmty; that is, the coating elements are
noncontmuous, while the substrate and mount materials are continuous m at least one dlmen-
FIG 4--[hermal ~pra) ~oalmgpo~osl[t measurcmen[ (a)as-apphedelectr~c-arc sp~al coalmg rmcro-

sltuclure (b) spa)' coating stlucture sho~mg slmEap grey leve]~ bet~een porosity, oxides and mount
rnaterml (c) obso ration o/poto~ttv and mount rnalertai wlth fluorescence hghtmg microscopy, and (d)
thresholdmg of por<)gll~ and mount materml, and converslon to binary zmage
slon When detected and thresholded by grey level, the coating components of a given grey
level range will therefore be observed as many particles, each of which is smaller in some
dimension than the mount or substrate material that has also been detected This is illustrated
in Fig 5a, where the mount material and coating porosity and oxides have been thresholded
together As shown m Fig 5b, the coating constituents are separated from the mount material
by placing sJze limitations on the binary image features The same concept is used to separate
the light coating background from the substrate material, as shown in Figs 5c and d By
manipulating the image such that the mount and substrate materials are all that remain, the
coating can be identified as the image portion that has not been detected As shown in Fig 5e,
the coating retains its charactensUc shape, but is now observed as a continuous entity Mea-
surement of coating thickness can now take place by superimposing a template of parallel lines
that are normal to the coatmg length, retaining that portion of the lines that Intersect the coat-
ing area, and measunng the length of these lines Figure 5fshows the resulting correspondence
FIG 5 - - l hermal splay ~oalmg thuknes s measurement (a) deleclton o! mount material and coating
poro~lt~/o~ldes, (b) mount material removal from the "green" hmar~ tma,~e, (c) dete~tton o/substrale
materta/ a n d c ore el slon lo "blue" binary mTage, (d) e h m m a t m n o/ substrate [rom blue binary ~mage, (e)
tdentthcatzon o f t oaring matep ml, and (f) grtd supertmposed on image to m e a sure coatmg thteknes s"
between the coating mlcrostructure and the generated hnes that are used to measure coating
thickness As an example of obtained results, a thickness of 543.35 _+ 60.26 ~m was found for
an electric-arc spray coating
Summary
Quantitative image analysis procedures have proven to be fast, accurate, and reproducible
m the evaluation of various corrosion-resistant coatings The thickness and powdenng of hot-
dip galvannealed coatings, and the thickness and porosity of chromlzed and thermal spray
coatings are measured readily by QIA techniques The systematic evaluation of microstruc-
rural features with QIA may enhance the understanding of these coatings and lead to the estab-
lishment of valuable structure-property relationships
Acknowledgments
The authors would hke to thank Arian Benscoter for metallographlc consultation, and the
members of Pennsylvania Electric Research Council (PEERC) for their support
References
[1] Kalson, A M, "Coated Steel Sheets in North America--An Automotive Perspective," GALVA-
TECH, The Iron and Steel Institute of Japan, Tokyo, 1989, pp 271-272
[2] Denner, S G , "An Overview of the Manufacture and Apphcatlon of Zinc and Zinc Alloy Coated
Steel Sheet m North America," GALVATECH, The Iron and Steel InsUtute of Japan, Tokyo, 1989,
p 101
[3] Hada, T, "Present and Future Trends of Coated Steel Sheet," GALVATECH, The Iron and Steel
Institute of Japan, Tokyo, 1989, p 112
[4] Uhhg, H, Corroston and Corrosion Control, Wdey, New York, 1985, pp 234-235
[5] Hlsamatsu, Y, "Science and Technology of Zinc and Zinc Alloy Coated Steel Sheet," GALVA-
TECH, The Iron and Steel Institute of Japan, Tokyo, 1989, p 3
[6] Informatzon supphed by the International Lead and Zinc Research Orgamzatlon
[ 7] Rowland, D, Transactzons, American Sooety for Metals, Vol 40, 1948, p 983
[8] Rapp, R A, Wang, D, and Welsert, T, Htgh Temperature Coatmgs, M Khobalh and R C Kru-
tenant, Eds, The Metallurgical Sooety of the American InsUtute of Mining, Metallurgical, and
Petroleum Engineers, Warrendale, PA, 1986, pp 132-142
[9] Wada, T , et al, MetaOurgwal Transacttons, Vol 3A, No 11, 1972, p 2865
[10] Perry, A J and Horvath, E, Journal ofMatertal Sctence, Vol 13, 1978, p 1303
[11] Saunders, S J R, and Nlcholls, J R, Material Sctence& Engmeermg, Vol 5, 1989, p 780
[12] Sequelra, C A C and Nunes, C M G S, SurfaceEngmeermg, Vol 3, No 2, 1987, p 161
[13] Samuel, R L and Lockmgton, N A, Metal Treatment and Drop Forgmg, Oct 1951, p 440
[14] McPherson, R, Surface and Coatings Technology, Vols 39/40, pp 173-181
[15] Herrmann, E, PractlcalMetallography, Vol 20, 1983, pp 371-387
George F. Vander V o o r t I
Examination of Some Grain Size

Measurement Problems
REFERENCE" Vander Voort, G F , "Examination of Some Grain Size Measurement Prob-
lems," Metallography Past, Present, and Future (75th Anmversary Volume), A S T M STP 1165,
G F Vander Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for
Testing and Matenals, Philadelphia, 1993, pp 266-294
ABSTRACT: The measurement of grain size is performed nearly always on a metallographically

prepared cross section, suitably etched to reveal the gram structure, using methods that pertain
only to the grain cross sections These measurements are termed planar and some may be con-
verted mathematically into spatial estimates of the size of the three-dimensional grains How-
ever, the vast majority of such work is planar where no assumptions about grain shape are
required and grain size is described in one- or two-dimensional terms (intercept length, diameter,
or area) based on sections through the grams The most frequently used measurement methods
are described m this paper and compared using the same images These methods are the Jeffnes
planimetnc method, the tnple-polnt count method, and the Heyn intercept method These
methods base grain size on two-dimensional, zero-dlmensmnal, and one-&mensmnal features
of the mlcrostructure, respectively (that is, areas, points, and hnes)
Test lines can be utdized to count grain mterceptmns or grain boundary intersections, or,
actual intercept length measurements may be made Furthermore, the test hnes may be straight
or curved (circular test lines being commonly employed) Does the curvature of a circular test
line cause a bias in e~ther mtercept/intersectmn counts or intercept length measurements9 When
a digitizing tablet is used w~th a c~rcular test line, either chord lengths between sets of gram
boundary intersections, or arc lengths between the grain boundary intersecUons can be mea-
sured Does either practice cause bias, or are the results s~mdar? How do averages of intercept
lengths compare to the mean hneal intercept calculated from the reoprocal of the number of
intercepts (or intersections) per unit length9 Does the triple-point count method produce the
same results as the planimetnc results and how do these esUmates of the ASTM grain s~ze num-
ber compare to that from the intercept procedures9 These questions are addressed
KEY WORDS: metallography, grain size, quantitative metallography, Jeffnes plammetrlc

method, Heyn intercept method, dlgaUzlng tablet, statistical analys~s, metallurgical specimens,
mlcrostructure, metallographlc techniques
G r a i n size m e a s u r e m e n t s are p r o b a b l y the single m o s t i m p o r t a n t m l c r o s t r u c t u r a l m e a s u r e -

m e n t p e r f o r m e d , for either quality c o n t r o l or research p u r p o s e s G r a i n s are t h r e e - d i m e n s i o n a l
features; but, in the vast m a j o r i t y o f cases, they are viewed a n d m e a s u r e d o n a Nsectlng, two-
d i m e n s i o n a l p l a n e t h a t is p o l i s h e d a n d e t c h e d Because o f this, m o s t m e a s u r e m e n t s are o f a
p l a n a r r a t h e r t h a n a spatial n a t u r e . N u m e r o u s a p p r o a c h e s h a v e b e e n developed to m e a s u r e
grain size o n p o h s h e d a n d e t c h e d cross sections, a n d several a p p r o a c h e s are avmlable to trans-
late p l a n a r d a t a to spatial e s t i m a t e s o f g r a m size All o f these require s o m e simplifying a s s u m p -
t m n a b o u t grain s h a p e that, o f course, is n o t c o n s t a n t in a n y s p e o m e n D~rect m e a s u r e m e n t
Materials Characterization, Carpenter Technology Corporation, R & D Center, Reading, PA 19612-

4662
266
Copyright
Copyright*by1993
ASTMbyInt'l
VANDER VOORT ON GRAIN SIZE 267
of spatial grain size is very difficult requmng either serial section analysis or mtergranular dis-
integration (liquid metal embnttlement) and direct measurement of the liberated grains
These methods are only applied m research studies
While there are a number of approaches for measuring planar grain size [ 1 ], some are more
efficient than others The chosen method should produce the most precise value for the least
amount of work For any method, the procedure must be well defined and clearly descnbed
This has been the goal of ASTM grain size standards, such as ASTM Methods for Determining
Average Grain Size (E 112-88), ASTM Methods of Estimating the Largest Gram Observed in
a Metallographlc Section (ALA Grain Size) (E 930-83), ASTM Test Methods for Character-
lzmg Duplex Grain Sizes (E 1181-87), and ASTM Test Methods for Determining the Average
Grain Size Using Semiautomatic and Automatic Image Analysis (E 1382-91). In this paper,
we will deal only with planar grain size measurement methods. These are free of any assump-
tions about grain shape
Definition of Grain Size

Dtfferent measurements have been used to assess the "size" ofgrmns Hlstoncally, the plan-
1metric method, suggested by Albert Sauveur [2] and refined by Zay Jeffnes [3,4], was the first
widely used techmque m the United States while the intercept method, developed by Emil
Heyn of G e r m a n y [5], was the first method widely used in Europe With the plammetnc
method, the grain size was described in terms of either the number o f grains per square md-
hmetre (mm 2) at • 1, NA, or as the square root of the average grain area, A, which is called d.
With the intercept method, the grain size was defined as the mean hnear (or lineal) intercept
length, L3, which is the reciprocal of the number of intersections of grain boundanes per unit
length of test line, PL, or the number of grams Intercepted per unit length of test line, NL The
subscript, 3, means that the measurement is valid m three dimensions The use o f d t o describe
grain size by the Jeffnes method should be discouraged as it is calculated as the square root of
the average grain area that suggests that grains are square on the cross section, which they are
not Calculation of the diameter of a circle ofeqmvalent area ("equivalent circle diameter") is
a shght Improvement, but not much better Use of NA, a basic stereolog~cal parameter, to
define the planar grain size is recommended
The lack of a simple mterconverslon between the results of these two methods, that is,
between NA and NL or PL, has been a well-recognized weakness NA is a function of the total
length of grain edges per unit volume, Lv, while NL or PL (for a single-phase structure) is a
function of the grain boundary surface area per unit volume, Sv [6] Thus, these two measures
of grain size are based on different geometric characteristics of the grain structure To date,
there is no direct relationship between Lv and Sv and no experimental data linking the two for
the same specimens as a function of grain size
While the first (1930) comparison grain size chart (for copper and copper-based alloys)
scaled the grain size based on uniform linear increments of d, later charts used a power senes
and scaled the chart pictures based on NA increasingly exponentially The charts listed either
the NA value (number of grains per square Inch at • 100) or the "ASTM grain size number,"
G, from the following equation
n = 2 G-I (1)
where n is the number of grams per square inch at • 100 magnification To obtain NA as the
number of grains per m m 2 at • 1, multiply n by 15 50031 Hence, NA lS related directly to G
and is measured readily by the Jeffnes method, or by the triple-point count method.
Jeffries Planimetric Method

This method requires the counting of the number of grains m a known test area, usually
circular m shape. A orcle of 79 8-ram dmmeter (5000 m m 2) is drawn on a mlcrograph or a
template with such a circle ~s placed over a ground glass.projection screen or televlsmn mon-
itor The magnification is chosen so that at least 50 grams are within the test area Next, the
number of grains completely within the test area, n j, and the number of grams intersecting the
circle, n2, are counted. To obtain an accurate count, the grains must be checked offor n u m -
bered which slows down the analysis as either a new template must be used for each field count
or It must be cleaned between counts. Several fields must be counted in order to obtain a sat-
isfactory level of preoslon This number would depend upon the umformlty of the gram
structure.
The sum of n j and n2/2 is mulUphed by the Jeffnes factor,f, for the magmficatmn employed
with the 79 8-ram-diameter circle to obtain NA, the number of grains per m m 2 at • 1 T h e f
value is obtained from
f = M2/5000 (2)
where M is the linear magnification Ifa circle of a different diameter is utilized, substitute its
area (m m m 2) for 5000 m Eq 2
The average grain area, A, is obtained from the reciprocal of N~
-A = 1/NA (3a)
where A is I n m m 2, or
= 106/NA (3b)
where A is m square mlcrometres (um 2) The Jeffnes grain diameter, d, is the square root of A,
but use of d should not be encouraged because grain cross sections are not square G can be
calculated from NA (number of grams per m m 2 at • l) from
G = (3 222 log N~) - 2.954 (4)
or, from Table 2 ofASTM E 112-88
Triple-Point Count Method

This method, suggested by Cynl Stanley Smith [ 7], utlhzes Euler's law to obtain NA A orcle
of known size is placed over a mlcrograph, or a template with such a circle ~s placed over a
ground glass projection screen or television momtor. Although no statlsUcal studies of this
method have been made, the magnlficatmn should be chosen so that at least 40 to 50 tnple
points are present Too high a n u m b e r per test area may make counting imprecise and difficult
Again, a n u m b e r of such counts should be made and the triple points must be marked off as
they are counted to obtain an accurate count If a four-ray grain juncUon ~s observed, which
is rare, it is gwen a count of two NA ~Sdetermined from
N~ - (P/2) + 1 (5)
Ar
where P is the n u m b e r of triple points 0unction point of three grains on the plane of polish)
counted, ATIS the test area in m m 2 at • l, and NA is the number of grains per m m 2 at • 1 G
is calculated from Eq 4 or from Table 2 ofASTM E 112-88.
Heyn Intercept Method

Unlike the Jeffnes method and the triple-point count method, the Heyn intercept method
does not require marking off of the intercepts or intersections to obtain an accurate count.
Hence, this method is faster than the other two, and the same degree of precision can be
obtained in less time The intercept method is useful for deformed grain structures, and a mea-
sure of their elongation can be obtained while G is determined Interest In the Heyn Intercept
method in the United States was stimulated by the work of John Hllliard [8] and Halle
Abrams [9].
Lines of known length are drawn on a template and placed at random over a micrograph,
projection screen, or TV monitor For a deformed (nonequiaxed) grain structure, one or more
parallel straight test lines are placed over the grain structure with orientations parallel and per-
pendicular to the deformation (longitudinal usually) direction For an equiaxed gram struc-
ture, ASTM E 112-88 recommends circular test lines (three concentric circles with a total cir-
cumference [line length] of 500 ram) Circular test lines are also used for amsotropic structures
to average out the anisotropy
For a single-phase grain structure, a count can be made of either the number of grains inter-
cepted by the test lines, N, or the n u m b e r of grain boundary intersections with the test lines,
P Both approaches produce equivalent results With straight test lines, it may be easier to
make N c o u n t s where the grains partly intercepted by the ends of the hnes (unless the end lies
exactly on a grain boundary, which happens seldomly) are counted as half values. For circular
test grids, there are no line ends to deal with and either P or N counts can be made. Many
raters prefer to make P counts (grain boundary intersections) The number of N o r P c o u n t s
is divided by the true test line length (mm at • l) to obtain NL or PL. The true test line length
is found by dividing the total test line length by the magnification For a single-phase grain
structure, Sv is twice PL or NL
The mean lineal (or linear) intercept length, L3, is the reciprocal of NL or PL (for a single-
phase grain structure) For a deformed grain structure, NL or PL will be higher using test lines
perpendicular to the deformation axis than for test lines parallel to the deformation axis
Because L3 is the reciprocal Of NL or PL, the intercept lengths are inversely proportional Thus,
if straight test lines are placed parallel (ll) and perpendicular ( • to the deformation axis, an
amsotropy index, AI, can be defined as
AI = NL• = L3111L3• (6)
To obtain the gram size of a deformed grain structure, we can average the above L3Hand L3•
values, use randomly placed straight test lines, or use circular test lines
The determination of the ASTM grain size number, G, from mean lineal intercept values
has been a weak part of this method. The first published relationship between L3 and G was in
ASTM Method for Estimating the Average Femte Gram Size of Low-Carbon Steels (E 89),
Introduced in 1950 but discontinued in 1961 after ASTM E 112 was adopted. This standard
suggested making intercept counts on two sets of mutually perpendicular test lines to obtain
NL• and NLt, at magnification M The following equation was used to calculate the number of
grains per square inch at • 100, n
n = 0 8(M/IOO)Z(NL• (7)
This equation was in ASTM E 112 when it was proposed Later, it was changed to a relation-
ship between L3 of a orcular gram and its area, A
L3 = (TrA/4) '/2 (8)
As grains are not circular in cross secnon, this value of L3 is underestimated and an a d d m o n
of 0 52% is made For any value of NA (or A), one can calculate L3 using Eq 8 and then Increase
it by 0 52% to develop the needed relationship between G and the measured L3 The differ-
ences in L3, calculated by these two methods, are very small From L3 in mllhmetres, the
ASTM grain size number, G, can be calculated from
G = ( - 6 6439 log Ls) - 3 288 (9)
Example of These Methods

Pieces of an experimental hot-work tool steel were heat treated using three different austen-
ltlzmg temperatures 1052, 1066, and 1080~ (1925, 1950, and 1975~ After soaking, they
were quenched to 704~ (1300~ and held long enough to permit a minor amount of precip-
itation at the pnor-austenIte gram boundaries, then air cooled to ambient Etching with Vilel-
la's reagent fully revealed the grain structure
Photographs were made oftypmal regions m each specimen (areas chosen bhndly) and 203
by 254 m m (8 by 10 in ) enlargements were made. One print for each austenInzIng treatment
was chosen for comparative measurements
First, the planimetnc method was employed ASTM grain sizes were 9 9, 9 5, and 8 7 for
the samples austemtlzed at 1052, 1066, and 1080~ (1925, 1950, and 1975~ respectively
Next, the three-circle test grid was used to measure the same photographs The ASTM gram
size numbers were 10, 9 5, and 8 9, respectively Finally, a digitizing tablet was used to measure
intercept lengths directly through use of a template with straight test lines applied randomly
over the grain structure The A S T M grain size numbers were 9 9, 9 6, and 8 7, respectively,
for the three specimens The data are given m Table 1
In the Heyn method, or the Abrams three-circle intercept method, actual intercept lengths
are not measured For each test grid placement, an average intercept length is determined
based upon Nintercepts or Plntersectlons These L3 averages for each placement (or field) are
then averaged and a standard deviaUon can be computed Using the average and standard
devmtlon, the 95% confidence interval and the percent relanve accuracy may be calculated
The Abrams three-circle intercept method recommends that the magnification be chosen so
that a relatwely high number of P or N counts per field is made, ideally 100, and five fields are
measured for a total of(Ideally) 500 counts I r a large number of fields were to be measured,
the distribution of the N or P counts would be observed to be Gaussian Thus, calculation of
the arithmetic standard deviation 1s valid and precision can be assessed F o r most speomens,
measurements on five fields gives acceptable precision and is highly efficient The magnitude
of the standard devianon gives some insight into the uniformity of the grain structure
However, to properly assess the uniformity of a gram size distribution, individual gram mea-
surements must be made Individual measurements of Intercept lengths of test hnes through
grains or individual grain areas may be measured With strictly manual techniques, individual
intercept lengths are easier to measure than grain areas Templates illustrating a graded series
of circles of varying diameter could be employed to classify individual grains, but precise area
measurements cannot be made in this way
Semlautomahc digitizing tablets can be utilized along with a template to measure mdlwdual
intercept lengths, and grains can be traced to measure grain areas, although this is tedious and
VANDER VOORT ON GRAINSIZE 271
TABLE 1- - G r a m stze measurements o f hot-work tool steel spectmens
JEFFRIES PLANIMETRIC METHOD

Specimen Number Average, Average, Jeffnes, NA, ASTM
Code of Fields nl n2 f mm -2 G
1925~ 4 40 75 30 25 134 95 7540 1 99

1950"F 4 29 75 25 75 133 24 5679 1 95
1975~ 3 25 67 23 33 85 26 3183 2 87
ABRAMSTHREE-CIRCLEINTERCEPTMETHOD
Specimen Code Number of Fields Lr, ~ mm NL, mm-~ L3, tim ASTM G
1925"F 8 4 92 100 2 10 0 10 0
1950~ 10 6 19 83 0 12 1 95
1975~ 12 7 41 67 8 14 8 89
INDIVIDUALINTERCEPTLENGTHMEASUREMENTSb
Specimen Code Number of Intercepts L3, ~m ASTM G
1925"F 500 10 5 99
1950~ 432 11 6 96
1975~ 379 15 6 87
a L r 1Sthe total test hne length
b Straight test hnes used
requires a steady hand Automatic image analyzers could also be employed to make either type
measurement, so long as the grain structure can be properly delineated Once grain areas have
been measured, it is possible to compute the Jeffnes diameter, d, or the equivalent circle diam-
eter, ECD Furthermore, when the grains are detected, other statistical diameters may be mea-
sured, for example, a m a x i m u m caliper diameter (maximum Feret's diameter)
After a suitable number of measurements have been made, the data can be grouped into
classes usmg linear, logarithmic, or exponential class interval widths The amount in each class
can be computed as a simple numerical percent or as a weighted average, by length fraction
for intercept lengths or diameters, or by area fraction for grain area measurements
The digitizing tablet intercept length data for the three hot-work tool steel specimens were
grouped into 13 linear classes of equal width and eleven classes of uniform logarithmic spac-
Ing, producmg arithmetic and logarithmic intercept length groupings The frequency per class
was expressed as a simple number fraction or as a linear fraction, both as percentages The
percentage by length (sum of intercept lengths per class divided by the total intercept length,
times 100) puts greater emphasis on the data in the larger class intervals Figures 1 and 2 pre-
sent these data with the n u m b e r frequency at the top and the lineal fraction at the bottom
The hnearly scaled h~stograms, F~g 1, clearly demonstrate that the data are not Gausslan in
nature The lineal fraction percent, bottom of Fig 1, better reveals the emerging duplexity of
the grain size distribution than the n u m b e r fraction percent It is also apparent that the width
of the distribution increases with gram growth This has been observed in numerous prior stud-
ies of grain growth In contrast, the logarithmic histograms reveal slightly skewed, nearly uni-
formly shaped curves lndlcatmg a lognormal distribution of the data Many studies of such
data have also concluded that grain size distributions are essentially lognormal, although some
researchers have suggested that certain other more esoteric dlstnbutions may exhibit some-
what better fits to the data. In any case, grain size distribution data are not normal (Gausslan)
Hence, it is really not correct to compute an arithmetic standard deviation for lndwldual grain
size distributions, although this is done regularly due to the simplicity of such calculations
Percent
....... 9 ................................................................................. ........
0 20 40 60 80
Intercept Length,/z rn
0 1925F ~ 1950F o 1975F
Lineal Fraction, %
4~1 ~ 1925F L. 9 10.5 #m
3020I................................
.............................................................................................
~ .........................................................................................................................................................................................................................
~ ~ 1950F L = 11"6 ~l'm
1 0 ~ 0 .......................................
0 20 40 60 80
Intercept Length,/zm
0 1925F ~ 1950F o 1975F
FIG. 1--Intercept length distributions by number percent (top) and by linear fraction percent (bottom)
using linear size classes for heat-treated specimens of an experimental hot-work tool steel.
Intercept Counting Problems

A recent paper by Willis and Lake [10] discussed the measurement of grain size using cir-
cular test grids. When a circular test grid is employed, the number of grain boundary intersec-
tions (or grain intercepts) is divided by the circle circumference(s) to obtain P, (or Nt) and the
reciprocal of PL (or NL) gives the average intercept length, L3, which is an arc distance. On the
other hand, a digitizing tablet could be used with circular test patterns and the chord distance
VANDERVOORTONGRAINSIZE 273
Percent
30
1925F [. 9 10.5 /~m
25- 1950F L" 11.6 /~m ~ i i
20 .......................................................................................................................................................................................................
5 . . . . . . . . . . . . . "........
0
0.5 5 50
Intercept Length, Nm
l o 1925F " 1950F ~ 1975F ~
Lineal Fraction, %
4O
1925F [. 9 10.5 /~m ~
30 .................................................................................................................................................................... .................. o ................................................................
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ............................................
1975F L 91 5 ~
10 .........................................................
0 ~r A~ L .L 9 I I I I I I I I I I I III"1"
0.6 5 60
Intercept Length,~ m
0
1925F 9 1950F o 1975F
FIG. 2--1ntercept length distributions by number percent (top) and by linear fraction percent (bottom)
using logarithmically scaled size classesfi)r heat-treated specimens o[an experimental hot- work tool steel.
between successive grain boundary intersections could be measured and averaged to obtain
L~. Alternatively, one can trace the circle circumference and measure the distance between
successive grain boundary intersections and the mean of these arc distances would be L3. Are
these two measurements equivalent, or is there a bias? Willis and Lake stated that for any
curved test line, the probability of intersecting grain boundaries depends on the test line length
but not on its curvature. They stated that the use of arcs rather than chords increases the overall
test line length and the probability for intersecting grain boundaries They further concluded
that the test line length is arbitrary.
Willis and Lake [10] presented data to show that determination of L3 by Intersection counts
is not influenced by curvature, that is, test circle diameter An annealed low-carbon steel spec-
imen with a mean lineal intercept length of about 7 8 um (ASTM l0 7) was measured using
circles with true diameters, D, from 5 16 to 67 6 u m (D/L3 ratios from 0 66 to 8 7 l) and from
1274 to 482 intersection counts (fewer counts were made as the circle diameter increased)
Intersection counts were also made using straight test lines They concluded that multiple
application of small circles gives equivalent results to a reduced number of applications of a
larger circle if the number of intersection counts are similar Application of their two smallest
diameter circles did produce some placements without any Intersections Because the diame-
ters of these circles were less than L3, this is to be expected
While Willis and Lake concluded that intersection counts using circles of varying diameter
(that is, curvature) were not biased by the curvature, they stated that the measurement of indi-
vidual chord lengths, rather than arc lengths, using circular test grids did produce bias They
stated that such chord measurements did underestimate L3 and experimental data were shown
to substantiate these claims
Willis and Lake [10] stated that their observations were contrary to statements in ASTM E
112 where it is claimed that chord measurements of grain size using circular test lines are valid
Willis and Lake stated that arc lengths should be used, not chord lengths Further, they stated
that if L3 was the only desired measurement, measurements of Individual arc distances were
not required because the total arc distance (the circumference) would be known and the num-
ber of intersections could be counted easily.
Willis and Lake concluded that the use of test circles to obtain L3 through intersection
counts produced valid results even if circles with diameters less than L3 were used They rec-
ommended use of test circles that produce about ten intersections per application They also
concluded that the use of individual chord distances, measured and averaged to obtain L3, was
incorrect and produced a 5% underestimation of L3 for a test circle having an average of ten
intersections (For their data, this would be a 25 #m diameter test circle, that is, a circle with
a diameter about three times larger than the mean lineal intercept length.) They concluded
that the distribution of arc intercept distances using circular test lines was not the same as
obtained with strmght test lines and that the distribution of chord lengths produced even
greater disagreement
First, It must be stated clearly that nowhere in ASTM E 112 are either arc or chord intercept
length measurements recommended ASTM E 112 deals only with counts of grains per unit
area, grain intercepts, or grain boundary intersections, that is, the Jeffnes planimetrlc method
and the Heyn (Abrams) intercept methods ASTM E 112 is a totally manual method It does
not describe any automated method for grain size measurement Furthermore, it does not
describe gram size distribution measurement methods. There is no known simple manual
method for measuring arc lengths on a circle and none are described in ASTM E 112 Hence,
ASTM E 112 does not recommend either individual chord or arc measurements on circular
grids
When the Abrams three-circle intercept method was added to ASTM E l 12 in its 1974 revi-
sion, one of the Committee E4 members claimed that the use of a circular test grid biased the
intercept measurement This claim was on a theoretical basis and was not tested by experi-
ments Originally, this information was in Paragraphs 11 2 and 11 3 3 and Tables 6 and 7, but
since the 1982 revision, it has been in Paragraphs 12 2 and 12 3.3 and Tables 6 and 7. Para-
graph 12 2 states that this bias decreases as the n u m b e r of grain interceptions increases, being
negligible when N (or P) IS greater than 18 Also, it should be noted that Hllhard [8] has rec-
ommended that the test circle size be 100 or 200 m m and that the magnification be adjusted
so that N or P exceeds six per placement
In their experiment, Willis and Lake [10] first made intersection measurements using
orthogonal straight lines (test line length, magnification, and number of placements not
stated) A total of 606 intersections were counted yielding an average Intercept length of 7 76
/~m By back calculation, the total test line length would have been 4 7 m m Next, intersection
counts were made using six circles with true diameters (template circle diameters not given)
from 5 16 to 67 6 ~zm Two of the circles had diameters less than the mean intercept length
Rather than making a constant number of counts with each circle, which would have been a
better comparison, they increased the number of intersection counts as the circle diameter
decreased. Not surprisingly, the reported 95% confidence limits improved (becomes smaller)
as the number of counts increased The number of grid placements were not given but can be
calculated Table 2 presents their reported results for the circular test patterns (except for the
range of intersection data) The bottom of Table 2 shows the calculated number of circle place-
ments, the total circumference line length, PL, and the number of placements required to
obtain about 500 intersection (P) counts for each circle.
Note that for the largest circle, P was 482 and this was obtained with 18 placements or
"fields" and the total test line length was 4 7 mm. For the smallest circle, P was 1274 (264%
greater), requiring 625 placements and a test line length of l0 l mm, see Fig 3 It should be
immediately obvious to any practicing metallographer that far more effort was required for
the measurements with the smallest circle For each placement, the stage must be moved, the
microscope refocused, the count made and recorded. Even lfa constant P count was made for
all of the test circles, 245 (rather than 625) fields must be rated with the smallest circle Also,
if the P d a t a are to be evaluated m a manual method, each value must be entered into a hand
calculator or PC that obviously takes much more time for 625 (or 245) versus 18 (or 19) values
The Wilhs and Lake mean lineal intercept values show good agreement over the range of
test circles that experimentally suggests there is no bias between use of straight test lines and
curved (circular) test lines for the case of intersection counts However, these authors state that
for individual intercept length measurements, there is a bias between arc and chord measure-
ments Also, even if very small test circles can be used to obtain precise average PL and L3
values, the effort required is far greater than for larger test circles with higher counts per circle
TABLE 2--Data of Wdhs and Lake [ 10]
Circle Diameter, Number of Average Number of L3, 950/0

um Intersections Intersections um CL
67 6 482 26 8 7 90 0 46
306 554 12 3 7 81 043
19 0 707 7 86 7 59 0 38
13 4 822 5 41 7 78 0 35
6 66 854 2 74 7 64 0 35
5 16 1274 2 04 7 94 0 28
INFORMATION CALCULATEDFROM THEIR DATA
For Constant Counts
Circle Diameter, Number Total Length, PL,
~m of Fields~ mm mm-J EP, Number of Fieldsa
67 6 18 4 703 128 9 509 19

30 6 45 3 823 126 1 504 41
19 0 90 5 372 131 6 503 64
13 4 152 6 399 128 5 498 92
6 66 312 6 528 130 8 501 183
5 16 625 10 132 125 8 500 245
Number of times the test circles are apphed
NO. of I n t e r s e c t i o n s
1400
Smallest Circle ----~~
1200
1000
800
600 i_ o
^ ^ ^ _~ ~ Constant Counts
400
Largest Circle
200 I ..... I t I t
0 100 200 300 400 500 600 700
N u m b e r of Fields M e a s u r e d
FIG 3--Plot showing the increased number ofP tntersecttons as a funcHon of the number of measure-
ment fields for ctrcular test hnes used by Wtlhs and Lake [ 10] versus condtttons for constant intersection
counts
Additionally, with the use of small test circles, the test data will not be Gausslan and the usual
arithmetic statistical approaches are not valid
Circular Intercept Experiment

Because the Willis and Lake experiment did not use a constant count approach and the data
d~stnbutlon was not reported; and, because the arc versus chord individual intercept length
measurements were reported to be biased, but not the circular versus straight line intersection
count data, the writer deoded to repeat their experiment. A specimen of AISI 304 stainless
steel with an apparent ASTM austenltiC grain size of about 5 was selected for the measure-
ments. The specimen was etched electrolytlcally using 60% aqueous nitric acid that fully
reveals the grain boundaries but not the twin boundaries, Fig 4 The 101 6 by 127 m m (4 by
5 in.) negative was enlarged and 203 by 254 m m (8 by 10 in.) prints were made at a magnifi-
cation of • 207.3
First, the ASTM three-circle method was employed to measure the mean lineal intercept
The grid was dropped onto the p n n t thirteen times until about 500 intersection counts were
obtained The results are gwen here (triple points mtersect)ons were counted as 1~, tangent
hits as ~)
A S T M Three-Circle Intercept Method

Number of fields = 13
N u m b e r of intersections (P) -- 527
Total test line length = 31 356 m m (6500 m m on the photographs)
PL = 16.807 per m m
L3 = 595 + 4 6 t ~ m
ASTM grain size, G = 4 85
FIG. 4--Grain structure of AIS1304 stainless steel specirnen revealed by electrolytic etching with aque-
ous 60o6 IIN03 (6 V dc, 2 rain, Pt cathode, 20*6"). Note that the grain structure appears to be slightly duplex.
Next, a series of parallel diagonal lines were drawn across the photographs, with both diag-
onal orientations (45* to longitudinal direction), and the lines spaced about 10 mm apart. Indi-
vidual intercept lengths were measured with the following results.
Individual Intercept Measurements (Diagonal Lines)

Number of intercepts = 463
Total line length = 28.041 m m (5812.7 m m on photographs)
L3 -- 60.4 _+ 3.7 um
ASTM grain size, G = 4.80
The distribution of these intercept lengths was examined, Fig. 5, but was not quite Gaussian.
It was right skewed (/3~ = 1.51) and the kurtosis (/32) was 5.178, a bit more peaked than for a
normal distribution. The logarithmic distribution appears to be a bit more symmetrical.
Next, a set of 150-ram-long straight, parallel test lines were applied using parallel and per-
pendicular orientation. Forty-five placements in each orientation were made to obtain about
500 intercepts (N) per orientation with the following results.
Straight Lines--Parallel to 2 5 4 - m m (lO-in.) Side

Number of lines = 45
Number of intercepts, N -- 505 (466 + 78/2)
Total line length = 32.562 m m (6750 m m on photograph)
NL = 15.509 per m m
L 3 - - 6 4 . 5 + 3.1urn
ASTM grain size, G = 4.61
Percent
3~ by Number
~o4 .....................
:/ ................ ..............................................................................................
,~ 7 ............... .........\.. \ ....................................... ..............................
,://t 0 50 100
Intercept
150
Length,/J,m
200 250 300
Percent
50
N = 463 ,,
40
i
L3= 60.4/xm
30
20
10
0
0.1 1 10 100 1000
Intercept Length,/xm
FIG. 5--1ntercept length distributions for manually obtained intercepts using straight test lines placed
on a 203 by 254 mm (8 by 10 in.) photograph of AISl 304 showing number and length percentages and
linear and logarithmic scaling of the size classes.
Straight Lines--Parallel to 203-mm (8-in.) Side

N u m b e r o f lines = 45
N u m b e r o f intercepts, N = 529 (487 + 84/2)
T o t a l line length = 32.562 m m (6750 m m o n p h o t o g r a p h )
Nz = 16.246 p e r m m
L3= 616_+27#m
A S T M grain size, G = 4 75
The preceding data were c o m b i n e d yielding the following results
All Orthogonal Lines

Number ofhnes = 90
N u m b e r of intercepts, N = 1034
Total line length = 65 124 m m (13 500 m m on photograph)
NL = 15 877 per m m
L3 = 63 _+ 2.1 ~zm
A S T M gram size, G = 4 68
T h e a g r e e m e n t between the three methods is not bad, although the intercept counts on the
straight orthogonal lines p r o d u c e d a slightly coarser gram size measurement, perhaps due to
the p r o b l e m of deahng with lines that end within grains
Next, interception counts were m a d e using eleven test circles o f varying diameter, from 8
to 180 m m , that is, from true diameters from 38 6 to 868 ~ m The 8 - m m orcle, hence, had a
true & a m e t e r less than the m e a n lineal intercept length However, the next smallest circle, 16-
m m diameter, had a true d i a m e t e r of 77 2 u m which is larger than L3 but not larger than the
largest grains present Thus, s o m e placements should, and did, gwe no intersections. These
test patterns were dropped onto the photographs and grain b o u n d a r y intersections were
counted and recorded This process was repeated until about 500 intersections were obtained
with each test circle T e m p l a t e selection was done in r a n d o m order and none of the data were
analyzed until all o f the counting was completed. Table 3 presents the data from this part o f
the experiment
N o t e that the n u m b e r o f placements, or"fields," for about 500 P counts decreased from 242
for the 8 - r a m - d i a m e t e r circle to 12 for the 1 8 0 - m m - & a m e t e r circle Actually, w~th the two
largest circles, the photograph could not be fully sampled due to the large circle size and the
need to keep all o f the circle on the photographs N o t e that there is some v a n a t l o n in L3 and
G, but It is m i n o r The 8 - m m test circle p r o d u c e d a slightly lower estimate of L3, but the spread
TABLE 3--Intersectton counts usmg test ctrcles of varying diameter, AISI 304 stainless steel
Circle True 95% Relatwe ASTM

Diameter, Diameter, Number Number PL, S, CL, Accuracy, L3, Grain
mm ~m of Fields of H~ts mm-~ mm-~ mm-J % ~m S~ze,G
8 38 6 242 501 17 075 12 304 1 582 9 27 58 56 4 89

16 77 2 131 503 15 835 6 954 1 215 7 67 63 15 4 67
24 115 8 87 513 5 16 227 4 866 1 043 6 43 61 62 4 75
39 7 191 5 54 509.5 15 682 3 731 1035 6 60 63 77 4 64
50 241 2 41 504 16 222 3 185 1 015 6 26 61 64 4 74
79 381 1 26 499 5 16 046 2 776 1 119 6 98 62 32 4 71
99 477 6 21 508 16 123 2 541 1 157 7 17 62 02 4 73
119 5 576 5 17 506 16 435 2 013 1 044 6 35 60 85 4 78
140 675 4 15 521 16 37 1 711 0 947 5 79 61 09 4 77
160 771 8 13 494 15 671 1 301 0 787 5 02 63 81 4 64
180 868 3 12 512 15 64 1 727 1 097 7 02 63 94 4 64
m G values is only 0 3 A S T M units, which is quite acceptable Fxgure 6 shows how PL and L3
vaned with test circle diameter The _4-2s hnes were calculated based on all of the data except
for the 8-mm-dmmeter c~rcle
Table 3 also hsts the computed standard devlatmns (s), the 95% confidence hmlts (95% CL),
and the percent relative accuracy (% RA) Note that the standard devlaUon decreased (Fig 7)
w~th increasing circle dmmeter and fewer fields but approximately equal counts Note also that
the standard devlatmn rises rapidly for test circles < 40 m m in dmmeter (193 um or about three
Mean NO. I n t e r s e c t , o n e / m m
19
18
17 §
O 0 b 0
16 Mean
o o o
15- -2s
14-
13 I I I I I I I P I
0 20 40 60 80 100 120 140 160 180 200
Test Circle Diameter, mm
Mean Intercept Length,~,m

70
65 +2s
+ + +
+
+ Mean
+ +
+ +
60 -2s
+
55 I I I I I I I [ I
0 20 40 60 80 100 120 140 160 180 200
FIG 6--Plots showing the vartatton m measured PL (top) and L3 (bottom)for the AISI 304 specimen
when measured wtth circles of varying dtameter The +s, - s , and mean values were calculatedfrom all
of the data except for that from the 8-ram-diameter circle
VANDER VOORI- ON GRAINSIZE 281
s(P/L) or % RA
14
12
10
A
% Relative Accuracy
8
0
0 50 100 150 200
FIG. 7--Plot showing the variation of the standard deviation and the ~ OfPL measurements made
using 8- to 180-mm-diameter test circles and the A1S1304 specimen.
times the mean lineal intercept length). The 95% confidence limits are calculated from the
standard deviation, the appropriate Student-t value and the number of fields. Then, the 95%
CL is divided by the mean value of PL and expressed as a percentage to determine the % RA.
Note that these values, except for the 8-mm-diameter test circle, are nearly constant with a
very slight decrease as the test circle increased. This, of course, disagrees with the confidence
limits published by Willis and Lake where the 95% CL decreased considerably with decreasing
test circle diameter (however, they increased the counting effort as the test circle diameters
decreased).
For these circle placements, 62 of the 242 (25.6%) fields yielded no intersections for the 8-
mm-diameter test circle, while 8 of the 131 (6.1%) placements yielded no intersections for the
16-mm-diameter test circle. Consequently, the statistical analysis could only be performed on
the PL values per placement, not on the L3 values (L3 = 1/0 yields infinity for PL = 0).
Figures 8 and 9 show the distribution of the P counts per circle placement for the 8-, 16-,
and 24-mm circles and for the 24-, 40-, and 50-mm diameter circles. In Fig. 8, the number of
0 intersection hits (P = 0) is plotted at 0 on the x-axis. The x-axis is in whole integer units
from 0 to 13. Due to tangent and triple-point hits, some Pvalues were in half rather than whole
values. Therefore, at 1 on the x-axis is plotted the total percentage of P placements with 0.5
and 1.0 hits. Likewise, at 2 on the x-axis, the percentage of 1.5 and 2.0 P hit placements is
plotted. This procedure was followed for all three distributions on Fig. 8. For the 24-, 40-, and
50-mm test circles, no placements resulted in zero hits and the range of hits per placement was
greater. Hence, I grouped the hits in units of two. For example, at 1 on the x-axis, all of the
hits from 0 to 2 were plotted as a percentage. At 3 on the x-axis, all of the hits greater than 2
(2.5) to 4 were plotted as a percentage, and so forth.
Figure 8 clearly shows a non-Gaussian distribution for the 8- and 16-mm test data due to
the abnormally high P = 0 counts at the left-side tail of each distribution. Note that in each
case, the percentage of zero hits is greater than the percentage of 0.5 and 1 hits. For the 24-
mm-diameter test circle, the distribution appears to be approximately normal. In Fig. 9, all
FIG. 8--Graph showing the distribution of P intersection counts for the 8-, 16-, and 24-mm-diameter
test circles applied to the AIS1304 grain structure.
three distributions appear to be approximately normal. There were not enough placements for
the circles of diameters greater than 50 m m to properly evaluate their data distributions, so
these have not been plotted. However, their distributions certainly will be normal.
Next, using the larger test circles, Jeffries planimetric and triple-point count measurements
were made to determine the number of grains per m m 2 at • l, NA. The total number of grains
FIG. 9--Graph showing the distribution of P intersection counts for the 24-, 40-, and 50-mm diameter
test circles applied to the AISI 304 grain structure.
VANDER VOORTON GRAIN SIZE 283
No/mm 2
260
250 G = 5.0
240
Plammetric
230
220 o
~ /x /x 0
210
~ = = ~ Triple-Point Counts
200
190
180
G - 4.5
I I I I I I I I I I 1 I
170
70 80 90 100 110 120 130 140 150 160 170 180 190 200
Circle D i a m e t e r , mm
FIG 10--Graph showmg the vartatton m NA values obtained by use o f the Jeffrles plammetrtc method
and the trlple-pomt count method usmg test ctrcles o f varymg dtameter apphed to the A I S I 304 gratn
structure
or triple points counted were not held as constant as desired For the 180-mm-dlameter circle,
only one placement was used because of the limited ability to shift such a large circle over the
photograph and sample different grains Except for the 180-mm-dlameter circle, the number
of grain counts (nj + n2/2) vaned from 163 to 236, while the number to triple points counted
varied from 300 to 435 Tables 4 and 5 present the test data and results Figure l0 shows the
N~ data generated by both methods Although the computed ASTM grain size numbers vary
by only 0 2 G units, which is excellent, we note a consistent trend that NA from the triple-point
count method was slightly lower than from the planimetrlc method
Next, a digitizing tablet was used to trace 180 grains and measurements were made of the
areas and m a x i m u m diameter of each grain. For the grain areas, the mean area, A, was 4091 8
tzm2, the standard deviation was 4892 13 ~m 2, and the grain areas ranged from 46 7 to 34800
/~m2 Figures 11 and 12 show the distribution of the grain areas plotted as both number per-
centages and area fraction percentages (by class) using linear (Fig 11) and logarithmic (Fig
12) scaling of the class sizes Note the very high skew (rio and kurtosis (f12) values using the
TABLE 4--Plammetrle gram stze analysts, A I S I 304 stainless steel spectmen
Circle Diameter, Jeffnes Factor, Number n~/(n~ + n2), NA, ASTM

mm f of Fields En~ En2 % rnm-2 G
79 0 8 767 8 132 156 45 8 230 1 49

99 0 5 582 6 166 140 54 3 219 6 48
1195 3831 4 169 115 595 2170 48
140 0 2 792 2 132 62 68 0 227 5 49
1600 2 137 2 174 75 699 2260 49
180 0 1 689 1 106 43 71 1 215 3 48
284 M E T A L L O G R A P H Y : PAST, PRESENT, A N D FUTURE
T A B L E 5--Triple-point count method, AISI 304 stainless steel specimen.
Circle Diameter, Number Average Number of Circle Area, N~, ASTM

mm of Fields Triple Points mm 2 mm -2 G
79.0 8 49.25 0.1141 224.6 4.9

99.0 6 72.17 0.1791 207.0 4.7
119.5 4 108.75 0.2610 212.2 4.8
140.0 2 150.0 0.3582 212.2 4.8
160.0 2 196.5 0.4679 212.1 4.8
180.0 1 248.0 0.5922 211.1 4.8
Percent
6O
o N- 180 ,t31- 9.83
50 ...........................................................................................................................................................................................................................
9~ 9 4 0 9 1 . 8 ~ m 2 /~2 9 17.63
40 ...........................................................................................................................................................................................................................
3 0 ...........................................................................................................................................................................................................................
OlOo
0 10 20 30 40
Grain Area, sq.~,m (Thousands)
A r e a Fraction, %
35
sol . . . . . . . . . . . . . . . . . .o. . . . . . . . . .N.,lS0_

. . . . . . . . . . . . . . ...............................................
... ..............................
2s ..................... A 9 4091.8 ~m 2 ~2 9 17.63
2105....of...~.........f.......................................................................
10 ......................................................................................
O ................................................................................................................ o ....
5 ............................. ~ ....................
Q......................................................................................................
~ ....................
o
0 10
,
20 30
\ 40
Grain Area, sq.~rn (Thousands)
Copyright
FIG. 1by ASTM Int'l (all rights
l--Distribution reserved);
of grain Thuthe
areas for DecAIS1304
29 00:42:12 EST 2011
stainless steel specimen shown with linear class
size intervals and by
Downloaded/printed with number percent (top) and area fraction percent (bottom) freauencies.
V A N D E R V O O R T ON GRAIN SIZE 285
Percent
III,'18Q ................................o............................ ........................................... ..........................
~, 9 4 0 9 1 . 8 / J , m 2
30-
20-
10-
0 9../i I I IIIlll I I I Iiiiii i i II
10 100 1000 10000 100000 100000

Grain Area, sq./j,m
Area Fraction, %
60
N-180 /~1 9 - 0 . 3 8
60- - o
9~ 9 4 0 9 1 . 8 p,m 2 /~2 = 2 . 7 6
4 0 .......................................................................................................................................................
30-
o
20-
10- ........................................................................................................................................ O ...................
0 c~ [ I I q I III i I I i i i iii i I i I I I f
lo lOO lOOO 10000 ~ooooo 100000

Grain Area, eq./j,m
FIG. 12--Distribution of grain areasfor the A/S/ 304 stainless steel specimen shown with logarithmic
class size intervals and with number percent (top) and areafraction percent (bottom)frequencies.
linear class intervals, Fig. 11. However, ifa logarithmic scale is employed, Fig. 12, and logs of
the grain areas are evaluated, the skew and kurtosis values fit a lognormal distribution.
From the grain area values, the Jeffries diameters were calculated and plotted in the same
way, Figs. 13 and 14. The linear distribution and data analysis indicate a slightly nonnormal
distribution, while the logarithmic plots and data analysis reveal a lognormal distribution. The
mean d value was 55 ;Lm, somewhat less than L3. The standard deviation was 32.68 gm.
Percent
40 /
/ N 9 180 /~1" 0.85
cl- .. /~2-4.^46
/
3 0 -t .................................................
~
~
...........................................................................................................................................................................................................................
,,.~ 55/J,m
20-
10-
0 I I I v I v
0 50 100 150 200 250

Jeffries Diameter, d,~m
Lineal Fraction, %
40
N 9 180 /31 = 0.85

o
30
20
10
0 so 100 150 200 250

Jeffriee Diameter, d,/j,m
FIG. 13--Distribution of the Jeffries diameters for the A / S / 304 stainless steel specimen shown with
linear class size intervals and with number percent (top) and area fraction percent (bottom)frequencies.
The maximum grain diameter values were also plotted as linear and logarithmic distribu-
tions, but only number percentage data are shown in Fig. 15. Note that the linear plot (bottom
of Fig. 15) reveals a somewhat nonnormal distribution, while the logarithmic plot and data
analysis again reveal conformance to a lognormal distribution. The mean maximum diameter
was 75.9 um, somewhat greater than L3 and d. The standard deviation was 41.55 #m.
VANDER V O O R T ON GRAIN SIZE 287
Percent
5O /
/ N 9 180 /31 9 - 0 ' 3 8

4 0 ~ .................................................................................................................................................................
(9.......................................................................................
I
~o-' ........... .........................................................................

- .................................. 2:r ~ ........
~,J I I I"-/i F I I I I I I I I I I i I i I I r,-*" I i i f i
10 100 1000
Jeffries Diameter, d,~m
Lineal Fraction, %
ZII ........ ............................................................................

o ....................
,o_ ~ . . . . . . . . . . . ..............................................................................~ - ...... 2:~6 ...........
3 0 .........................................................................................................................................................................................................
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .....
/ o\
'i- , ........................
:................. ...........................
1 10 100 1000
Jeffries Diameter, d,/cm
FIG. 14--Distribution of the Jeffries diameters for the A/S/ 304 stainless steel specimen shown with
logarithmic class size intervals and with number percent (top) and area fraction percent (bottom)
.frequencies.
Next, the digitizing tablet was used to measure intercept lengths with straight test lines, just
as was done previously by a manual approach. A total of 428 intercepts were measured and
the average was 60.9 um, nearly identical to the manual method. Linear and logarithmic num-
ber percent and lineal percent distributions are shown in Figs. 16 and 17. For the linear dis-
tribution of intercept lengths, the skew was 1.60 and the kurtosis was 5.41, nearly identical to
Percent
30
/31" - 0.38 o N = 180
25-
20
15
10
5
o . . . . . . . .
0 i |,
10 100 1000
D Max./J,m
Percent
25 ................................................
~ ..............................................................................
-- ........................................................................................
ax 75.9~, m
. . . . . . . . . . . .
ls~ ................................................. B1 = 0 . 7 4
,o~
0
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ...................................................... t
0 50 100 150 200 250 300
D Max,/J,m
FIG. 15--Numberpercentfrequency distributions of the maximum grain areasfor the AIS1304 stain-
less steel grain structure using logarithmic (top) and linear (bottom) scaling of the size classes.
the manually generated data. Note that the logarithmic plot reveals a more normal appearance
and the skew and kurtosis values of the logarithmic values indicate conformance to a lognor-
mal distribution.
The final experiment consisted of measuring individual chord and arc lengths between adja-
cent grain boundary intersections using test circles of varying diameter and a digitizing tablet.
Because it is far easier to measure chord than arc lengths, more chord length measurements
Percent
30
[
3 60.9//,m
2 0 | ~ .......I \ ............................................................................................ ....................
1
15
10
6 ...............
0
0 50 100 150 200 250 300
Intercept Length,/.Lm
Lineal Percent
26 ........................................................................................................................................
L a eo.9 ~m
ili .....l..........\.................................................
. ,.60 .....k
,o
6 . . . . 1
0
o 50 loo 1so 200 250 aoo
Intercept Length,/j,m
FIG. 16--Distribution of intercept length measurements made with a digitizing tablet and straight test
lines with the AIS1304 grain structure plotted using linear size classes and number percent (top) and lineal
percent (bottom)frequencies.
were made. The writer made chord length measurements with each of the test circles and arc
length measurements with the 16- and 79-mm-diameter circles. Then, two different metal-
lurgy students at Lehigh University (Operators 2 and 3) measured both chords and arcs using
four of the test circles. The students were unaware of any of the other test data in this paper,
and they were not aware of each others results. Figure 18 shows all of the test data listed in
Percent
40
N 9 428
- b
L 3- 60.9 ~ m
30
20
10
0
0.1 1 10 100 1000
Intercept Length, ~ m
Lineal Percent
50
N 9 428
o
40 ...........................................................................................................................................................................................................................
L 3- 60.9/J,m
30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
20
10
o
I I III
0
0.1 1 10 100 1000
Intercept Length, ,u, m
FIG. 17--Distribution of intercept length measurements made with a digitizing tablet and straight test
lines with the AIS1304 grain structure plotted using logarithmic size classes and number percent (top) and
lineal percent (bottom)frequencies.
Table 6. Note that the chord measurement for the 16-mm-diameter circle produced a very low
L3 value, and one chord measurement with the 160-mm-diameter test circle had a slightly high
L3 value. The other two sets of chord and arc measurements with the 160-mm-diameter test
circle were in good agreement. The writer and one student (Operator 2) consistently had higher
L.~ values for the arc measurements, while the second student (Operator 3) had the opposite
Mean I n t e r c e p t Length,j[l,m
80
z <> Arcs
+ oA Chords
7O
s
z o
60
9 o o
50
o
40 i t J i i ~ J J i
0 20 40 60 80 100 120 140 160 180 200

FIG. 18--Mean lineal intercept measurements u ~'ing chord or arc lengths on circles ~[varying diameter
fi~r the ,4 IS1304 grain structure. A digitizing tablet was used to m a k e the measurements by three different
operators.
trend for all four measurements. Operator 2 made more measurements per test circle than
Operator 3, and this may be a factor. At any rate, except for the 16-mm test circle, the results
are reasonably similar, at least for test circles > 4 0 mm in diameter (true diameter about three
times L3). Arc data is extremely difficult to generate compared to chord data. With larger test
circles, and more grain boundary intersections, the difference between arc and chord lengths
decreases.
Figure 19 illustrates the distribution curves, using only a linear size class scale and the num-
ber percent, for simultaneously measured arc and chord lengths with the 79-ram-diameter test
circle. The two curves are shown independently as they overlap nearly perfectly. This illus-
trates the very close agreement that can be obtained using arc and chord measurements with
a test circle much greater in diameter than L3 ( D / L s is slightly greater than 6).
In plotting distribution curves, one must decide how many size classes to use. Too few size
classes produce a loss of sensitivity, especially if duplexity is of interest. A high number of
size classes can only be used if the number of measurements is very high. Otherwise, away from
the mode region, the percentages per class will be rather erratic. In general, from 8 to 15 classes
should be used (Fig. 20). If the number of measurements is somewhat low, use 8 to 10 classes.
If N is very high (for example, above 1000), a higher number of classes may be used suc-
cessfully.
Conclusions
Analysis of the same images revealed excellent correlation among ASTM grain size num[bers
produced by the Jeffries planimetric method, the triple-point count method, the Heyn or
Abrams intercept methods, or by individual intercept length measurements using either
straight or circular test lines. In general, NA values by the triple-point count method were con-
TABLE 6--1ntercept lengths usmg arcs and chords wzth test ctrcles of varying dtameter
Circle Diameter, True Dmmeter, Number of Average Chord ASTM

mm ~m Chords Length, #m s, um G
16 78 3 90 43 0 19 4 5 81
24 117 5 80 57 0 29 3 50
32 156 6 79 60 6 30 1 48
40 195 8 130 57 5 35 4 49
50 244 7 119 64 4 36 9 46
79 386 7 157 61 6 37 7 48
79 386 7 151 58 1 37 6 49
99 484 6 157 61 6 38 5 48
119 5 582 5 158 64 5 38 3 46
140 680 4 159 60 0 38 3 48
160 783 2 97 70 4 39 2 44
180 881 1 199 63 7 40 0 47
50 244 7 300 63 0 36 3 4 72
119 5 582 5 300 62 1 40 97 47
140 680 4 300 59 6 35 25 48
160 783 2 300 64 8 39 00 46
50 244 7 565 64 4 41 86 4 63
119 5 582 5 45 63 2 43 12 47
140 680 4 64 63 6 34 00 47
160 783 2 114 63 2 37 73 47
C~rcle Dmmeter, True Dmmeter, Number of Average Arc ASTM

mm #m Arcs Length, #m s, ~m G
16 78 3 169 64 2 42 8 4 61
79 386.7 157 62 I 39 1 47
50 244 7 300 63 6 39 54 4 72
119 5 582 5 300 62 9 39 97 47
140 680 4 300 62 2 38 19 47
160 783 2 300 65 7 40 24 46
50 244 7 231 61 0 41 45 4 83
119 5 582 5 57 604 36 35 48
140 680 4 64 62 7 34 10 47
160 783 2 114 62 9 37 41 47
1.2.3Pertain to data developed by Operators 1, 2, and 3 (students were Operators 2 and 3)
slstently slightly smaller than by the Jeffnes method, although this difference was so small that
the A S T M G values were essentially unaffected.
Use o f test circles w~th true diameters less t h a n three times the m e a n hneal intercept length
is not r e c o m m e n d e d . With single test circles, the effort required to obtain the same degree of
precision increases dramatically as the circumference decreases. For efficient measurements,
the d i a m e t e r o f the circle (or circles) should be greater than six times L3 A total hne length of
500 m m , as r e c o m m e n d e d by A S T M (but with three concentric circles to m l m m l z e the size
o f the test pattern), p r o d u c e d about 500 intercepts or Intersections with only 13 placements
(for this grain size and photograph magnification, a lower magnification would have been pre-
ferred for best efficiency) T h e 160-mm-dlameter test circle also produced about 500 lntersec-
titans with 13 placements.
Test circles smaller than the largest grains should never be employed. First, they are highly
inefficient. Second, s o m e placements will produce no intersections For such work, if P = 0
and PL = 0, L3 = oo, which is absurd Hence, in such cases, P or PL data must be averaged
and the m e a n values used to calculate L3; the individual field data cannot be converted to L3
Percent
s~iT o N 9 157
.....~
40301L~ ...........'...............................................8.....Class
..... Intervals
O,o
ol I , I I -r--, I
0 50 100 150 200 250 300
Intercept Length,/l,m
Percent
sol '~ N = 157

40 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
.. 8 Class Intervals
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
O~ I ' ~ I I -'-'-~'--= ', o

0 50 100 1so 2o0 2so 3o0
Intercept Length,/J,m
FIG. 19--Distributions of arc (top) and chord (bottom) intercept lengths made simultaneously using
the digitizing tablet and the 79-ram-diameter test circle with the AISI 304 grain structure showing eight
linear size class intervals and number percentfrequencies.
values and then an average value calculated. Statistical analysis must be performed on the PL
data rather than L3 data.
ASTM E 112 is a totally manual method and only describes the Jeffries planimetric method
and several types of intercept count m e t h o d s - - b u t not individual arc or chord measurements
on test circles. There are statements in ASTM E 112 concerning bias introduced using small
diameter test circles. This information will be revised.
Percent
50 v
o
6
40 v
30
20 ~
10
v
No. o f C l a s s e s
0~. I ' ~ "' --

0 50 100 150 200 250 300
InterceptLength,~m
FIG. 20--Example of the use q/'dtf]erent numbers of linear size classes on the shape of the histogram
fi)r the chord lengths shown in Fig. 19.
Measurement of individual intercept lengths using a digitizing tablet is best performed using
straight test lines. Measurements with test circles, either chord or arc lengths, should not be
made using small diameter test circles. Such measurements are extremely tedious. All arc
length measurements are very tedious. Chord lengths using large diameter test circles (D/L~
> 6) appear to be relatively free ofbias. However, use of large circles provides little advantage
over straight lines except for the fact that anisotropy can be averaged out. With straight test
lines, they may be applied using several different orientations to even out structural anisot-
ropy; or, they can be applied parallel a n d perpendicular to the deformation axis to assess the
anisotropy with the data c o m b i n e d to obtain an average.
References
[ I ] Vander Voort, G. F., "'Grain Size Measurement," Practical Applications of Quantitative Metallog-
raphy, ASTM STP 839, J. L. McCall and J. H. Steele, Jr., Eds., American Society for Testing and
Materials, Philadelphia, 1984, pp. 85-131.
[2] Sauveur, A., Transactions, American Institute of Mining, Metallurgical, and Petroleum Engineers,
Vol. 22, 1894, pp. 546-557.
[3] Jeffries, Z.. Kline, A. H., and Zimmer, E. B., Transactions. American Institute of Mining, Metal-
lurgical, and Petroleum Engineers, Vol. 54, 1916, pp. 594-607.
[4] Jeffries, Z., Transactions. The Faraday Society, Vol. 12, 1916, pp. 40-56.
[5] Heyn, E., The Metallographist, Vol. 5, 1903, pp. 39-64.
[6] Gokhale, A. M., Transactions, Indian Institute for Metals, Vol. 35, 1982, pp. 595-600.
[ 7] Smith, C. S., "Grain Shapes and Other Metallurgical Applications of Topology,'" Metal Interfaces,
American Society for Metals, Cleveland, 1952, pp. 65-113.
[8] Hilliard, J., Metal Progress. Vol. 85, May 1964, pp. 99, 100, 102.
[9] Abrams, H., Metallography. Vol. 4, 1971, pp. 59-78.
[ 10] Willis, D. J. and Lake. J. S. H., Scripta Metallurgica, Vol. 21, No. 2, 1987, pp. 1733-1736.
Wdliam D r u r y 1 and Arun M. Gokhale 1
Measurement and Interpretation of Fracture

Surface Fractal Dimension
REFERENCE: Drury, W and Gokhale, A M , "Measurement and Interpretation of Fracture
Surface Fractal Dimension," Metallography Past, Present, and Future (75th Annwersary Vol-
ume),ASTMSTP1165, G F VanderVoort, F J Warrnuth, S M Purdy, andA Szlrmae, Eds,
American Society for Testing and Materials, Philadelphia, 1993, pp 295-310
ABSTRACT: The use of fractals in the analysis of fracture surfaces 1s increasingly being inves-
tigated in the hope that this concept may prowde a means of characterizing these complex irreg-
ular surfaces While the prehmmary experimental evidence is interesting and encouraging, ques-
tions concerning the correct measurement and interpretation of fracture surface fractal
dimension remain This paper seeks to address these issues to the extent possible In particular,
it is noted that currently accepted techniques for measunng surface fractal dimensmn are flawed,
and a new alternate techmque based on vertical section profilometry is proposed Important
aspects of this new technique are that it is assumption-free and the required data are obtained by
standard methods involvingreasonable operator effort Finally, possible interpretations of fractal
results are briefly discussed, focusing on potential advantages of use of the entire "fractal plot"
for developing a clearer understanding of surface geometry and the role of mlcrostructure in the
failure event
KEY WORDS: quantitative fractography, fractals, fractal dimension, metallography, metaUur-

glcal specimens, mlcrostructure, metaUographic techniques
The generation of fracture surfaces is the ultimate result of any fracture process The under-
lying premise of fractography, the study o f fracture surfaces, is that the geometry of a particular
fracture surface is a function of the material's mlcrostructure and mechanical and physical
environment dunng failure Therefore, the surface may contain important information con-
cernlng the failure event
The qualitative study of fracture surfaces is well accepted and established, with a broad base
of empmcal knowledge as its foundation. Identification of such features as fatigue striations,
river patterns, and chevron markings are an important, even central component to most frac-
ture studies Fractography in this sense has played a major role in materials science at least
since the advent of the scanning electron microscope (SEM) However, there has been increas-
ing interest of late in the development of a more quantitative approach to fractography, in
which the analysis of the fracture surface is accomplished through the use o f various morpho-
logical parameters measured from the surface geometry The motivation for such a quantita-
tive approach lies In the hope that the geometric data obtained from a surface may provide
deeper insight into the material's failure process than might be acquired by tradmonal obser-
vation-based techniques In particular, it is hoped that the role ofmicrostructure in failure may
be more clearly understood in this way With this in mind, the concept of fractals has recently
received growing attention for the geometric charactenzatlon of fracture surfaces In fractog-
~Graduate research assistant and faculty member, respectively, Georgia Institute of Technology,
School of Materials Engmeenng, Atlanta, GA 30332-0245
295
Copyright
Copyright*by1993
ASTMby Int'l
raphy, fractal dimension is proposed specifically as a parametric descriptor of surface tortu-

osity or complexity It has been proposed that this tortuosity is in turn related to certain impor-
tant matenal properties, most notably toughness, that is, resistance to failure However, owing
to the microscopic scale of the features of interest on a fracture surface, the application of frac-
tals to the study of fracture surfaces raises certain specific questions that bear careful
consideration
1 What is the appropnate means of measuring or estimating the fractal charactenstics of a

fracture surface9
2 How can the resulting fractal data be interpreted once acqmred9
The importance of these particular issues Is self-evident In the case of the former, it is clear
that in order for fractal dimension to be of use m the study of fracture surface geometry, there
must be no ambiguity or uncertainty associated with the collection of the data itself Hence,
the determination of surface fractal dimension should either be performed on an assumption-
free basis or through the use of a limited number of demonstrably reasonable assumptions As
will be discussed later, the currently accepted technique for estimating fractal dimension falls
this crucial requirement
The ultimate usefulness of fractals m fractography hes not in the mere plotting of property
correlations but rather in the understanding that th~s type ofanalys~s may provide on the inter-
action of microstructure and the failure process To perform this function, it must be undei-
stood how the measured fractal data may be used to interpret fracture surface geometry The
importance of the interpretation of acquired fractal data is thus apparent
It is the purpose of this work to address these two topics in turn to the extent possible First,
the issue of the measurement o f fractal dimension from fracture surfaces will be covered, with
the discussion leading to the proposal of a new assumption-free technique for calculating this
parameter Then, aspects of fractal data analysis will be addressed Here, the focus shall be on
the use of the entire set of geometric data available as a result of fractal characterization, rather
than solely on fractal dimension itself
Measurement of Fractal Dimension by Slit-Island Analysis

By far, the most popular technique currently used for estimating the fractal charactenstlcs
of fracture surfaces is the so-called Slit-Island Analysis ongmally proposed by Mandelbrot
[1] The technique is based on analysis of the geometnc features observed on metallographtc
sectioning planes passing honzontally through the surface, as depicted in Fig 1 Two types of
features are observed on these sections islands of fractured matenal isolated against a back-
ground of plating or mounting matenal, and lakes of mounting material within these islands
(see Fig 2) These features are termed "slit-islands" and "slit-lakes," respectively Slit-islands
and sht-lakes are horizontal cross sections through the local perturbations of the surface Thus,
their individual geometry must be related m some way to the overall geometry of the surface,
and it has been proposed that their fractal charactenstlcs can be used to determine the fractal
dimension of the surface [1] In practice, Slit-Island Analysis involves the measurement of the
perimeters and areas of either individual slit-islands or slit-lakes The resulting set of perime-
ter-area data points is plotted on log-log axes, producing a nominally linear plot whose slope,
% yields a fractal parameter, Dp(Fig 3)
Dp = 23' (1)
DRURYAND GOKHALE ON FRACTALS 297
horizontal
sectioning plane
fraet
FIG. 1--Horizontal sectioning plane as applied in Slit-lsland Analysis. Planarfeatures (slit-islands and
slit-lakes) are observed on the metallographic section.
FIG. 2 Sill-islands and slit-lakes as observed on horizontal section for Slit-Island Analysis. Specimen
is 4340 steel failed by impact. Islands and lakes represent perturbations on the fracture surface.
4.0- PLOT ID 1902

SLOPE 0.582
Y-INT 0.551
CORR. COEFF. 0.997 ,,,
t_
o~ 3.0
t_
o~
2.O- &
t_
1,0-
0.0 I I I 9 I
0.( 1.0 2.0 3.0 4.0 5.0
log ,;1"island area (microns 2)
FIG. 3--Fractal area-perimeter relationship from Slit-Island Analysis.
According to Mandelbrot, the fractal dimension of the parent surface, D,, is then given by the
simple expression [ 1]
Dr = Dp + 1 (2)
As just noted, Slit-Island Analysis is the most popular technique for fractal characterization
of fracture surfaces, and numerous attempts have been made to use it in studying possible
correlations between fractal dimension and material toughness. The first of these studies may
be attributed to Mandelbrot, who observed that fractal dimension was related inversely to
impact toughness of 300-grade maraging steel; as impact energy increased (as a function of
tempering temperature), fractal dimension decreased [1]. Subsequent work with various
metallic and nonmetallic materials has produced conflicting results. Fractal dimension is seen
to decrease with increasing toughness in some cases [ 1-3] and to increase in increasing tough-
ness in others [4-8]. In some cases, no correlation at all is observed [9]. It has been demon-
strated recently that a possible source of this general discrepancy and confusion may be found
in the application of Slit-lsland Analysis itself. In a study of impact toughness of a commercial
steel alloy, the nature of the fractal dimension-impact energy correlation was seen to depend
strictly on whether the Slit-lsland Analysis was performed on the slit-islands or slit-lakes
[ 10]. As shown in Fig. 4 (from Ref 10), when performed on the same group of fracture surfaces,
analysis of slit-islands was seen to produce a positive correlation while a negative correlation
was obtained from analysis of slit-lakes. Due in part to this discrepancy, the general applica-
bility and validity of the Slit-Island Analysis may be called into question. In fact, detailed dis-
cussions of the practical and conceptual flaws of the technique have been presented recently
DRURYAND GOKHALEON FRACTALS 299
150 -
0
130 -
110 -
0
90_
slit-lakes slit-islands
70_ 0
0
[-
50-
0 9
30-
E 0 9
Ol
10-
I I I I I
1.20 1.25 1.30 1.35 1.40
Fractal Dimension Dsi
FIG 4--1mpact toughness as a functton offractal dtmenston by means of Sht-lsland Analysts for CK45
steel tempered at different temperatures (sht-lslands and sht-lakes) (reproducedfrom Ref 1O)
[3,10] For the present purposes, it will suffice to summarize briefly these arguments, which
fall into three general categories
First, as has been noted already, the calculated fractal dimension is dependent on subjectwe
operator choice as to whether to perform measurements on the slit-islands or sht-lakes
observed on a given surface To the authors' knowledge, no gmdehnes or rationale for making
this decmlon has been provided to date
Second, the central assumption m the conceptual development ofSht-Island Analys~s is that
the analyzed features, whether sht-lslands or sht-lakes, are geometrically self-similar regardless
of size. That is to say, it is assumed that features d~ffer from one another only m scale, w~th
large features being statlsUcally eqmvalent m shape to smaller ones. There ~s no fundamental
metallurgical reason for this assumption to hold, and recent studies have found that larger
islands tend to be more eqm-axed than smaller ones [3]. Violation of the key self-similarity
assumption introduces arbitrary error into the calculaUon of Ds
The thwd and most powerful argument against Sht-Island Analysis is that no rigorous math-
emaUcal derivation of Eq 2 has yet been provided As a result, the vahdlty of this expressmn
is uncertain and thus it cannot be known under what condmons Sht-lsland Analysis ~s actually
apphcable
Unhl these specific issues can be successfully addressed, the fractal dimension results
obtained by Sht-Island Analysis suffer an unknown extent of uncertainty and the usefulness
of the techmque must be considered limited In order to ehmmate these amblgumes and to
estabhsh fractal analysis as a rigorous and general tool for fracture surface characterization, an
alternate technique for estimating surface fractal dimension is reqmred Such a method based
on digital profilometry of surface profiles is introduced and d~scussed later
fracture surface
fracture
profile
observed section
of fractu re surface
vertical seclioning plane

FIG. 5--Orientation of(vertical) sectioning plane for profilometry.
Measurement of Fractal Dimension by Profilometry

As was the case with Slit-Island Analysis, the determination of fractal dimension by profi-
lometry involves the analysis of features observed on planar metallographic sections inter-
secting the fracture surface. In this case, vertical sections (as opposed to horizontal sections)
are cut through the surface, revealing profiles as indicated in Fig. 5.
In practice, profilometry is performed by manual tracing of the (magnified) profile on a dig-
itizing tablet, resulting in a digital profile map consisting of(X, Y) coordinate points at regular
intervals along the profile. Summation of the segments connecting the coordinate points pro-
vides an estimate of total profile length. Obviously, the profile length estimate depends on the
measuring segment length, ~ (that is, coordinate point spacing), thus introducing the resolu-
tion dependence from which fractal dimension is calculated. Expressing profile length in terms
of dimensionless profile roughness parameter, RL, 2 this resolution dependence is given math-
ematically by the well-known Mandelbrot-Richardson equation
RL(rl) = girl l-~ (3a)
2 Profile roughness parameter is defined as the ratio of total apparent profile length to projected length
RL = total length/projected length
Thus, the RL parameter represents a normalized dimensionless measure of profile length, taking values
upwards from RL = 1 (for a perfectly straight horizontal line).
DRURY AND GOKHALE ON FRACTALS 301
or, in logarithmic terms
log RL(~) = log R~ + (1 -- DL) log n (3b)
where DL is the fractal dimension of the profile. Note that in expressing Eq 3a as a logarithm,
the value of the R~ parameter is seen to be a constant equal to the profile roughness parameter
at unit n length. Higher values of DL are indicative of more tortuous or complex profiles. From
this expression, the value of DL for a given profile is easily measured from profilometry data.
Log-log plots of apparent profile roughness (that is, length) as a function of measuring segment
length, ~, produce a nominally linear plot whose (negative) slope, a, yields DL
DL = 1 -- a (4)
Such plots are known as "fractal plots," and a schematic example is provided in Fig. 6. It
should be noted that only one actual tracing of a given profile is required to generate the entire
fractal plot. This trace, made at sufficiently high resolution (that is, small 7) gives a single esti-
mate of RL at the selected (minimum) n value. Subsequent RL -- n points on the fractal plot
are determined by re-estimating profile roughness from the same profilometry data, but this
time skipping over alternating coordinate points, effectively increasing 71and leading to lower
apparent roughness as small-scale profile features are stepped over. As illustrated in Fig. 7, this
process can be repeated iteratively, each time skipping over increasing numbers of coordinate
points for ever larger values of 7. Further procedural details concerning profilometry and pro-
file fractal dimension are available in the literature [11,12].
A limited amount of work has been performed comparing fractal dimension acquired by
vertical section profilometry to toughness. As noted earlier, the profilometry technique is not
as popular as Slit-Island Analysis and, correspondingly, the body of related work is consider-
ably less. The principal drawback to the use of profile fractal dimension in studies of fracture
surfaces is simply that the parameter that is measured, DL, is not the geometric characteristic
actually desired. It is the fractal dimension of the surface, Ds, that is in fact sought. The rela-
tionship between the fractal characteristics of profiles and their parent surfaces has not previ-
ously been derived. Consequently, previous results obtained by profilometry are subject to the
log q
FIG. 6--Fractal plot of profile roughness. Profilefractal dimension, DE, is measuredfrom Slope a.
segment length: q = ql
segment length: q -- qZ
segmenl lellgth: r 1 = q~
rl I < r l 2< l l 3
R L(q 1) > RL(rl2 ) > RL(rl3 )

FIG 7--Schematzc profile ind~catzng decrease m apparent roughness, RL, wzth tncrease m measuring
element,
same type of uncertainty or a m b l g m t y that occurs m the case o f Sht-lsland Analysis There-
fore, it is relevant at th~s point to introduce and discuss a new technique for calculating the
fractal d i m e n s i o n o f surfaces f r o m profilometry data
It can be seen that the resolution dependence o f the observed fracture surface area can be
expressed through a M a n d e l b r o t - R l c h a r d s o n equation of the same form as that presented ear-
her for profiles, that is,
R,(K) = R : 2-~ (5)

In this expression, r = r/2 and is the m e a s u n n g area element size, Rs is the surface roughness
parameter 3 analogous to the profile roughness p a r a m e t e r introduced earlier, and the R : term
is likewise the surface roughness parameter at unit r
3 Surface roughness parameter ~s defined as the ratio of total apparent surface area to projected area
Rs = total surface area/proJected area
Thus, the parameter is the three-dimensional analogue to profile roughness and vanes m value upwards
from Rs = 1 (for a horizontal planar surface)
In order to determine the value of D, directly from Eq 5, it must be possible to estimate or

directly measure the area of the fracture surface as a functmn of measunng area element size
Currently, there are no practical means for directly carrying out such measurements on the
small scales associated w~th fracture surfaces Recently, however, a general assumption-free
expression relating surface and profile roughness parameters has been derived. This expression
replaces previous linear R, - RL equaUons that are based on various assumptions of artificial
surface geometries F o r the present purposes, the new expression ~s useful in that it provides a
means of determining the resolution dependence of the surface roughness from profilometry
data on an assumption-free basis That is to say, surface fractal dimension can now be calcu-
lated without the assumptmns and ambiguity associated with previous methods
Introducing a structure factor, ,It, that is a functmn solely of the angular distribution func-
tion of the profile segments, it can be shown that [ 13]
R, = RL ",I' (6)
The detailed derivation of Eq 6 and practical issues assocmted w~th its ~mplementation are
presented in the hterature [13,14] Here, it will suffice to surn manze certain key features of the
expression
1 As noted, the expression is general and assumption-free and is therefore applicable to all
fracture surfaces regardless o f geometry or anisotropy
2 It is emphasized that the RL and ~ parameters are both easily obtained from profilometry
data The digitized profile trace contains all the information needed to calculate the val-
ues of RL and 9 The 9 term, which typically ranges from 1 l0 to 1 35, is calculated by
a relatively simple integration of the probability distribution function of the angular ori-
entations of the individual profile segments A practical tabulated solution to the angular
distribution function integration is available [14]
3 Finally, the ( - - ) is included in Eq 6 to indicate that surface roughness IS equal to the
" m e a n " of the RL 'I' product (not the product of means) averaged over one or more
vertical sectioning plane orientations In the case of anisotropic surfaces (that is, those
surfaces displaying considerable dlrectmnahty or preferred orientation in the plane of the
fracture), it can be shown that profilometrlc sampling on at most three sectioning plane
onentaUons IS sufficient [14]. In the case oflsotropic surfaces (that is, no dlrectlonahty),
only one vertical sectioning plane is required as all such planes are statistically
equivalent
The use of Eq 6 for the estimation of Ds is straightforward After sectioning and metallo-
graphically prepanng a representative section through the fracture surface of interest, profi-
lometry is performed at the desired resolution using a digitizing tablet optically linked via
video camera or optical drawing tube to an optical microscope Profile tracing may also be
performed using photomicrographs of the profile if the required imaging equipment is not
available The surface roughness parameter is then calculated from the resulting geometric
data using Eq 6, which is rewritten here as follows to emphasize the dependence of the calcu-
lated Rs on the size of the profile measuring segments
R~(y) = RL(y) ~(~) (7)
The calculation is performed repeatedly at ever increasing values of n (that is, decreasing res-
olution) that are obtained from the original profilometry data by skipping over increasing
numbers of intervening coordinate points when measunng for RL and ~'. This procedure
results in a range of Rs(n) values varying as a function ofn A fractal plot of surface roughness
0.40.
0.20. SLOPE= - 0 . 0 7 0
m
0.00.
-'2.0 -'I .0 0'.0 I'.0 2'.0 3'.0 4'.0 5'.0 6'.0

log ruler area (112 )
FIG. 8--Fractal plot. 4340 steel (tensile failure). Traced at • 200 with a minimum n of 3.5 ~m.
is next generated by plotting log Rs(n) versus log n2. Figure 8 presents an example of a typical
fractal plot obtained in this way for a fracture surface of a tempered 4340 steel specimen failed
in tension. The characteristics of this particular plot will be discussed in more detail later.
Referring to Eq 5, it can be seen that the fractal dimension of the surface can then be obtained
from the slope, ~, of the fractal plot
Ds= 2- 2/3 (8)
The following comments are reiterated to emphasize the characteristics of the proposed
technique.
1. The Ds parameter obtained using Eq 7 is identically the fractal dimension of the fracture
surface and is the result of a general, assumption-free calculation. Thus, aside from sta-
tistical sampling considerations (which may be quite important), there is no uncertainty
or ambiguity associated with this technique or the interpretation of the resulting fractal
data.
2. The Ds parameter is calculated from data that is readily acquired from profilometry of
vertical sections through the fracture surface. A simplified algorithm for calculating the
structure factor, xI,, from the profile angular distribution function is available in the
literature.
3. Finally, it is noted again that only one sectioning plane is needed for the analysis ofiso-
tropic surfaces; at most, three sectioning plane orientations are required in the case of
even the most extreme anisotropic surfaces.
Interpretation of Fractal Data

To this point, a new technique that gives a more solid, less ambiguous foundation to the
determination of the fractal dimension of fracture surfaces has been presented and discussed.
Thus, the first of the questions posed at the outset has been addressed. Attention is now turned
to the interpretation of the resulting fractal data. Interpretation, in this case, is meant to imply
the development of an understanding of the underlying fracture surface geometry from con-
sideration of fractal characteristics. The establishment of fracture mechanisms or functional
DRURYAND GOKHALEONFRACTALS 305
material property relationships based on fractal data represents a far more ambitious topic that
will undoubtedly be the focus of considerable future investigation In addition, rather than
focussing solely on the fractal dimension parameter discussed thus far, emphasis is placed here
on consideration of the entire fractal plot generated by a given surface As wdl be discussed
later, these plots may contain a large amount of geometric information related to the surface
of which fractal dimension is but one aspect Certain characteristics of the fractal plots gen-
erated by real fracture surfaces will first be discussed Possible implications of these character-
lStiCSwith regard to the material's microstructure and fracture surface will follow. However, it
should be noted that the interpretation o f fractal data acqmred from fracture surfaces ~s a rel-
atively recent concept and one that is undergoing continuous refinement Therefore, the fol-
lowing discussion is intended primarily to propose possible concepts that may provide avenues
for future theoretical and experimental effort
Figure 9 presents a schematic fractal plot of the form that is commonly encountered in the
analysis of real fracture surfaces. The curve displays a reverse-sigmoidal form, with upper and
lower plateaus bounding a linear so-called "fractal domain " T h i s deviation from classic frac-
tal behavior at the plateaus is well understood and expected On the right-hand side of the
figure, the lower plateau occurs at the point at which the profile measunng segments are span-
ning virtually all features of the profile Effectively, no features are encountered and the profile
and surface roughness values approach their lower limits OfRL = R, = 1 The existence of the
upper plateau is based on logic and experimental observation Simply put, it is not possible for
a fracture surface to have infinitely increasing surface area at ever greater resolutions, as would
be implied by a classic linear fractal plot The surface's scale must at least be expected to be
bounded at the atomic scale There have been attempts to argue against the existence of the
upper plateau on the grounds that profile lengths or roughnesses are often not experimentally
observed to approach asymptotic upper limit values at small n However, this is merely a ques-
tion of inadequate resolution, as profile traces performed at too low resolution will fall below
(that is to the right of) the upper plateau on the fractal plot and the effect will not be observed.
An example of this is provided in the fractal plot for the 4340 tensile fracture surface presented
previously as Fig 8 This figure was produced from profilometry performed at a magnification
of • 200 and a corresponding profile segment length of r/ = 3 5 #m No upper plateau is
observed m this figure Now consider Fig 10, which is a fractal plot resulting from portions of
upl)er plateau
1 - (Ds/2)
m
fractal
donmin lower plateau
0.0
2
h)g
FIG 9--Fractal plot with reverse stgmotdal form indtcated, upper and lower plateaus devtate from clas-
sw fractal behavior
r'q
0 40. [] -~ ~ , ~
[]
020. SLOPE= -0 072
m
m ~]CB
m r'~
mD []
0 00.
- '2 0 -'1 0 0'0 10 2'0 .5'0 4'0 5'.0

2
Io~ railer area (I 1 )
FIG l O--Fractal plot 4340 steel (tenstle fadure) Traced at • 10 000 with a minimum ~ of O 06 ~rn
the identical profile traced at • 10 000 on an SEM, providing a m a x i m u m resolution of ~ =

0 06 um The upper plateau is readily seen in this figure. (Because only portions of the profile
are traced for this latter figure, absolute values of roughness cannot be compared between Figs
8 and 10.) This observation is further supported by Fig. 1 l, an SEM mlcrograph of this fracture
profile taken at • l0 000 It can be seen from this micrograph that the physical size limit of
the profile features (and hence the surface features) has been reached at this resolution--there
are no more details to be observed or to contribute to increased profile length at yet higher
magnification
Attention is now turned to the implication of the fractal plot's form for the analysis of frac-
ture surface geometry Figure 12 presents a schematic fractal plot on which four specific points
have been identified Clearly, these points, labeled Rs*, Ds, ~o, and fl in the figure, are interre-
lated and their values are determined by the shape of the plot. Since surfaces with dlffenng
geometric characteristics may be expected to yield different fractal plots, the Rs*, D,, ~o, and
parameters reflect characteristics of the surface and may therefore provide useful lnformaUon
regarding its geometry Moreover, because these parameters are interrelated, each serves to
give addmonal reformation concerning the others This is best demonstrated by way of
example
It has been noted that surface fractal dimension is a descriptor of surface tortuoslty, with
higher values o l D , indicative of more intricate or complex structures. However, fractal dimen-
sion is by definition independent of physical scale, and thus provides no insight into that
important aspect of a surface's geometry That is to say, two surfaces may have equal fractal
dimensions and yet contain features lying m widely disparate size ranges In both a geometric
and a metallurgical sense, such surfaces are not equivalent and Ds alone does not identify or
quantify the difference However, when the scaling terms, w or fl or both, are included, the
scale range can be estimated and a more complete impression of the surface ~s achieved Of
course, similar examples may be conceived for relationships between Re* and the other fractal
plot variables
Although it is well known that fractal dimension is a measure of tortuosity, there is a com-
mon misconception that this can be translated into the thought that D~ therefore represents
an alternate indicator of surface roughness. Consideration of Fig 12 shows that th~s is not so,
at least m the sense that the term roughness is generally applied m quantitative fractography
FIG 11- - S E M mtcrograph of fracture profile observed at • 10 000 Note smooth contour of profile,
ln&catmg that the scale hmu of the profile features ts attained
0 I
Rs
0~ m I
I
co 2 D.
log 11
FIG 12--Fractalplot wlth Rs, Ds, oa, and ~ parameters zndtcated
In addition, statements to the effect that "as fractal dimension increases so does surface rough-
ness" are misleading. The two properties, though related, are separate characteristics of a given
surface and it is easy to conceive of two fractal plots (stemming from two fracture surfaces) for
which the preceding statement does not hold. As is demonstrated in Fig. 13, the relationship
between fractal dimension and roughness is dictated by the range of scale over which fractal
behavior is observed.
It has been noted that the w and ft scale parameters reflect the physical scale of a fracture
surface. As a result, the parameters may provide some insight into the relationship between
surface geometry and the material's microstructural features. In locating the fractal plot upper
plateau, the w term effectively defines the scale of the smallest features encountered on the
profile (or surface). Surface features naturally originate from the underlying microstructure,
with particle-nucleated dimples and grain boundary surface facets being two notable exam-
ples. Thus, o~ may be representative of the scale of the smallest microstructural features that
are involved in the failure process. This size information may in turn be used to help in the
identification of those features. Of course, the scale relationship between ~0and microstructure
is not expected to be 1: 1 (that is, the value of~o cannot be matched directly to particle diameter,
for example) due to the presence of complicating deformation processes. Nevertheless, the
parameter does represent a geometric characteristic of the fracture surface and appears to war-
rant further investigation.
The ~ parameter locating the lower plateau of the fractal plot is somewhat more complicated
(Rs)1 )1> (R)2> (R)3
=
~o
(Rs)2[ "'
s
1
s
2
s
(Rs)3
t...
i
i
ml 2
log of resolution (rl 2)

FIG. 13--Schematicfractalplot indicating the interdependence between roughness paramelers, fractal
dimension, and the scale range of thefracture surface.
DRURYAND GOKHALEONFRACTALS 309
to interpret. The parameter cannot, for example, be hnked to a speofic m~crostructural or

surface feature as its value is due to the cumulative effect of all smaller features. However, ~2
may represent some measure of surface homogeneity--features smaller m scale than ~2will be
represented w~thm surface samples of s~ze f~ m the same stahstlcal proportions as the surface
as a whole The parameter should also therefore indicate a m i n i m u m size reqmrement for the
purposes of statistical samphng of surface features Work is currently ongoing to further Inves-
tigate and demonstrate these surface scahng concepts
Summary
In this work, certain important considerations for the use of fractals in the characterization
of fracture surface geometry have been addressed (a) how to measure fractal dimension and
(b) how to interpret the resulting data With regard to measurement of fractal dimension, a
new technique based on vertical section profilometry is proposed The method offers the
advantage of being assumption-free and unambiguous in terms of the surface characteristics
actually estimated In addition, it is felt that this technique does not entad an impractical level
of operator effort--the required input IS entirely prowded by standard profilometry data
acqms~tion procedures
On the topic of fractal data interpretation, it is felt that consideration of the entire fractal
plot may provide more useful geometric information than use of fractal dimension alone In
particular, the location points of the upper and lower plateaus of the reverse-slgmoldal fractal
plots may provide a hnk between the scale of surface geometry and mlcrostructure.
Acknowledgment
This work is supported by the National Science Foundation sponsored project DMR-
9013098, entitled "Quantitative Analysis of Fracture Surface Using Stereologlcal Methods"
Dr Bruce MacDonald is the project monitor. Additional support is provided by ALCOA
References
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[2] Mu, Z Q and Lung, C W, "Studies on the Fractal Dlrnenslon and Fracture Toughness of Steel,"
Acta Metallurgtca Smtca, Vol 24, No 2, 1988, pp 140-146
[3] Pande, C S, Rlchards, L E, Louat, N, Dempsey, B D, and Schwoeble,A J, "Fractal Character.
lzatlon of Fractured Surfaces," Acta Metallurgwa, Vol 35, No 7, 1987, pp 1633-1637
[4] Huang, Z H, Txan,J F, and Wang, Z G , "Analysis of Fractal Characteristics of Fractured Surfaces
by Secondary Electron Line Scanning," Matertals Science and Englneermg, Vol A 118, 1989, pp
19-24
[5] Mecholsky, J J, Passoja, D E, and Femberg-Rxngle,K S, "Quantitative Analysis of Brittle Frac-
ture Surfaces Using Fractal Geometry," Journal, American Ceramics Society, Vol 72, No 1, 1989,
pp 60-65
[6] Mecholsky, J J and Mackm, T J, "Fractal Analysis of Fracture in Ocala Chert," Journal of Mate-
rtals Scwnce Letters, Vol 7, 1988, pp 1145-1147
[7] Wdhford, R E, "MulUfractal Fracture," Scrlpta Metallurglca, Vol 22, 1988, pp 1749-1754
[8] Wang, Z G , Chen, D L, Jlang, X X, AI, S H, and Shlh, C H, "Relationship Between Fractal
Dimensionand Fatigue Threshold Value in Dual-Phase Steels," Scrtpta Metallurgtca, Vol 22, 1988,
pp 827-832
[9] Rlchards, L E and Dempsey, B D, "Fractal Characterization of Fractured Surfaces in T1-4 5 AI-
5 0 Mo-1 5 Cr (Corona 5)," Scrtpta Metallurgwa, Vol 22, 1988, pp 687-689
[10] Huang, Z H, Tlan, J F, and Wang, Z G , "A Study of the Slit-Island Analysis as a Method for
Measunng Fractal Dimension of Fractured Surfaces," Scnpta Metallurgtca, Vol 24, 1990, pp 967-
972
[11] Underwood, E E and Baneol, K, "Quantltatwe Fractography," ASMMetals Handbook, Vol 12,
9th ed, Amencan Society for Metals International, Metals Park, OH, 1987
[12] Banerjl, K, "Quant~tatwe Fractography A Modern Perspectwe," Metallurgtcal Transactions A,
Vol 19A, 1988, pp 961-971
[13] Gokhale, A M and Underwood, E E, "A General Method for Estimation of Fracture Surface
Roughness Part I Theoretical Development," Metallurgical Transacttons A, Vol 21A, 1990, pp
1191-1199
[14] Gokhale, A M and Drury, W J , "A General Method for Estlmatxon of Fracture Surface Rough-
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1207
Applications I
J a m e s A. N e l s o n I
In Search of Microstructure
REFERENCE: Nelson, J A , "In Search of Microstructure," Metallography Past, Present, and
Future (75th Anmversary Volume), ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M
Purdy, and A Szlrmae, Eds, American Sooety for Testing and Materials, Phfladelphm, 1993,
pp 313-326
ABSTRACT: When metals were discovered over 8000 years ago, there was no scientific basis for
understanding their properties Although metal producUon and working were developed by tnal
and error, skills were developed that produced amazing works of art and utlhty Based upon sur-
face evidence, Renaissance philosophers and alchemists speculated that metals possessed a dis-
crete internal structure It was not until the m~d-mneteenth century that Henry Sorby developed
the first successful method ofreveahng the mmrostructure of metals and alloys From th~s begin-
ning, the search for mlcrostructure was aided by new developments such as synthetic abrasives
and improved equipment With each new wave of alloy development, metallographers modified
the simple technique developed by Sorby to accommodate the new materials Cemented car-
Ndes, super alloys, and nuclear materials were challenges that were overcome by adapting tra-
dmonal metallography However, when tradmonal metallography was apphed to the most
recently developed advanced matenals such as fine ceramics, composites, and thermally sprayed
coatings, it was apparent that a new dlrectmn was needed Using a comblnatmn of fixed, semi-
fixed, and free abraswes, and a graded series of lapping platens and cloths, a three-stage system
has been developed that is capable of solving the challenges represented by the new wave of
advanced materials
KEY WORDS: metals, metallurgy, metallography, mlcrostructure, advanced matenals, fine

ceramics, composites, thermally sprayed coatings, lapping, deformatmn, pohshmg, abrasives,
metallurgical speomens, metallographlc techmques
The Roots of Metallurgy

Mlcrostructure has been present m our m a t e n a l world since its formation but not until
recent times has it been possible to reveal it Metals were first discovered eight to ten thousand
years ago w h e n a n o e n t m e n found metallic meteorites lying on the ground after a meteorite
shower. Figure 1 is an artist's depiction o f such an event, titled, Metals from Heaven It is evi-
dent that ancient people believed that meteorites c a m e from G o d and therefore treated t h e m
as rehgmus objects.
However, this sketch also suggests that early discoverers o f m e t e o n t e s must have recogmzed
a dramatic difference in the properties o f this new material c o m p a r e d to the m o r e familiar
stone that it resembled This appreciation of the unique properties o f m e t e o n t i c iron ulti-
mately led to ItS use for m a k i n g tools Archaeological discoveries indicate that m e t e o n t l c ~ron-
working lasted until approximately 2000 B C. w h e n iron smelting began [ 1]
T h e discovery o f natwe metals such as gold and free copper gave ancient m a n an early appre-
cmtlon of malleablhty and enabled him to shape these materials into m a n y forms, including
extremely thin foils that were used to overlay other less beautiful matenals W i t h o u t previous
experience and a soentlfiC base, m a n learned the metallurgical arts by tnal and error experl-
J Manager, Educational Services, Buehler, Ltd, Lake Bluff, IL 60044
313
Copyright
Copyright*by1993
ASTMbyInt'l
FIG 1 --Metals from Heaven--the discovery of meteoric iron by the Egyptians (courtesy of Basw Cor-
poratton, Jrom an ortgmal drawmg by Paul Calle)
mentatlon By this stow, tedious process, the ancients gradually learned to produce exqmslte
items of jewelry and other fine works of art In particular, the dazzling works of wrought gold
crafted by the a n o e n t Egyptians have been exhibited throughout the world and never cease to
amaze those who v~ew them
The low hardness and scarcity of native (free) copper made it unsuitable for durable tools
As a result there never was a "Copper Age" period ofhlstory However, the discovery of smelt-
ing gave the a n o e n t metal workers a new and larger source of raw material The &scovery of
alloying provided harder materials that were statable for tools and weapons Sturdy bronze
tools such as the ones shown in Fig 2 were produced by the Chinese around the fifth century
B C [2] When temperatures high enough to melt metals were achieved, mtncate shapes could
be produced by the casting process Although metal casting did not originate in China, the
Chinese elevated the craft by their typical skdl and imagination Figure 3 shows an elaborate
cast bronze wine vessel that dates back to Warring States period of Chinese history
The beginnings of iron making have been traced to the area around the Black Sea where the
earliest evidences ofcarburlzatlon were found This development made it possible to heat-treat
irons to produce superior tools and weapons Harder tools and weapons gave certain nations
a powerful advantage over their less advanced neighbors Even without an awareness of micro-
NELSON ON MICROSTRUCTURE 315
FIG 2 - - H ~rought bronze tools"From be~ore the frith centur)~ B C
FIG 3 - - A n intricate cast bronze wine vessel--the Warring States perzod
structure, man slowly learned to obtain, refine, and shape metals and alloys Empirical met-
allurgy quietly revolutionized the world
The Search Begins

The search for mlcrostructure began when it occurred to thinking minds that its existence
might explain why the metals possessed such unique properties Like any search, it was
impeded by obstacles In the case of the search for mlcrostructure, they were
1 A lack of prior knowledge and experience

2 False assumptions and premises
3 The mabihty to understand the nature of deformation, the main obstacle to viewing
mlcrostructure
The first hints of mlcrostructure may have been the patterns seen on swords that existed
even before they were described in recorded history m 540 A D Damascus swords, as shown
in Fig 4, are legendary for both their extreme sharpness and beautiful designs that graced their
blades These pleasing patterns were the result of their high (1 5 to 2%) carbon content and a
series o f forging and heat treatments that cause the matenal to have great strength and hard-
ness without becoming brittle The beauty of the damask pattern has long respired both
esthetic and the technically minded persons since it first appeared From this first encounter
with Damascus swords, men of metals have tried and still try to duplicate its patterns and prop-
ert~es The presence of the damask pattern gave the world a glimpse of mlcrostructure that was
yet to be revealed [3]
It was not until the Renmssance period of Western history that alchemists and philosophers
became convinced that the unique properties of metals and their alloys were related &rectly
to their mlcrostructure Such speculations were further stimulated by observations such as
FIG 4--The Damask pattern oJ a Damascus sword (~ourtesy o/h,~ Wads'worth)
grain facets in coarse-grained fractures or dendntes in the sink head of castings These inquir-
ing minds tried to imagine what microstructure looked like without having ever seen it Many
of these conceptions seem ludicrous to us today while others were surprisingly plausible con-
slderlng the lack of a true science [4]
The development of the microscope offered the opportunity for investigators to make mag-
nified observations of metallic surfaces, but what they saw was mostly surface artifacts such as
gouges When they tried to prepare metallic surfaces to reveal the true mlcrostructure, their
lack of understanding of deformation in ductile materials prevented them from seeing the true
mlcrostructure These early attempts at polishing were unsuccessful because their techniques
did more to hide microstructure than to reveal it.
The ability to consistently reveal the true mlcrostructure of metallic materials was not made
public until 1864 when Henry Sorby, shown in Fig 5, presented a paper describing his suc-
cessful efforts to reveal the mlcrostructure of steel His success no doubt resulted from his
understanding that microstructure cannot be seen unless deformed material is completely
removed
He wrote, "Anything approaching to a burnished (deformed) surface and polished scratches
is fatal to good results" [5]
Sorby contributed other firsts to metallography by adapting a transmitted light microscope
for use as a reflected light microscope, enabling himself to view mlcrostructures by bright field
illumination He also made numerous observations during the brief three-year period he
worked with metals exclusively and is responsible for giving the iron-carbon eutectoid micro-
FIG 5--Henry Sorby, thefather oJrnetallography
structure its name, pearllte His successful method was almost simultaneously duphcated by
other investigators on the continent This simple concept became widely used, modified, and
improved by those who followed, but the basic prlnople remained essentially the same
With the axd of mlcrostructural analysis, it was possible to increase the production and
improve the quality of steel by momtorlng the microstructure at various stages of production
Together with the advances m physics, chemistry, and the development of analytical tech-
tuques such as X-ray crystallography, steel metallurgy advanced through the first part of the
twentieth century It was now possible to develop new alloys from a soentlfiC base rather than
by trial and error This resulted in new alloys such as duralumlnum that made metal aircraft
a practical reality
The Search Continued

Those who followed after Sorby made their own unique contributions to the advancement
o f metallography John Edward Stead, for example, designed and bmlt his own sample prep-
aration eqmpment and devised improved techniques that were better and faster than Sorby's
He employed photomlcrography extensively and, by 1897, had produced over 600 photomi-
crographs of good quahty [6]
The search for microstructure was also encouraged by the development of improved mate-
nals to aid sample preparation Synthetic alumina and silicon-carbide abrasives were intro-
duced at the turn of the century, giving metaUographers the ablhty to prepare the newly devel-
oping harder and tougher alloys When cemented carbides were developed in the 1920s,
dmmond abraswes were used to polish samples for mlcrostructural analysis Later, when super
alloys were developed for high-temperature turbine apphcatlons, more challenges were faced
by the metallographer Again, it required modifications in procedures such as attack pohshmg
to remove tenacious deformation layers that still haunted the microstructural analyst The use
of these potentially hazardous solutions and the need for higher pressures and better control
led to the development of semiautomatic pohshlng devices such as the one shown in Fig 6
If metallographers who followed Sorby and the other pioneers of metallography had only to
deal with iron and steel, there would have been httle incentive to seek unique new ways to
prepare samples As ~s often the case, the need for new materials to make war spurred the devel-
opment of the superalloys
This impetus that began during World War II, carried over into the post-war period of the
1940 to 50s It also saw the emergence of the nuclear industry and the need to prepare radio-
active samples remotely without the usual personal touch Metallography had to be performed
with the operator behind 3 ft ofh~gh density concrete lined w~th stainless steel Remote sample
preparation in a hot cell, such as shown m Fig 7, made effectwe use of a hitherto httle appre-
ciated polishing device known as the vibratory pohsher This device allowed maximum acces-
sibility to the samples because there was no need to secure them m a mulUple sample fixture
Photomicrography and m~crohardness testing were also performed remotely using specmlly
adapted devices [7]
The invention of the transistor in 1948 spawned the electronic industry and a whole new set
of sample preparation challenges Solid-state mlcroelectromc devices may include combina-
tions of brittle silicon, ductile metal conductors, and extremely thin oxide layers mounted on
refractory metal or ceramic bases and encased in stainless steel, glass insulators w~th iron-
nickel lead pins. The highly dissimilar properties of the component materials made it difficult
to avoid relief such as shown in Fig 8 This condmon plus the brittleness of silicon combined
to give the metallographer/fadure analyst a severe test ofh~s skdts The low-speed saw was first
developed to section fuel pellets but became a key player m the mlcroelectromc sectioning
FIG 6--An early semtautomattcpohsher
laboratory This small but powerful tool made it possible to section through the highly fragile
and highly dissimilar materials without destroying their integrity
It Is apparent that metallography has served as well through adaptation, modification, and
a wllhngness of metallographers and materials scmntlsts to search for new and creatwe ways
to solve each new challenge that comes their way The story does not end here The search for
mlcrostructure has in recent days been challenged by yet another round of change, the
advanced materials
The Search Renewed

Ltmltatlons of Tradttlonal Metallography
One important pnnclple o f education recognizes that we learn by progressing from the
known to the unknown However, the tendency to resist significant change often stands m the
way As new alloys were being developed and metallographers applied the new abrasives and
apparatus, they generally followed the basic method developed by the pioneers of metallog-
raphy This conventional metallography was simple and easy to employ and has been the
backbone of metallography for over a hundred years It can best be described as a method that
FIG 7--Operating face of a hot cell used for high radiation level metallography
employs a series of increasingly fine abrasive steps, each step replacing deformation left by the
previous one but with a lesser amount of deformation
Metallographers have used this method successfully, making whatever modifications that
have been necessary to cope with a specific sample material Because this method worked so
well for so many c o m m o n metals and alloys, little effort was made to understand the basic
pnnclples of matenal removal Metallographers were often entrepreneurs who devised their
own special "recipes" that they kept on index cards in a file box. This trial and error philosophy
of metallography has been partly responsible for its label as a black art rather than a scientlfc
dlsophne
With the development of advanced materials such as englneenng (fine) ceramics, metal and
polymer composites, and high-performance surface coatings, some weaknesses o f t r a d m o n a l
metallography soon became apparent. When these sample preparation techniques were
applied to the new materials, the results were generally unacceptable for the reasons summa-
razed in Table 1
The normal response ofmetallographers to these problems had been more steps, increased
pohshlng times, or add some individual operator finesse Clearly, this approach did not work
well and it was apparent that fresh thinking and a new approach was needed
The Search for a N e w Dtrectton

The renewed search began with a new look at the basic parameters that control the abrasive
surface preparation process. While the parameters that influence the matenal removal process
are well known, their actual role and interaction had never been fully explored The choices
o f abrasives, cloths, and other parameters were often based upon the the work of others, or on
arbitrary selections later confirmed or disproved by tnal and error It smacked of the p n m m v e
p e n o d of metallurgy.
FIG 8--Mlcroelectromc devwe consisting of many hzghly dlsstmtlar materzals as pohshed, • 100
It Is ironic that the secret to finding a new approach to solving the challenges of advanced
materials lay m the s~mple p n n o p l e that gave Sorby his original success "Anything approach-
ing to a burnished (deformed) surface or polished scratches is fatal to good results" Sorby
understood this pnnclple as it applied to ductile materials but he also knew how to handle
brittle materials because he had previously developed petrographic thin sectioning techmques
TABLE 1--Specimen preparatlon challenges of advanced

matertals
Fine ceramics fractunng/pull-out

edge rounding
lengthy preparaUon t~mes
Composttes fiber fractunng
extreme rehef
persistent matnx scratches
Thermally sprayed coatings lnterfaclal rehef
edge rounding
constituent pull-out
soft constituent smear
for rocks and minerals The big difference was that he hadn't encountered both extremes in
the same material as is so often true with advanced materials.
A more complete appreciation of these problems may be realized through a comparison of
the sharply different material removal mechanisms that control the abrasive sample prepara-
tion process Samuels shows how material is removed from ductile materials by a mlcroplan-
lng mechanism [8] and Zipperlan has described the fracturing mechanism that controls abra-
sive material removal during the polishing of brittle materials [9] The question that naturally
arises is "Can both mechanisms operate simultaneously to prepare advanced materials that
contain both ductile and brittle constituentsg"
The Problem Analyzed

Sample preparaUon consists of three basic operations flattening, deformation reduction,
and scratch removal Unfortunately, these operations often run cross-purpose to each other
Hattenlng requires a high material removal rate but heavy material removal with bonded
(fixed) abrasives causes considerable depth of deformation and fracturing With ductile mate-
rials, this can be corrected by adding additional finer grinding steps However, brittle materials
or constituents may be seriously damaged by surface fracturing, pull-out, and subsurface
cracking This damage may be so severe that no reasonable number of subsequent steps and
pohshlng times will succeed in removing it
Deformation reduction has traditionally employed a series of silicon-carbide abrasive
papers in the range of 240 to 800 grit Although this works well for softer materials, it is inef-
fective for the removal of material from harder samples having slgmficantly deep damage
Unfortunately, silicon-carbide papers break down rapidly on harder materials, making it nec-
essary to repeat each step up to three times Furthermore, finer bonded abrasives Initiate edge
rounding that is amplified during the subsequent cloth pohshlng steps Various investigators.
beginning with Gendron [10], recognized the potential of lapping as a means of deformation
reduction Later, Nelson [11] described the use of a single lapping platen method and Bous-
field [12] proposed the use of a graded series of platens as part of a comprehensive materials
preparation concept Low-napped or napless polishing cloths charged with diamond abrasives
in the 3 to 15 #m range are also part of the deformation reduction stage of sample preparation
Scratch removal is normally the function of the final stage of sample preparation Too often
this stage IS expected to correct problems that were created by inadequately performed prior
steps This results In overpohshlng, producing edge rounding, mIcrostructural relief and pit-
ting in ductile materials There is a general worsening of any polishing artifacts that have been
initiated in previous steps No amount of operator finesse or special products can turn final
pohshlng into a problem-solving step The material removal rate is too low to effect any sig-
nificant change
If this analysis is true, how is it possible to prepare difficult advanced materials to reveal the
true microstructure9 It should be obvious that a rehash of conventional metallography had
little chance of producing the results needed to prepare advanced materials The solution to
the dilemma was found through a reexamination of the parameters that control matenal
removal It was found that the employment of a combination of material removal mechanisms
was necessary to achieve the desired result Since detailed descriptions of this advanced mate-
rlal preparation approach has already been published in the open literature [13-16], only the
basic principles will be highlighted here
The new concept addresses the challenging properties of the advanced materials by using a
varied combination of abrasive mechanisms In the planar grinding stage, both fixed abrasives
and coarse free abrasives applied to hard lapping platens are used to obtain the needed high
material removal rates Free abrasives on moderately hard lapping plates and semifixed abra-
FIG. 9--Comparison of resu#s obtained by conventional versus advanced specimen preparation of alu-
mina: as polished, • 100,"(a) conventional specimen preparation and(b) advanced specimen preparation.
FIG l O--Comparison of ~onventzonal versus the advanced preparation of a 95Nz-5Al thermal spray
coat as poh~hed, d~erentlal mterJerenc e contra~t (DIC) tltummatton, • 100, (a) conventtonat spectmen
preparatzon and (b) advanced spectmen preparation
slves on napless cloths are used to remove deformation in the sample integrity stage Final
pohshmg is performed using sem~fixed abrasives on e~ther napped or napless cloths, depending
on the hardness of the specimen matenal. This combination of surfaces and abrasives makes
it possible to solve the most challenging advanced matenals specimen preparation problems
New approaches to the preparation of the advanced materials further are incorporating pol-
ishing principles long ignored by metallographers Combined with carefully selected elements
of tradmonal metallographIc practice, the true mlcrostructure of wrtually any matenal may
be revealed without artifact The benefits of this concept are best appreciated by companng
the results achieved using the advanced method versus those produced by the conventional
technique Figure 9a shows how even good conventional specimen preparation leaves damage
in the form of pull-out, but when the same material is prepared by the advanced method, there
is virtually no damage produced Figure 10a is a thermally sprayed coating polished conven-
tionally and shows severe rehef and some obscured porosity when compared to Fig 10b, the
same material prepared using the advanced preparation method
Summary
The discovery of mlcrostructure and parhculady the secret to reveahng it was a truly sig-
mficant event m man's history Its realization played a significant role in promoting metallurgy
from an art to a science The nature of mlcrostructure eluded investigators for hundreds of
years until a skilled scientist learned the secret that kept it hidden Henry Sorby's understand-
ing of deformation and what was necessary to remove it led to his development of the first
successful sample preparation method
Since that initial discovery, materials scienUsts have developed many new engineering mate-
nals that have challenged the metallographer's skills However, each challenge has been met
with a new abrasive, a new piece of equipment, or a new techmque Just when it appeared that
all the material worlds had been conquered, advanced matenals presented us w~th new and
greater challenges Each new challenge serves as a fresh reminder that the removal of defor-
mation and brittle damage is the key to success "Those who cannot remember the past are,"
in the words of George Santayana, "condemned to repeat it" [17]
Today the search for m~crostructure differs from that of the anoents who began theirs with
httle knowledge, expenence, and no technical library Hopefully, our renewed searches begin
with a knowledge of the materials we prepare, a thorough understanding of the preparation
processes we intend to use, an appreciation for what is already known, and finally, thoughtful
planning and thorough expenmentatlon Each time a materials scientist or metallographer
begins the process of sample preparation, his or her search for microstructure begins again
References
[1] Ehade, M, "The Forge and the Crucible," 2nd ed, Umverslty of Chicago Press, Chicago, 1962, pp
19-26
[2] "Tonglushan--Pearl Among Ancient Mines," edited by Huangshl Museum, Hubel, Chinese Soci-
ety of Metals, Beljmg University for Iron and Steel, Cultural Relics Pubhshlng House, Beljlng, PRC,
1980
[3] Sherby, O D and Wadsworth, J, "Damascus Steels," Scientific American, Vol 252, No 2, Feb
1985, pp 112-120
[4] SmJth, C S, A History of Metallography, University of Chicago Press, Chicago, 1965, pp 71-85
[5] Smith, C S, A History ofMetallography, Umverslty of Chicago Press, Chicago, 1965, pp 266-280
[6] The Sorby Centenmal Symposium on the Hwtory of Metatlography, C S Smith, Ed, Gordon and
Breach Science Pubhshers, Cleveland, OH, 1963, pp 67-69
[ 7] Gray, R J, Long, E L, Jr, and Rlcht, A E, "Metallography of Radioactive Materials at Oak Ridge
National Laboratory," Apphcatlon of Modern Metallographw Techmques, ASTM STP 480, Amer-
ican Society for Testing and Materials, Phdadelphxa, 1970, pp 67-96
[8] Samuels, L E, MetallographlC Pohshmg by Mechamcal Methods, Pitman and Sons Ltd, Mel-
bourne and London, 1971, pp 23-65
[9] Zlpperlan, D and Mours, M, "Characterizing Advanced Materials," Quahty, Hltchcock Publishing
Co, Carol Stream, IL, March 1990
[10] Gendron, N, "Lapping Produces Smooth Surfaces on MetallographlC Specimens," Metals Engt-
neermg Quarterly, Feb 1973, pp 13 and 14
[11 ] "Lapping Techmques for Mlcrostructural Analysis," Metal Dzgest, Vol 23, No 1, 1984, pp 3-7
[12] Bousfield, B, The New Theory of Sample Preparatton, Buehler, Coventry, U K Internal Commu-
mcation, Aug 1987
[13] Nelson, J A, "A New Direction for Metallography," Practical Metallography, Rlederer Verlag,
GmbH, Stuttgart, March 1989, pp 225-240
[14] Bousfield, B and Dlaz, D, "New Concepts for Specimen Preparation," Mtcrostructural Science,
Vol 17, 1989, pp 203-216
[15] Blann, G, Dlaz, D, and Nelson, J A, "Raising the Standards for Coating Analysis,Advanced Mate-
rials and Processes," Journal, American Society for Metals International, Dec 1989
[16] Nelson, J A and Ahmed, W, "Techniques for Reveahng the Mlcrostructure of Corrosion Speci-
mens," Mtcrostructural Sczence, Vol 17, 1989, pp 217-227
[17] Santayana, G, The Lfe of Reason, C Scnbners and Sons, New York, 1953, p 82
David E. Bell 1 Tern A. Marsico, 2 Kathleen Petrolonts, 1
Paul E. Denney, 3 and Paul R. Howell ~
The Microstructure of Laser-Welded

Aluminum Bronzes
REFERENCE- Bell, D E , Marsxco, T A , Petrolonls, K , Denney, P E , and Howell, P R ,
"The Microstructure of Laser-Welded Aluminum Bronzes," Metallography Past, Present, and
Future (75thAnnlversary Volume), ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M
Purdy, and A Szlrmae, Eds, American Sooety for Testing and Matenals, Phdadelphm, 1993,
pp 327-343
ABSTRACT: Macrophotography, hght microscopy, scanning electron microscopy (SEM), and

transmlssmn electron microscopy (TEM) have been employed to charactenze the microstruc-
tures that develop in laser-welded nickel-aluminum bronze (NAB) The mvestlgaUon has also
documented the mlcrostructures that are present in the base plate prior to welding and has shown
how these latter mlcrostructures change the nature of the heat-affected-zone (HAZ) The weld
zone Is pnmanly martensltlC but also contains proeutectold a (the copper-rich face-centered
cubic (fcc) sohd solution) Small parBcles of a second phase are also present and would appear
to be nickel aluminum (NiAl) In general, the structure of the weld zone is equlaxed although
columnar grams are observed occasmnally m the wcmity of the fusion hne Mixed a/martenslte
and mixtures of a/eutectoldal mlcrostructures develop m the HAZ and these m~crostructures
are strongly influenced by the microstructure of the base plate Finally, in addition to the various
r phases an as yet unidentified phase, which develops as plates on the {111 }~matrix planes, has
been documented
KEY WORDS: mckel-alumlnum bronzes, laser welding, cast material, wrought matenal, micro-
structural analysis, scanning electron m~croscopy, transm~ssmn electron m~croscopy, metallog-
raphy, metallurgical specimens, mlcrostructure, metallographlc techmques
N ~ c k e l - a l u m m u m - b r o n z e (NAB) materials have been used for m a n y years in m a n n e apph-

catmns, and considerable effort has been directed at The Pennsylvania State U m v e r s l t y to the
welding of these bronzes As part of the overall effort, the mlcrostructures that are developed
in laser w e l d m e n t s have been d o c u m e n t e d The results o f this stdl on-going metallographlc
study are presented m this paper Since the focus of these proceedings is on metallography, the
often subtle d~fferences reduced by variations m welding parameters will only be discussed
briefly In the following, the effect of two &sslmllar base plate mlcrostructures (wrought and
cast) on mlcrostructural d e v e l o p m e n t m the heat-affected zone (HAZ) and the w e l d m e n t are
presented It is also shown that there are s o m e striking metallographlc Slmllarmes between
wrought bronzes and hot-rolled hypoeutectold steels
Graduate students and professor, respectively, Department of Materials Science and Engineering, The
Pennsylvania State Umverslty, University Park, PA 16802
2 Research assistant, Department of Materials Science and Engmeenng and The Apphed Research Lab-
oratory, The Pennsylvama State University, University Park, PA 16802
3 Research assistant, The Apphed Research Laboratory, The Pennsylvania State University, Umverslty
Park, PA 16802
327
Copyright
Copyrightby1993
TABLE 1--Alloy composltton (percentby welghO
AI Fe NI Mn Cu
Casting A 9 06 3 91 4 42 1 56 balance
Casting B 10 30 3 67 4 39 0 87 balance
Experimental
Laser Weldmg
Cast and wrought NAB alloys were autogenously laser welded with a continuous-wave car-
bon-dioxide laser The compositions of the two alloys are given in Table 1 Casting A was also
examined in the wrought condition, that is, after it had been hot-rolled in the/3 region The
laser power and welding speed were vaned to produce welds having heat input of 2 0 to 13.8
kJ cm -1
Metallography
Reflected Ltght Mtcroscopy--Cross sections of the weldments were taken transverse to the
welding direction using a water-cooled abrasive cut-off wheel The specimens were then
mounted in bakelite and ground using progressively finer-grit slhcon-carblde papers (240, 320,
400, and 600) using standard metallographlc practices [1]. Rough polishing of the specimens
was performed using 600-grit alumina powder followed by final pohshlng using 0 05-um alu-
mina powder The samples were then etched using either 10-g a m m o n i u m persulfate in 90 ml
of d~stllled water or a mixture containing equal volumes of a m m o n i u m hydroxide, hydrogen
peroxide, and distilled water
Scanning Electron Mwroscopy (SEM)--Speclmen preparation was performed as just
described, with the exception that the samples were purposely overetched to enhance the con-
trast In addition, a line of silver paint from the metal, across the bakelite, to the speomen
holder was used to prevent charging
Transmlsston Electron Microscopy (TEM)--Speclmens were prepared for TEM analysis
using the following steps First, sections approximately 0.4 m m thick were cut from the bulk
alloy using a low-speed diamond-coated wafering saw. Imtlal grinding of the sections was then
performed using 240-grit silicon-carbide paper until the section thickness was approximately
0 08 to 0 1 m m Then, 3-mm-dlameter disks were punched from the section These disks were
ground using 600-grit silicon-carbide paper to a thickness of approximately 0 05 to 0 06 m m
A small circular area at the center of the disk was dimpled to a thickness of approximately 0 01
m m Dlmphng is beneficial since it results in a thin area at the center ofthe disk and it increases
the a m o u n t of electron transparent area obtained after ion beam milling Lastly, the dimpled
areas were ion-beam milled for approximately 8 h with a gun angle of 15* followed by a few
hours at a gun angle of 7 ~ The gun voltage was 3 5 kV, and the gun current was 1 0 mA

Structure IdenUficatlon and the Base Plate Mwrostructures
Macroscopic Exammatlon of the Weldments--Typical macrographs of laser weldments in
the cast material and wrought specimens are shown in Figs 1 and 2, respectively Reference
to Figs 1 and 2 show that
BELL ET AL ON LASER WELDING 329
FIG 1 - - M a c r o g r a p h o~ a ( a s [ r a g B laser ~e/dme~zt (a) heat mpul = 2 8 k l / ( m a n d etchant = 10%

a m m o m u m pet sulfate m dr su/led ~ ate~ a n d (b) heat ml)Ut = 7 5 ],J/~ m a n d et~ hant = 10% a m m o n m m
per~ul/ate :n :h.s:Eled ~ aler
FIG 2 - - M a c r()graph ~ ()[ laset- ~ e l d e d ~vrm~ght p & t e (a) ~,eel ~tWut = 0 2 kd/c m a n d etz k a n t = a m i n o -
m u m hydroxtde-h)'drogen pero~:zde-d~sIE[ea ~,aler, a,~d (b) heal input = 12 5 /&/~m a n d etchant =
a m r n o m u m h) droxlde-h~dro(r pepo_xlde-dlstEled water
1. as the heat input to the weldment is increased, the width of the weld zone also increases;
and
2. there are major differences in the microstructures of the base plate and a "banded"
microstructure is evident in Figs. 2a and b.
To facilitate discussion, a vertical section of the Cu-A1-5Ni-5Fe equilibrium phase diagram is

presented in Fig. 3 (after Cook et al. [2]).
Figures 4 and 5 (light micrographs) are typical examples of base plate microstructures for
Castings A and B, respectively. Figures 4a and b show the presence of large Widmanst~itten
rods of a (the copper-rich solid solution with a ~ 3.64 ,~). This phase can be termed proeu-
tectoid a since reference to the phase diagram of Fig. 3, and the experimental images of Figs.
4 and 5, reveals the presence of a degenerate eutectoid product of a and what is termed the Ki,
phase (see Hasan et al. [2]). The K,~phase has the B2 crystal structure and is based on nickel-
aluminum (NiA1) with a = 2.88 A.
Large rosette/dendritic particles of the K~phase are also present in the images presented in
Figs. 4a and b (the phase identification is due to Hasan et al. [3]). The distribution of the Ki
phase, wholly within single c~grains (for example, see Fig. 4b), or at the junction of several a
grains (for example, see Fig. 4a), could well be indicative that the K~//3interface is a potent
nucleation site for the proeutectoid a reaction. The K~phase is only observed in bronzes of a
relatively high iron content and this might explain the absence of Kiphase in Fig. 5a and b.
1000
900
800
2 700
N 6oo
500
o~+~+w,
400 l 1
8 9 10 11 12
A1, wt.%
FIG. 3-- Vertical section of the Cu-AL5N#5Feequilibrium phase diagram.
FIG 4(a and b )--Lzght mtcrograph ()[NAB cast materml (bage plate) white areas are c~sohd solutzon
whzle dark m e a s are K phase (note dtJferent morphologzes) and etchant = lO g a m m o m u m per~ulfate zn
90 m l o! dtstdled water
FIG 5(a and b ) - - C a s t m g B base plate mtcrostructure, etchant = 10 g a m m o n i u m persulfate in 90 m l

o f dtstEled water
BELL ET AL. ON LASER WELDING 333
The ~ grains in Figs. 4a and b, and to a much lesser degree in Figs. 5a and b contain Kiv
particles that are based on Fe3AI with a = 5.77 A. Fig. 4b shows the presence of Kioprecipitate-
free zones (PFZs) in the vicinity of the eutectoid. This could well be due to preferential parti-
tioning of aluminum to the eutectoidal r,~ phase. Figure 5b contains the last intermetallic
phase, namely, the K, phase (see arrows). These particles display a dendritic-type morphology
and are frequently associated with the eutectoid. The K, phase is based on Fe3A1with a = 5.71
A. Many of the K, particles in Fig. 5b are associated with regions that are "featureless." The
nature of these regions is uncertain at this time although their location (surrounded by the
eutectoid product) might indicate that they are martensitie regions (sometimes called retained
3). Hasan et al. [3] have shown that the martensite has either the 3R or 2H structure. The only
other possibility is that the featureless regions are 3'2. In summary, Fig. 6 (modified from Hasan
et al. [3]) is a schematic diagram of the location of the various phases in the cast weldments.
Figure 7 is an SEM image of the wrought NAB specimen. As demonstrated by the macro-
graphs of Figs. 2a and b, the microstructure is banded and consists primarily of bands of a
together with bands of the eutectoidal mixture of a plus the K,~phase. However, the discrete
precipitates, both at the a grain boundaries and within the a-matrix, could also be the K~vphase.
The image in Fig. 7 bears a marked resemblance to manganese-bearing hypoeutectoid steels
that may yield banded ferrite/pearlite microstructures after hot-rolling and slow cooling from
the austenitic range.
Weld Metal Microstructure and the H A Z

Cast Material--Figure 8 is a light micrograph of the weld zone. Proeutectoid ~ appears to
be outlining the prior 3 grain boundaries and the interior of the grains would appear to be
FIG. 6--Schematic diagram of the morphology and location of the various phases in the weldment of
the cast material.
FIG 7 - - S E M mzcrograph showmg banded ~tructure of the wrought base plate, etchant = ammomum
hydroxtde-hydrogen peroxlde-dtsttlled water
FIG 8--Ltght mzcrograph of an area of the weld zone near the fuslon hne of the wrought NAB matertal
heat mputby=ASTM
Copyright 3 15 kJ/cm and
Int'l (all etchant
rights = 10 Thu
reserved); g ammomum persulJate
Dec 29 00:42:12 EST m 90 ml of dlsttlled water
2011
FIG 9--Light mtcrograph of an area of the fuston hne of the cast NAB material heat mput = 3 15 kJ~
cm and etchant = 10 g ammonium persulfate in 90 ml of dlstdled water
comprised of very fine Widmanstatten a and martensite Further discussion on this point will
be deferred to the section on TEM Figure 9 is a light mlcrograph of the fusion line region,
and a change in morphology from an equiaxed to a columnar structure is noted in the
weldment The HAZ in the vicinity of the fusion line is comprised predominantly of a
and martenslte This zone is relatively narrow, and Fig l0 shows that the K phase soon
develops in the HAZ and mlcrostructures similar to that documented in the base plate are
produced
Wrought M a t e r i a l - - F i g u r e I 1 is a low-magnification SEM image of the weldment, HAZ,
and base plate regions The banding discussed previously is particularly evident in Fig 11 and
persists up to the fusion line Figures 12 through 14 are higher-magnification SEM images of
the region shown in Fig 11 and show the weld metal (Fig 12), the HAZ close to the weld zone
(Fig 13), and the HAZ well removed from the fusion line (Fig 14) tn common with Fig 8,
the weld zone (Fig 12) consists of ct plus martenslte Close to the weld zone, all of the bands
of the eutectoldal mixture ofc~ + K,.,together with a large fraction of each proeutectold a band,
have transformed to 13 on heating and subsequently to martenslte on cooling Hence, the
microstructure consists primarily of martensite bands together with predominantly a bands
FIG 10--Fuszon hne mwrostructure of Castmg B heat mput = 3 15 kJ/cm and etchant = 10 g amino-
mum persulfate m 90 ml of dlstdled water
FIG 1 1 - - S E M mtcrograph of the Ji~slon hne of the laser-welded wrought matertal heat input = 7 7
kJ/cm and etchant = ammomum hydroxMe-hydrogen peroxlde-dlstdled water
FIG l 2 - - S E ~I talc ro~ aph o/an a~ea o~ the ~ eld zone o/lhe la ser-~ e/ded ~ fought mat el m l heat input
= 13 8 kJ/cm and elchan[ = a m m o m u m hvdroY1de-h~ dtogen peroxide-oh slz//ed ~ aler
FIG 13--SEI~I mlcrograpk o f lke t L 4 Z o f the laser welded-wrought materla/ heat mpul = 5 2 kJ/em
and etchanl = amrnomum hydroxide-hydrogen pero:~zde-dtslEled water
FIG 14--SE34 mlcrograph ~howzng the banded strueture o / t h e la.ser-welded wrought material near the
H A Z heat input = 4 5 k J / c m and etchant = a m m o m u m hydroxide-hydrogen peroxlde-dlsttlled water
FIG 15--BF image o f proeutectold a m the base plate
(Fig 13) In regions that have experienced lower peak temperatures (that is, further away from
the fusion hne), the volume fraction of the/3 formed upon heating will be less, and hence httle
of the a bands will transform to/3 upon heating Consequently, on cooling, the bands o f m a r -
tenslte will correspond primarily to the bands of a + K,. that were present pnor to welding as
shown in Fig 14
A Prehmlnary T E M Investlgatton o f the Base Plate and the Weldment
Figure 15 is a bnght-field (BF) image ofproeutectoId a in the base plate The beam direction
for this region is [ 110]~ and a typical [110]~ selected area dlffracUon pattern (SADP) is given
In Fig 16 Analysis of this (and other patterns) yields a ~ 3 64 A Fig 15 shows that
1 a relatively coarse, internally twinned K,vprecipitate is present (this was a c o m m o n occur-

rence), and
2 there is a fine dispersion of plate-like particles on the {111 }. planes
Confirmation for the latter observation is provided by noting that the angle between the two
upright precipitate variants in Fig 15 is approximately 71 ~ In addition, Fig 16 reveals the
presence of streaks m the ( 111 ) directions and m association with the 002 reflections Thus
far, the structure o f these precipitates has not been determined However, using symmetry
arguments, it is likely that they are e~ther tngonal or hexagonal in that they precipitate on the
{111 }~ planes In addmon, it is unlikely that this phase corresponds to that which was unlden-
tiffed in an earlier report by Sahoo et al [4]
Figures 17a and b are centered-dark-feld (CDF) images of the K,, eutectoidal constituent
FIG. 16-- Typical [110]4 SADP of proeutectoid c~in the base plate.
FIG 1 7 a - - C D F tmage o f the K,,, eutectoldal phase m the base plate

FIG 17b - - C D F linage o f the K,,, eutectotdal phase m the base plate
FIG 18--S tDP/tom lhe h,,, parHJe s h o ~ ~,~t~lg 17b
from the base plate, and Fig 18 is an SADP from the particle shown in Fig 17b Analysis of
this, and other patterns yielded results that were fully consistent with the findings of Hasan et
al [3] that is, K., has the B2 structure with a ~= 2 88 A Finally, Fig 19a is a BF image of the
martenslte m the weld pool and Fig 19b is the corresponding SADP At present, both the
details of the martensmc substructure and its exact lattice type and crystal structure are under
Investigation Although not shown in Fig 19a, numerous second-phase particles have been
found m the weldment In light of a previous study [3,4], these are likely to be N1AI
Conclusions
This study has shown that, in common with earher studies [2,3], cast nickel-aluminum
bronzes contain the copper-rich sohd solutmn as Wldmanstatten rods, eutectmd c~ + K,., dis-
crete K. and K,v, and, depending on composmon, large dendritic-rosette particles of K, Con-
versely, the wrought plate consisted almost exclusively of bands of a together with bands of
the eutectoldal m~xture of ~ + K,. The different structures in the two base plates affected the
structure of the respective HAZs Hence, the HAZ for the cast plate was predominantly Wid-
manstatten a and martenslte Conversely, the HAZ for the wrought plate consisted of alternate
bands of a and martenslte, with the width of the martenslte bands increasing as the fusion line
was approached For both materials, the weld zone contained pnmarlly proeutectoid a and
martenslte
Acknowledgments
The authors are grateful to the Applied Research Laboratory, The Pennsylvania State Uni-
versity, for financial support and for the assistance of the Manufactunng Science Research
Facility staffand facilities
FIG 19--(a) BF image o f the martensue m the weld zone, and (b) SADP from the martenslte shown m
Ftg 19a
References
[1 ] 1979 Annual Book of A S T M Standards, Part 11, No 3, Amencan Society for Testing and Matenals,
Philadelphia, 1979, pp 15-71
[2] Cook, M, Fentlmen, W P, and Davis, E, Journal, Institute of Metals, Vol 80, 1952, pp 419-429
[3] Hasan, F , Jahanafrooz, A, Lonmer, G W, and Rxdley, N, Metallurgtcal TransacnonsA, Vol 13A,
1982, pp 1337-1345
[4] Sahoo, M, Edwards, J O, and Thompson, R, AFS Transacttons, Vol 88, 1980, pp 80-125, 769-
776
W i l l i a m J. D. S h a w ~
Metallography of Mechanically Alloyed

Aluminum
REFERENCE Shaw, W J D , "Metallography of Mechanically Alloyed Aluminum," Metal-
lography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Vander
Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing and
Matenals, Philadelphia, 1993, pp 344-362
ABSTRACT: This paper reviews the current state of metallographlc development as applied to
mechanclally alloyed AL 9021 and furthers the understanding of mechanical alloys In general
Also presented is a scanning electron microscope (SEM) technique for accurately and efficiently
determining gram size in this ultrafine-gralned material Considerable skill is required on the part
of the metallographer due to the high magnifications that must be used with the SEM Care must
be taken not to overetch the material, or large errors In grain size measurement will occur Var-
ious etchants were examined and results from the one providing the best detail are described
The effect of overaglng on the mlcrostructure is presented along with the unusual precipitation
reactions that take place The key to gaining a better understanding of the unique structure and
properties of mechanical alloys lies in the use of high magnification metallography
KEY WORDS: mechanical alloys, etchants, gram size determination, internal cracking, shear
ridges, aging, mlcrostructure, mlcrostructural changes, oxygen evolution, microsuperplastlclty,
metallography, metallurgical specimens, metallographlc techniques
A new class of materials k n o w n as mechanical alloys has been around now for a n u m b e r o f
years [1,2] The introduction o f this material was first m a d e in a general way by Benjamin [3-
6] Metallography is playing a m a j o r role in obtaining an understanding o f these continually
evolving materials These materials provide a considerable challenge to the metallurgist when
studying and classifying their mlcrostructure, due to their ultrafine grain size and unusual reac-
tions that take place within the material as a result of the unique processing Both rapid solid-
ification processed (RSP) material and mechanically alloyed (MA) matenals have grain sizes
that would be classified as ultrafine and are usually either submlcrometre, or nanometre, in
their dimensions Thus, due to the magnification limit of the light microscope, either a scan-
nlng electron microscope (SEM) or a transmission electron microscope (TEM) must be used
for most studies o f the mIcrostructure of these materials
The production of mechanclal alloys is centered in the grinding technique that is employed
in altering the structure o f the alloy materials V a n o u s elements are c o m b i n e d in a high-
energy-attrition grinding mill where they are processed for long periods of time The energy
input during processing is greatly in excess o f what would normally be required for regular
grinding of the material The key to the process is a balance of a cold weld/fracture m e c h a n i s m
that provides a mechanical mixing that eventually results in an extremely stable and fine-
grained material The powder particles that are m a d e using this process are very h o m o g e n e o u s
with a distribution of various elements mechanically mixed throughout each powder particle
Professor, Department of Mechanical Engineering, University of Calgary, Calgary, Alberta, Canada

T2N IN4
344
Copyright
Copyright*by1993
ASTMbyInt'l
SHAW ON MECHANICALLY ALLOYED ALUMINUM 345
D u n n g this processing, many interfaces are formed between the various subgralns within each
powder particle It is these interfaces, along w~th the ultrafine-grained structure, that give
mechanical alloys the specml charactenstics that cannot be achieved from any other processing
technique In a l u m i n u m alloys, oxygen ~s incorporated into the material as a result of origi-
nally exposing the alloy materials to the atmosphere In addition, carbon (or more likely
hydrocarbon) is also incorporated into the material due to the presence of steanc acid that is
used to control the cold weld/fracture balance
Once integral and stable mixing of the various elements has taken place w~thm each powder
particle, the attrition milling process is stopped The powder is collected and subsequently con-
solidated using conventional powder metallurgical techniques The material is consohdated
well below its melting temperature under the influence of pressure and temperature, resulting
m a solid-state reaction at the v i n o u s particle interfaces After consohdat~on, the matenal is
often processed using thermal methods to enhance its overall property characteristics Thus,
aluminum-copper mechamcal alloys are solution-treated and quenched to take advantage of
precipitation hardening
Generally, MA a l u m i n u m has extremely high strength and good ductility combinations and
~s very creep resistant as compared to other a l u m i n u m alloys The a l u m i n u m alloys made by
the mechanical alloying process show some very unusual charactenstics and are, for the most
part, thought to be metastable materials Properties that have been incorporated due to the
mechamcal alloying process will be lost if melting occurs.
The AL 9021 matenal used in this study has a chemical composition as shown In Table 1
This composition is analogous to 2024 ingot metallurgy a l u m i n u m alloy except for the quan-
tities of oxygen and carbon, or hydrocarbon, that have been incorporated d u n n g processing
At the present nine, ~t ~s not known exactly how the oxygen and carbon, or hydrocarbon, are
bonded within the matenal This is an area where work is continuing
The work described herein both presents new reformation and reviews an accumulation of
reformation obtained while studying this material--first for its microstructure and then for a
more general understanding with respect to the mechanical alloying process The techmques
described m this paper, even though specifically directed at AL 9021, should be apphcable to
other MA a l u m i n u m alloys and also to some RSP a l u m i n u m alloys
Grain Size Determination

One of the major difficulties in studying MA a l u m i n u m is in determining the grain size of
the matenal A c o m m o n techmque that has been used in this regard is the employment of
TEM microscopy with the use of thin foils A number of researchers have used this technique,
not only to determine grain size but also to investigate particle Interaction and general micro-
structure [7,8] This is a difficult and nine-consuming technique that requires the use of a
TEM Large areas must be prepared and stud~ed if representative grain sizes are to be deter-
mined This is difficult to do by TEM A better technique employs the SEM and is descnbed
herein
Using conventional metallographlc specimen preparation techniques of grinding, polishing,
and etching, component sections were prepared and examined with the SEM Figures 1a and
b show the grain size for AL 9021 a l u m i n u m alloy at two different magnifications It can be
TABLE l--Chemical composltton orAl 9021 (percent by weight)
Cu Mg C O $1 Fe Mn Cr Zn Al
40 15 11 08 005 002 001 001 001 balance
FIG l--(a) S E M mtcro<~raph, gram size o / A L 9021 aluminum alloy, Keller's reagent wtth wetting
agent (b) Higher magndTcatton SEM mtccograph, gram and s'ubgram ~tze
seen in Fig 1b that approximately 0 18 um is an average gram size However, th~s figure also
shows a subgram size of 0 02 um The question then becomes whether the actual gram size ~s
the small subgraln parhcles that are shown or the larger accumulations of apparent grams At
this t~me, ~t ~s thought that the small subgram particles are interfaces between various elements
that develop dunng the mechanical alloying process The larger gram parhcles are hkely rater-
faces between the final powder particles o c c u m n g dunng consohdatlon This has yet to be
proven conclusively
A major error can occur when using the SEM for determlnmg an accurate value for gram
size in these materials This is because the materials are attacked unevenly and a smoothing
or masking of actual gram boundaries occurs Figure 2 shows an overetched condition where
the apparent gram size ~s now about 0 30 um This figure should be compared with Fig la as
both are at the same magmficatlon for the same material condmon Thus, ~t can be seen that
overetchmg can lead to large errors in the measurement of the overall gram size of the material
as well as masking the subgram size It is possible that this same phenomenon might occur
when making TEM thin fods where uneven attack can preferentially dissolve the smaller gram
sizes leaving an apparent larger-graln-sxzed material
In order to obtain an accurate gram s~ze determination m MA aluminum, a careful process
of controlled etching must be carried out Materials should be examined m an unetched con-
dmon, followed by incremental controlled amounts of etching until an optimum etched con-
d m o n has occurred whereby the gram size and subgralns are clearly visible, but prior to an
enlargement of the apparent gram sizes o c c u m n g due to overetchmg condmons If this pro-
cedure is carefully adhered to, then SEM m~croscopy ~s a fast, efficient, and accurate way of
determining the gram size of these materials
In order to obtain good gram s~ze measurements, SEM microscopy must be conducted on
FIG 2 - - S L M rmcrogpaph, apparent gram stze A L 9021 a l u m i n u m alloy/or an overetched ~ondttlon,

Keller's reagent ~r ~etHng agent
this MA aluminum at magnifications between 20 and 60 thousand times These high magni-
fications require a finely tuned SEM, the utilization o f a short working distance and enhance-
ment of the surface for conductivity by using sputter-coated gold or gold-palladium The sput-
ter coating makes the etching technique more difficult as, once the component is etched and
sputter coated, it cannot be re-etched without going back and repollshlng the surface Thus,
the best technique is to etch the component and examine it in the SEM prior to sputter coating
Once a reasonably etched condmon has been obtained, then sputter coating should be carried
out prior to attempting to measure the gram size at the high magnifications
Etchants
As with any new material that becomes available, the investigation and development of
etchants that yield the best results is a necessity
A number ofetchants have been evaluated for the AL 9021 material These include a hydro-
fluoric etchant and a sodium hydroxide etchant as well as Keller's reagent [9] In addition, two
relatively new etchants developed for powder metallurgical materials were also tried, an etch-
ant by Graft and Sargent [10] and an etchant developed by Campbell [11] These etchants
have also been evaluated in a slightly m o d i f e d form by incorporating a wetting agent, sodium
trldecylbenzene sulfonate, at 1 g/100 ml of solution Wetting agents were first suggested by
Cohen et al [12] and have been used throughout the years [13-15], primarily on martensltlC
steels The importance of using a wetting agent with an MA material is to enhance attack of
the fine features that are present The wetting agent ensures that a better attack occurs along
the grain and subgraln boundaries
Keller's reagent (with a wetting agent) has been found to be the most satisfactory etchant,
producing the best delineation of the grain boundaries and subgrain boundaries Normal etch-
ing times are fmrly short, on the order of 10 s providing good grain-size delineation Campbell's
etchant is a close second but has a shght tendency to pit and results in larger amounts of local
attack The Graffand Sargent etchant caused extensive plttlng attack of AL 9021
Propensity to Internal Cracking

Mechanically alloyed aluminum has a tendency towards internal cracking that is a direct
result of the unique interfaces that are formed within the material The interface boundaries
also evolve oxygen that adds to the cracking problem (discussed later) Some of these materials,
when processed by forging after consolidation, exhibit small internal cracks Accumulations
of these small internal cracks can usually be seen by light microscopy, as shown in Fig 3 This
mlcrograph shows what appears to be stringer inclusions on the short transverse plane of the
billet material However, the limits of the light microscope prevent full analysis and SEM
microscopy must be utilized to identify these apparent stringer inclusions Thus, Fig 4 shows
a typical internal crack that was likely formed dunng the latter stage of processing Due to the
good ductlhty and reasonable fracture toughness of the material, these internal cracks are not
particularly damaging under slow tensile loading conditions but rather allow extra absorption
of energy This propensity towards cracking can be seen on an overload fracture surface from
atensllespeclmen, Fig 5 A number oflnterlorcrackswereelther present orlglnallyor formed
along planes of weak bondmg due to the Poisson's effect during the loading process These
features are known as "shear ridges" [16] This fracture mechanism has a tendency to form in
MA aluminum under all types of loading conditions such as stress corrosion cracking, fatigue,
and creep, as well as tensile tearing and tensile overload conditions
FIG 3 - - L t g h t mlcrograph, stringer cracks" on the short transverse plane m A L 9021 aluminum alloy,
Keller "s reagent
FIG 4 - - S E M mtcrograph, ~trmger cracks' on the shorl transvo ~e plane zn A L 9021 aluminum alloy,
unetched
FIG 5 - - S E M fractograph, ~hear ridges on a tensile overload component o/AL 9021 aluminum alloy
t80
AL 9 0 2 t - T 4 5 2 ALUMINUM ALLOY
t60 _ o A S RECEIVED
-lr
- ~ WATER QUENCHED -'j~'O
AGED t WEEK AT 20 ~ C
440 -
o
O
od
t 4 8 4 HRS NORMALIZED
(/3
t20
ILl
Z
a
n,"
O AS RECEIVED
:z: 400 a (AiR)
A CREEP (HRS)
0 QUENCHED (WATER)
I i I I I = l = I 1
800 t00 200 300 400 500 6OO
AGING TEMPERATURE (~
FIG 6--Relattonshtp of hardness versus heat-treatment condttton
Microstructural Changes Due to Aging

Complex relatlonshxps occur in this material due to various aging condlUons The overall
behavior is shown in Fig 6 that relates the hardness of the material to various aging condmons
of time and temperature Also incorporated on this figure are some data from creep tests and
a normahzed condlUon from solution treating and air cooling Most of the points on the graph
are a result of aging for 1 h and furnace cooling Generally, the material softens as the com-
ponent is aged or overaged from an optimum T452 con&tlon that corresponds to the as-
received material A mm~mum hardness condition occurs at approximately 380~ Beyond
this, there is a sudden increase and then a continual decrease in hardness up to a point
approaching the melting point of the material Material that is solution-treated and water-
quenched at 543~ and then naturally aged at room temperature for one week, approaches the
same hardness c o n d m o n as the original material Thus, for most practical purposes, the mate-
rlal, even though being metastable, appears to be completely reversible with respect to the var-
ious precipitation reactions that are taking place d u n n g the aging process
As aging progresses, a general coarsening of precipitates develops, resulting m a number of
&fferent preclpxtatlon mechamsms occurring within the material As the coarsening becomes
pronounced, regular light microscopy can be used to examine the mlcrostructures Long-term
aging at 200~ for 2339 h resulted m a precipitation ennched mlcrostructure, as shown in Fig
7 If the material is aged at 360~ for a period of 1 h, then the precxpltates coarsen by diffusing
to select areas within the material, as shown in Fig 8 Long-term aging con&tlons at lower
temperatures, or longer times at elevated temperatures, result in considerably greater coars-
ening, as shown in Fig 9 This m~crograph represents a con&tlon of 400~ for 1484 h The
black appeanng particles in this mlcrograph are, in fact, voids as confirmed using SEM
microscopy
FIG 7--Light mlcroglaph, creep component of 4L 9021 alummurn alloy, 200~162 2339 h, Keller;
teagent
FIG 8--Ltght mtcrograph, AL 9021 aluminum alloy aged 1 h at 360~ then furnace cooled, Kelh,r's
reagent
FIG 9--Light mtcrograph, creep component of AL 9021 alummum alloy, 400~ for 1484 h, Keller's
reagent
FIG lO--(a) Ltght mwrograph, rod-hke prectpttates m AL 9021 alummum alloy, agedJor 1 h at 5950~
and /urnace cooled, Keller's reagent (b) Enlargement
The very large grey precipitates were found to consist of approximately 50% copper with
traces of zinc and iron and a relatively high content of carbon, or hydrocarbon, with the
remainder being a l u m i n u m This analysis was obtained using energy-dispersive spectrometry
(EDS) conducted on gold sputter-coated samples The count rate at which the X-rays accu-
mulated was compared between gold and a l u m i n u m A slow accumulation of aluminum, with
reference to the gold, indicated a presence of carbon in the analyzed matenal This technique
resulted in a relative comparison between these two elements and allowed a rough determi-
nation of the a m o u n t of carbon, or hydrocarbon, present at any location The smaller, grey-
colored second-phase particles were found to consist of approximately 20% copper with a
small a m o u n t of carbon and the remainder being a l u m i n u m Thus, as normal aging takes
place, the m a t n x becomes leaner in copper at the expense of an accumulation of copper in the
precipitates At a temperature above 380~ an interaction of oxygen within the matenal
occurs It is believed that th~s general interaction initially results m the higher strength of the
matenal due to the formation of some a l u m i n u m oxides The oxygen reactions will be dis-
cussed later
When the material was heated to 595~ a new reaction suddenly occurred, resulting in a
rod-like precipitate phase as shown in Fig 10a This light mlcrograph shows the random dis-
tribution and relative density of these rod-like precipitates An enlarged mlcrograph of these
precipitates is shown m Fig 10b The EDS analysis showed their composition to be 30% cop-
per, 15% iron, a medium a m o u n t of carbon, or hydrocarbon, and the remainder a l u m i n u m
The matrix matenal changed, becoming very low m copper, ~ron, and carbon or hydrocarbon
It reverted primarily to a solid solunon of a l u m i n u m and magnesium These rod-like precip-
itates are fairly strong, as suggested by Fig 11, where it can be seen that a rod ~s bndgIng a
crack that has occurred m the material due to sudden heating and gas evolution creating gas
porosity pockets
FIG 11--SEM ml~ rograph, rod-hke preupllates m A L 9021 alummurn alloy brtdgmg a ga~ void, aged
595~ 1 h m a saltpol a n d a l l ~ooled
For highly aged materials, light microscopy IS totally satisfactory for the study and analysis
of mlcrostructures in this MA material Examination of material that has been treated at tem-
peratures as high as 595~ and water quenched shows that the hardness is similar to that of
the as-received material This indicates that the strengthening mechanism is reversible Even
though the material is metastable, it IS essentially a reversibly metastable material almost up
to its melting point
Oxygen Evolution
Most researchers believe that the oxygen within the material is tied up as a l u m i n u m oxide
and that the carbon is in the form of a l u m i n u m carbide In fact, some Investigators have lden-
tiffed a l u m i n u m oxide and a l u m i n u m carbide from TEM studies [17,18] However, the major
amount of oxygen within the material is not bonded as a l u m i n u m oxide Rather, it is tied up
in some low bond energy reaction that allows oxygen to evolve from the material once heating
occurs This oxygen evolution reacUon has been identified by Shaw [lP] The phenomenon
was found originally when mvesUgatmg attempts at welding this MA aluminum [20] These
effects can be seen in Figs 12 and 13 Figure 12 shows the large amount of porosity that has
resulted from gas evolution from within the material d u n n g the fusion process resulting in a
totally inadequate weld Figure 13 shows porosity from gas evoluuon that has taken place
below the fusion hne back into portions of the material that have not experienced melting
Thus, it is apparent that a general evolution of gas out of the material at some temperature
well below the melting point temperature of the material has occurred
The overall extent of gas evolution ~s probably best appreciated when viewing Figs 14a and
b These figures show the before and after effect of heating a small block of AL 9021 material
at a temperature of 600~ for approximately 1 h This block of material was immersed m a
salt pot maintained at this temperature and removed at the end of the l-h period. It was then
FIG 12--Light macro~eraph TIG /usIon weld end m AL 9021 alurnmurn alloy, unetched
FIG 13--SEM mzcrograph, weld poroslO near ]usmn hne m AL 9021 aluminum alloy, unetched
cut open As can be seen, the gas evolution in the matenal occurred in a manner such that the
matenal expanded approximately 300% m one direction but very little m the other direction
The material is full of gross porosity due to the evolution of gas, and this gas has been identified
as bemg primanly comprised of oxygen with small trace amounts of hydrogen, nitrogen, and
methane [19] Thus, sudden immersion at high temperatures near the melting point of the
material results in considerable and quick evolution of gas out of the base material
Examination of a polished and etched surface from material that has been quickly heated
under vacuum conditions in a sealed glass envelope revealed a crack network and Internal void
formation, as shown in Fig 15 This mIcrograph shows that networks of cracks formed
throughout the material, linking the voids and allowing gas passage and accumulation in local
areas within the material Since the material was at a high temperature, It crept and flowed
under the internal gas pressures allowing the creation of large internal voids It has been estab-
hshed that this oxygen evolution out of the matenal with internal cracking starts to take place
at approximately 380~ with times exceeding 1 h Thus, internal damage is accumulated in
the material when exposed to temperatures in this region The strong evolution of oxygen at
elevated temperatures is a major drawback of this material
Microsuperplasticity
A very unusual and distinct mechanism occurs in MA aluminum as well as in other RSP
aluminum This mechanism is known as "mlcrosuperplastlclty" [21] and has been described
in detail elsewhere [22] The mlcrosuperplastlc mechanism is one of high creep resistance
resulting in creep life many orders of magnitude greater than would normally occur in con-
ventional aluminum alloys The final outcome of this creep life is the formation of the micro-
FIG 14--(a) M a ~ ograph o/ A L 9021 aluminum all,o: aged m salt pot jor I h ~ompared to mmal spec-
imen slze (b) lnwrmr se~tton
FIG 15--SEM mlcrograph, AL 9021 aluminum alloy reduction heated under vacuum, mtemal void
/ormatlon and crackmg network, Keller's reagent with wetting agent
superplastlc fracture features at the instant of separation A typical fractograph of the creep
crack growth surface ~s shown in Fig 16 where the mlcrosuperplastloty is apparent This is an
environmental phenomenon that is promoted by the presence of oxygen [23] The base of a
mlcrosuperplastlc bundle is shown in Fig 17 The size of the fiber diameter IS extremely small
and a few grains contribute to the superplastic behavior taking place on a m~croscoplc scale
Individual grains can be seen surrounding the base of the fiber bundle Generally, the fibers
are of the same order of magnitude as the grain size of the material This means that normal
superplast~c mechanisms of grain boundary sliding do not take place to any significant degree
with the development of this mechanism Sudden heating of the material results in immediate
evolution of oxygen and gas pocket formation, which can also result in a coarse mlcrosuper-
plastic formation within the material, as shown by the mlcrograph in Fig 18
The understanding of the mlcrosuperplastlc mechanism and the high degree of creep resist-
ance that occurs within these local regions will likely be forthcoming from future detailed anal-
ysis of the mlcrostructures m these select locations The material exhibits extremely high creep
resistance in a few local regions where this resistance continues to build until an unstable con-
dltlon suddenly develops and the component separates The mechanism resulting in a high
degree of resistance to creep propagation is not presently known It is known that oxygen,
being supplied from within the material as well as from the external environment, is playing
a major role
Discussion
Metallographic analysis of MA a l u m i n u m presents a challenge to metallographers as a result
of the ultrafine structure of the material and the unusual behavior that occurs w~thln the mate-
rial Since etchants attack the material unevenly, likely due to the microgalvanlc effects of con-
FIG 1 6 - - S E M fractograph, mtcrosuperplastlctty on a creep crack growth surface o f A L 9021 aluminum

alloy tested m an air envtronrnent at a temperature o f 400~
centrations of different elements within the grams, a great deal of care must be maintained in
order to properly identify grain-size and subgraln structure This means that the material must
be carefully examined initially with respect to underetching, optimum etching, and overetch-
lng conditions for the metallographer to estabhsh the proper etching condition It has been
shown that a SEM technique of determining grain size can be conducted quite efficiently with
a lot less effort than that involved in making thin foils and using a TEM Additionally, the
advantage of using SEM microscopy is that large areas of material can be examined leading to
more representative grain-size determination.
A n u m b e r of etchants have been examined and the best etchant found to date for giving
good dehneat~on of grain boundaries and subgram boundaries is Keller's reagent modified
w~th the use of a wetting agent Due to the ultrafine structure of MA materials, as well as rapid-
sohdlfiCatlon-processed material, it is felt that a wetting agent considerably enhances the fine
details of the structure during etching It is recommended that this technique be evaluated for
all ultrafine-gralned structures
Due to the propensity for internal cracking as well as gas evolution out of the material, the
SEM is by far the best tool to identify voids and cracks that have formed on a small scale within
the material Thus, damaged condmons present in the material from overheating, incorrect
heat treatment, etc, can be readily ~dentified using SEM m~croscopy
FIG 17--SEM[ractograph, base o[ mlcrosuperplastu bundle m A L 9021 aluminum alloyJor a creep

cra~k growth component tested at 400~
FIG 18--SEM mtcrograph, coars'e mtcrosuperplastlu& m an internal votd formed from gas release
caused by sudden heatmg at 620~ in AL 9021 alummum alloy, unetched
The high creep resistance of the MA materials and the resulting mlcrosuperplastlc forma-
tion has opened up another area of metallographlc study since understanding of what is occur-
n n g in these areas is incomplete. Once understood, it will likely be possible to better utilize
this p h e n o m e n o n over larger portions of the material This understanding will likely be forth-
coming from future metallographlc work conducted on these materials
Generally, light microscopy can only be used on this material when substantial amounts of
overagmg have occurred and the precipitates have coarsened to the point where they become
visible with the light microscope The hght microscope can also be used In a limited way as a
quahty control tool for determining whether or not large amounts of processing cracks are
present in the material
Microscopy of these materials is particularly demanding and even more care than usual
must be taken in the preparation and use of microscopic techniques
Conclusions
A qmck and relatively easy-to-use SEM technique has been described for the determination
of grain and subgraln size for ultrafine-gralned materials
Care must be taken when using this technique to ensure that overetchlng does not occur, or
the apparent grain size will increase substantially from that of the true grain size of the
material
The best etchant, of those evaluated, for use on MA a l u m i n u m is Keller's reagent with the
addition of a wetting agent
The overall degree of internal cracking within the material from processing can be evaluated
using light microscopy as a general quality control tool
The small mlcrocracking damage within the matenal due to oxygen evolution can only be
evaluated using scanning electron microscopy
Considerable work needs to be conducted on the metallography and mlcrostructural rela-
tionships associated with microsuperplasticity in order that the creep properties of the material
can be understood
Acknowledgments
The author is grateful to the University of Calgary and to the Natural Sciences and Engl-
neenng Research Council of Canada for financial support of this work
References
[1] Alexander et al, U S Patent No 2 972 529, 21 Feb 1961
[2] Anders, F J, Jr, U S Patent No 3 159 908, 8 Dec 1964
[3] BenJamin, J S, "Dispersion Strengthened Superalloys by Mechanical Alloying," Metallurgtcal
Transactions, Vol 1, 1970, pp 2943-2951
[4] Benjamin, J S and Vohn, T E, "The Mechanism of Mechamcal Alloying," Metallurgwal Trans-
actions, Vol 5, 1974, pp 1929-1934
[5] Benjamin, J S, "Mechamcal Alloying," ScwnttficAmencan, Vol 234, 1976, pp 40-48,
[6] Gilman, P S and Benjamm, J S, "MechamcalAlloymg,"AnnualRevwwofMaterlalsSctence, Vol
13, 1983, pp 279-300
[ 7] Stager, R F, Ohver, W C, and Nix, W D, "Identification of Dlsperso~d Phases Created m Alu-
minum Dunng Mechamcal Alloying," Metallurgwal Transactions, Vol 11A, 1980, pp 1895-1901
[8] Kam, Y-W and Bldwell, L R, "Tensile Behavior of a Mechamcally-Alloyed AI-4 0Mg Powder
Alloy," Scrtpta Metallurgical, Vol 16, 1982, pp 799-802
[9] ASM Metals Handbook, 8th ed, Vol 8, 1973, p 124
[10] Graft, W R and Sargent, D C, "A New Gram Boundary Etchant for Aluminum Alloys," Metal-
lography, Vol 14, 1981, pp 69-72
[11] Campbell, J B, "An Advance in Powder Metallurgy Aluminum Alloy Etchants," Metallography,
Vol 18, 1985, pp 413-420
[12] Cohen, J B, Hurhch, A , and Jacobson, M , "A Metallographlc Etchant to Reveal Temper Bnttle-
ness in Steel," Transacttons, American Society for Metals, Metals Park, OH, Vol 39, 1947, pp 109-
138
[13] Dreyer, G A , Austin, D E, and Smith, W D , "New Etchant Bnngs Out Gram Boundaries m
Martens~tlC Steels," MetalProgress, Vol 86, No 1, July 1964, pp 116-117
[14] Karl, A and Boehmert, H , "Eanlge Praktlsche Hlnwelse zur Makroaetzung und Aetzmlttel zur
Makroskop~schen Untersuchung yon Staehlen," Prakttsche Metallographte, Vol 4, No 10, Oct
1967, pp 529-540
[15] Nelson, J A , "Use of Wetting Agents an Metallographlc Etchants," PraktlscheMetallographle, Vol
4, No 4, April 1967, pp 192-203
[16] Shaw, W J D , "Fracture Toughness of IN-9021 Aluminum Alloy," Metallography, Vol 18, 1985,
pp 405-412
[17] Kang, S K , "The Mlcrostructure of Mechamcally Alloyed Aluminum Alloys," American Society
for Metals, Metals Park, OH, Paper 8305-051, 1983, pp 1-10
[18] Gdman, P S and Nix, W D , "The Structure and Properties of Aluminum Alloys Produced by
Mechamcal Alloying Powder Processing and Resultant Powder Structures," Metallurgtcal Trans-
acttons, Vol 12A, 1981, pp 813-824
[19] Shaw, W J D , "Gas Evolution and Analysis from Mechamcally Alloyed IN-9021," Materials Let-
ters, Vol 6, No 3, 1987, pp 75-79
[20] Shaw, W J D , "Weldablllty of IN-9021 Aluminum Alloy," Mtcrostructural Sctence, Vol 14, 1987,
p 17-27
[21] Shaw, W J D , "Mlcrosuperplastlc Behavior," Materials Letters, Vol 4, No 1, 1985, pp 1-4
[22] Shaw, W. J D , "The Role of Mlcrosuperplastlc Flow in High Temperature Fracture of AL-9021
Mechanically Alloyed Aluminum," Journal of Materials Science Letters, Vol 24, 1989, pp 4114-
4119
[23] Shaw, W J D , "Mlcrosuperplastlc~ty in Aluminum Alloys," Proceedings, Symposmm on Hot
Deformation of Aluminum Alloys, The Minerals, Metals, and Materials Society, Oct 1990, pp
277-296
[24] Shaw, W J D and Rowell, R E, "Mlcrostructure and I~netlcally Induced Changes m a Mechan-
ical Alloy," MlcrostructuralSctence, Vol 16, 1988, pp 349-360
Kevin L. Zetk, ) Iver E. Anderson, 2 Donald A. KOSS, 3 and
Paul R. HowelP
Microstructural Investigations of Rapidly

Solidified Copper-Niobium (Cu-Nb) Alloy
Powders Produced by Inert Gas Atomization
REFERENCE. Zelk, K L, Anderson, I E, Koss, D A, and Howell, P R, "Microstrueturai
Investigations of Rapidly Solidified Copper-Niobium (Cu-Nb) Alloy Powders Produced by Inert
Gas Atomization," Metallography Past, Present, and Future (75th Anmversary Volume), ASTM
STP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amencan
Society for Testing and Materials, Philadelphia, 1993, pp 363-371
ABSTRACT: This study presents a metallographlc techmque that enables the mlcrostructural
examination of the cross-sections of individual, fine-scale (10 to 75 urn) powder particles The
technique was developed to permit characterization of the "as-solld~fied" features of copper-
based powders produced by high-pressure inert gas atomlzatmn (HPGA) in order to relate the
microstructures to processing history In order to perform the necessary microscopy to elucidate
the mIcrostuctural features, a metallographlc technique was developed to permit characteriza-
tion of the "as-atomized" mlcrostructures within the individual powder particles This techmque
revolved classifying, mounting, and pohshlng through the diameters of individual powder
particles and then using an "attack etch" to remove some of the copper matrix This enabled
characterization of the mobium-nch second phase Secondary electron imaging on a scanmng
electron microscope provided the necessary resolution to characterize the second phase mor-
phologies as a function of powder-particle size, ultimately relating the microstructures to pro-
cessmg condmons
KEY WORDS: metallography, copper-niobium alloys, high-pressure gas atomization, rapid

sohdlfication, powder metallurgy, metallurgical specimens, mlcrostructure, metallographlc
techniques
Rapid solidification processing has received increased attention as a method of producing

materials that may exhibit significant improvements in properties over their conventionally
cast counterparts In general, rapid solidification processing results in the generation of fine-
scale microstructures containing both stable as well as metastable phases Thus, metallo-
graphic techniques are needed that readily permit the characterization of the fine-scale micro-
structural features within rapidly solidified alloys
The present study introduces an "easy-to-use" metallographic procedure performed on
multiphase, copper-based powder particles in order to elucidate the fine-scale mIcrostructural
Senior research engineer, U S Steel Group, Unit of USX Corporation, Monroevdle, PA 15146, for-
mer graduate student with The Pennsylvania State University
2 Staffmetallurgist, Ames Laboratory, The Iowa State Umvers~ty, Ames, IA 50011
3 Professor of Metallurgy and department chmr, Department of Materials Science and Engmeenng, The
Pennsylvania State Umverslty, Umverslty Park, PA 16802
4 Professor of Metallurgy, Department of Materials Science and Engmeenng, The Pennsylvania State
University, Umverslty Park, PA 16802
363
Copyright
Copyrightby1993
features This procedure, which is demonstrated using high-pressure gas atomized (HPGA)
copper-niobium-molybdenum (Cu-Nb-Mo) alloy powder, should apply to a range of other
alloys, in both bulk and powder form
Experimental Procedure
Material
The Ames Laboratory High Pressure Gas Atomizer (HPGA) has been used to produce rap-
idly solidified, ultrafine Cu-21 2Nb- 1 8Mo (percent by weight) powder pamcles that ranged in
size from < 2 um to 100 um in diameter Details of the atomization procedure are described
elsewhere [ 1 ]. The powders produced were mainly spherical up to a diameter of approximately
63 urn, above which, some surface irregularities became apparent
Metallographtc Preparatton Techmque

In order to evaluate the mlcrostructural details of the rapidly sohdified powder pamcles and
relate those details to particle size, a technique was developed that permitted cross-sectioning
and etching of the individual powder particles Since the mlcrostructures of the powders
depend on particle size [2], a key step was to first classify the powder into several distinct and
narrow-size categories To accomplish this, the powder was hand-sieved using 7 6-cm (3-in.)
diameter, stainless steel sieves with openings of 63, 45, 38, 25, 20, 15, and l0 #m (the last four
sieves have not been accepted by ASTM as standard sizes) This operation was performed
inside a controlled-atomosphere glove box to prevent contamination from moisture that could
cause excessive agglomeration of the fine particles and prevent accurate sieving
In order to obtain cross-sectional views of individual powder particles without disturbing
the mlcrostructural details, the seven, narrow size classes of powders were mounted in epoxy
Since cross-sectioning was accomplished simply by polishing through the diameters of indi-
vidual powder particles, it was necessary to mount the various sizes separately in order to
ensure which powder size was being observed, as demonstrated by the schematic diagram pre-
sented in Fig l a To accomplish this, a small (0 5 to 1 0 g) sample of each size class of powder
was first blended with two or three drops of epoxy (Struers Epofix or equivalent) This pro-
duced a thick slurry that was then placed into the bottom of conical embedding capsule, 5 m m
diameter by 15 m m long. This capsule was then carefully backfilled with additional epoxy in
order to maintain the concentration of powder at the tip of the conical end, Fig lb Once
cured, these samples were removed from the plastic capsule and subsequently placed into the
center of a standard 2 54-cm ( l - i n ) diameter metallographic specimen mold Again, epoxy
was used to fill each of these molds As a result, this procedure produced metallographic
mounts that contained a small area with a substantial concentration of a narrow size-class of
"as-atomized" powder, see Fig 1b
The cross sections of the powder particles were exposed by carefully polishing each of the
specimen mounts with progressively finer silicon-carbide papers (240 to 600 grit) using dis-
tilled water as the lubricant/coolant and then, with progressively finer diamond compounds
(15 to 0 25 ~tm) using kerosene as a lubricant This technique generated a number of cross-
sectional views by simply polishing through the dense field of powder particles of a given, nar-
row size distribution For statistical precision, this polishing technique was repeated after the
first set of metallographlc analyses were completed in order to produce an additional set of
cross sections within the same powder size distribution
To determine the volume fraction of the mlcrostructural phases within the Individual pow-
der particles, backscatter electron imaging on a scanning electron microscope was performed
ZEIK ET AL. ON POWDER METALLURGY 365
FIG. 1--(a) Schematic drawing demonstrating the possible error involved when cross-sectioning
through a large size distribution of powder particles. Note that the cross-section diameters may be similar
depending on particle location, (b) Schematic'drawing of the specimen mounting procedure used to produce
a concentrated area of a narrow size range of powder particles.
on the as-polished surfaces. Since the atomic numbers of niobium and copper differ substan-
tially, good contrast was obtained using this technique. This enabled microstructural features
such as the volume fractions of the niobium-rich phases to be determined using standard ste-
reological techniques.
In order to determine the size, morphology and distribution of the niobium-rich phases as
a function of powder size, the copper-rich matrix surrounding these discontinuous features
was chemically dissolved This was accomplished by a two-step process First, each sample was
immersed for l0 to 20 s in a solution of 20% HF, 20% H2SO4, 20% HNO3, and 40% H20 in
order to remove any smeared niobium created during sample polishing Second, to remove
the copper matrix surrounding the niobium-rich phases, each sample was immersed subse-
quently into a solution of 30% H3PO4, 15% CH3COOH, 10% HNO3, and 45% ethyl alcohol
This etchant, previously used to delineate mlcrostructural features within chill-cast Cu-Nb
alloys [3], has been modified to promote slower, more uniform dissolution of the copper
matrix In order to further promote homogeneous removal of the copper matrix, the sample
and etchant were placed into an ultrasonic cleaner The duration of this stage of the etching
process varied from 30 s to 3 mln, depending on the age of the solution and the amount and
distribution of niobium present Once the sample was removed from the etching solution, it
was quickly placed into fresh, ultrapure l, 1,1 trichlorotrifluoroethane and agitated in the ultra-
sonic cleaner for 1 mln to remove all traces of the etching reagents Ifprehmlnary examination
under a light microscope revealed that additional matrix material had to be removed in order
to elucidate the second-phase features, the etching procedure was repeated (15 to 30 s
intervals)
The morphological features of the niobium-rich phases were then documented using an ISI
SX-40A scanning electron microscope operating in the secondary electron imaging mode To
enhance this imaging, each sample was sputter-coated with a thin layer of gold prior to
examination
The Cu-21 2Nb-1 8Mo alloy system, processed by HPGA, is a good system to demonstrate
the preceding metallographic technique in that significant differences in microstructure exist
within the size range of powders produced, as summarized in Table 1 [2] The "large" pow-
ders, classified herein as those particles between 45 and 75 um in diameter, exhibited a micro-
structure that is typified by Fig 2 The niobium-nch phase is present as fine-scale ~ 4 um den-
dntes (stalk diameters of 0 3 to 0.5 urn) distributed within the copper matrix The volume
fraction of the niobium-rich phase within the 45 to 75 #m diameter powders, 22 5%, was mea-
sured by quantitative metallographlc techniques applied to a n u m b e r of backscatter electron
images This analysis was performed on the samples prior to etching in order to maintain two-
dimensional surfaces This value compared quite well with one obtained from the actual
chemical analysis, in which the total volume fraction of second phase, 23 9%, was calculated
by summing the volumetric amounts of both niobium and molybdenum present in the alloy
This summation was done because results of qualitative energy dispersive X-ray analysis
TABLE 1--Surnmazv of the rnlcrostructural charactertzatlon o f HPGA Cu-21 2 Nb-1 8Mo powders as
a functton o f particle stze
Mlcrostructure
Second-Phase
Powder Size, Second-Phase Volume Spheroid Dendrite Stalk
~m Powder S h a p e Morphology Fractmn Size, um Diameter, um
- 15 spherical mainly spheroidal 35% <0 1 to 1 5 0 2 to 0 3

- 4 5 + 15 sphencal spherolds/dendntes ~25% <0 1 to 2 0 0 2 to 0 3
- 6 3 + 45 spherical dendntes 22 5% NAa 0 3 to 0 5
- 9 0 + 75 some irregular dendrites 22 5% NA 0 3 to 0 6
a Not available
ZEIK ET AL ON POWDER METALLURGY 367
FIG 2--Scanning electron rmcrograph of the rmcroslructure of a ~mgle, large (53 um m dmrneter) cop-
per-mobmm, HPGA powder parttcle containing a dzstrtbutzon of mobmrn-rlch dendrites
(EDS) mlcroanalysis had indicated that molybdenum is present within the dendntlc matenal
but absent from the matnx This observation was confirmed by previous work, that both mo-
blum [4] and molybdenum [5] are virtually Insoluble in copper and completely miscible
themselves [5]
In contrast, the mlcrostructures of the "fine" powders, classified as those less than 15 um in
diameter, consist primarily of a distribution of spheroidal particles ( ~ 2 um diameter) together
with a few dendrites distributed within tbe copper matrix, see Fig 3a Within the fine powder
particles, the volume fraction of this "second phase" approached 35% (10% d e n d n t e s + 25%
spheres) This indicates that the spheroids must contain considerable copper, assuming that
the dendrites are nearly pure niobium A cross-sectional view of the spheroids is shown in Fig
4b and reveals that they are, in fact, multlphase Scanning electron microscopy (SEM) imaging
in conjunction with EDS micro-analysis indicates that the spheroidal particles have niobium-
rich shell, arrowed 1 in Fig 3b, and an Interior consisting of both niobium- and copper-rich
phases, arrowed 2 and 3, respectively (this was further confirmed by transmission electron
microscopy (TEM) investigations) The significant amounts of copper in the spheroidal par-
tlcles results in the enhancement of the "second" phase volume fraction from ~ 2 2 % in the
large powder particles to a m a x i m u m of-~35% in the fine particles The diameter of the spher-
oid particles within the fine powders vaned from < 0 1 to 2 0 um In addition, a few small
dendntes were observed at both the powder particle surface and randomly distributed within
the interior.
The " m e d i u m " size powder particles, classified as those between 15 and 45 um in diameter,
possess mlcrostructures typified by F~g 4 Within this powder size range, as particle size
increases, the volume fraction of dendrites increases relative to the volume fraction of sphe-
roids As the dendrite volume fraction nears total dominance over the spheroids, the overall
volume fraction of the second phase(s) decreases toward 23% As previously noted, this value
FIG 3--Scannmg electron mzcrograph of(a) the mwrostructure o f a single, small (10 um m diameter)
copper-moblum, HPGA powder parttcle and (b) a cross-sectional view o f a smgle composzte spherotd con-
lamed w~thm this mtcrostructure
FIG 4--Scanmng electron mlcrograph o/the mlcros'tructure ofa single, medmm-slze (20 um m dmm-
eter) copper-moblum, ttPGA powder partlcle that ~ontams large amounts ()/both mobmm-rlch compos'lte
sT)herolds" and mobmm-based dendrites
compares favorably to that predicted from the chemical analysis of this alloy 23 9% by
volume
The preceding observations indicate not only the range of mlcrostructures present in the
H P G A Cu-Nb-Mo powders but also the ability of the present metallographlc technique to
delineate the cntlcal features without resorting to time-consuming, difficult-to-perform foil
preparation for TEM The observations of two distinct particle mlcrostructures within small
and large powder sizes and of a mixed morphology in medium powder sizes, are descnbed m
more detail elsewhere [2] In that study, the dependence ofmlcrostructure on particle size has
been interpreted in terms of a combination of undercoohng and rapid solidification Since it
has been determined previously that the amount of undercoohng achieved by an atomized
droplet is related directly to the size of that droplet [6], it follows that a mlcrostructural evo-
lution process sensitive to undercoollng may d~ffer over a range of powder s~zes As a result,
the formation of the niobium-rich spheroids within the fine powders, Fig 3b, suggests that a
fine-scale hquld-hquid phase separation occurred dunng rapid cooling and subsequent under-
coohng of the atomized droplets prior to solidification In contrast, the large (45 to 75 um)
powder particles are expected to cool at a rate such that the sohd~ficatlon path conforms to a
rapid, dendritic sohdlfiCatlon mode Upon atomization, these droplets are not hkely to under-
cool to the extent required to cause hqmd immiscibility, since there exists a high probability
that each would contain effective heterogeneous nucleation sites [6] This would prevent
access to the hquid phase separation and promote nucleation and growth of solid niobium,
forming a fine dispersion of dendrites within a copper matrix, as demonstrated in Fig 2
Finally, the mlcrostructure of the medium-size (15 to 45 um in diameter) powders, Fig 4,
charactenzed by a dispersion of both niobium-nch spheroids and dendntes randomly dis-
persed within an almost pure copper matrix, reflect a kinetic competition between the nucle-
FIG 5--Scanning electron mlcrographs of the cross-sectional vtews of a compression specimen pro-
duced from the 45 to 63 um HPGA powder and tested at 25 ~ Figure 5a Is perpendtcular to the load acts
whtle Ftg 5b lS parallel
atlon of nearly pure moblum dendntes and the nucleation of nlobmm-nch alloy spheroids via
liquid phase separation
In addition to the mlcrostructural evaluation of m&vldual powder particles previously pre-
sented, the deep-etch technique presented hereto was also used to document the flow behavior
of the m o b l u m - n c h second phase during deformation of bulk samples produced from the
h~gh-pressure gas atomized powders F~gure 5 contains SEM ~mages of the cross sections of a
compression test specimen, produced from the 45 to 63 gm dmmeter powders and tested at
25~ to a strain ofe = 1 0 A comparison ofth~s figure with the undeformed, parhcle m~cro-
structure m Fig 3 ln&cates that substantml deformation of the m o b m m dendrites has
occurred during the deformation of th~s "m~crocompos~te " Metallograph~cally, R ~s ~mpor-
tant to note that the copper matrix has been effioently removed from areas surrounding the
deformed m o b m m dendrites without disturbing those features Such a techmque has been
used to evaluate the flow behavior of the various mlcrostructural components generated by
the H P G A process over a w~de range o f test temperatures [1]
Summary
A metallographlc technique has been developed to emphasize the morphological features of
second-phase d~sperslons contained wRhm copper-based alloys As a model system, Cu-
21 2Nb-1 8Mo (% by weight) alloy powders have been produced by H P G A The microstruc-
tural evolution o f these powders has been documented as a function of powder particle size by
classifying, mounting, and polishing through the diameters oflndlwdual powder particles and
then using an "attack etch" to remove some of the copper matrix In conjunction with SEM,
this metallographlc technique has enabled a thorough characterization of the niobium-rich
second phase, relating the size and morphology of these features to the as-atomized powder
particle diameter This information has been used to develop a model for the mlcrostructural
evolution within this alloy and provide a relationship to the H P G A processing con&t~ons
References
[1] Zelk, K L, Ph D thesis, The Pennsylvama State Umverslty, University Park, 1991
[2] Zelk, K L, Koss, D A, Anderson, I E, and Howell, P R, submitted for pubhcat~on to Metallurgical
TransacUons, 1992
[3] Verhoeven, J D and Gibson, E D, Journal of Materials Sctence, Vol 13, 1978, p 1576
[4] Petrenko, V T , Tikhonovsku, M A, Berdnlk, A P, Somov, A I, Olekswnko, M M, and Arzhav-
ztm, V M , Voprosy Atomnot Nankt t Tekhmkt, Senya Obschchaya l Yadernaya Ftzeka (Problems
of Nuclear Science and Technology, Serges General and Nuclear Physics, Vol 9, 1979, p 20, (m
Russian)
[5] Brewer, L, Lamoreaux, R H, Ferro, R, Marazza, R, and Glrgls, K, Molybdenum Physzco-Chem-
teal Propertws oflts Compounds" and Alloys, L Brewer, Ed, International Atomic Energy Agency,
Vienna, 1980
[6] Anderson, I E and Kemppamen, M P, m UndercooledAlloyPhases, E W ColhngsandC C Koch,
Eds, The Metallurgical Society ofA1ME, Warrendale, PA, 1986
M a r k D. Fisher, ~Arnold F. Sprecher, 2 and Hans Conrad 2
Metallography Applied to the Structure of

Electrorheological (ER) Fluids
REFERENCE: Fisher, M D , Sprecher, A F , and Conrad, H , "Metallography Applied to the
Structure of Electrorheological (ER) Fluids," Metallography Past, Present, and Future (75th
Anmversary Volume), A S T M S T P 1165, G F Vander Voort, F J Warmuth, S M Purdy, and
A Szirmae, Eds, American Society for Testing and Materials, Philadelphia, 1993, pp 372-389
ABSTRACT: Employing optical microscopy and statistical analysis, the structure of a model
electrorheologmal (ER) fired consisting of 7 um (log-normal &stnbutlon) and 27 um (normal
dxstnbutlon) diameter glass beads m slhcone off was determined quantitatively as a functmn of
electric field and concentration of beads The arrangement of the beads m the lmtml structure at
zero field exhibited a high contlgmty, but showed no slgmficant alignment with respect to the
electrodes Upon application of an electric field, the beads aligned m the &rectlon of the field, E,
the degree of ahgnment increasing rapidly with E to ~ 1 kV/mm and then remaining relatively
constant A well-defined chain structure whereby most of the beads resided along chains that
bridged the electrode gap first occurred at a field of ~ 0 5 kV/mm, following which only slight
changes m the structure took place at higher fields The spacing of the chains decreased with
volume fraction of beads, their thickness increased The spacing-to-thickness ratm was slightly
larger than 1deal The mean free spacing of the chain structure was twice that of the beads prior
to the apphcatlon of the field, indicating that the chain structure was formed by the beads moving
m opposite dlrectmns towards their nearest neighbors No clear effect of bead s~zeor distribution
on the general behavmr was detected
KEY WORDS" electrorheologlcal fluids, glass beads, electnc field, chain structure, volume frac-
tmn, d~stnbutlon functmn, statistics, spacing, thickness, metallography, mlcrostructure, metal-
lographlc techniques
Electrorheologlcal (ER) fluids are dispersions o f fine polarizable particles In dielectric liquids
that u p o n application of an electric field change rapidly from hquld-hke to solid-like behavior
These fluids were first discovered by Wlnslow [1], who also d e t e r m i n e d that the particles in
t h e m form a chain-like or fiber-like structure (fibratlon) upon application of the field The
formation and strength o f these fibers is believed to be responsible for the large increase in
shear strength that results w h e n the field is applied [2] Therefore, to understand the strength
of an E R fluid, it is i m p o r t a n t to have a quantitative description o f the arrangement of the
particles therein This then was the objective of the present investigation For this purpose, we
e m p l o y e d a m o d e l E R fluid system consisting o f glass beads in silicone oil This system was
chosen for three m a j o r reasons (a) it exhibits E R behavior similar to hydrous-based E R fluids,
(b) the beads are readily visible under an optical microscope at magnifications o f • 50 to
• 200, and (c) the chemical c o m p o s i t i o n o f the glass spheres is comparable to that o f the silica
particles e m p l o y e d m experimental fluids being considered for practical applications [3] Pre-
h m l n a r y results of this study were presented in R e f 4, more complete findmgs are given here
Assooate project chemist, Dow Cornmg, M~dland, MI 48686

2 Senior research assocmte and professor, respectively, North Carolina State Umverslty, Materials So-
ence and Englneenng Department, Raleigh, NC 27695-7907
372
Copyright
Copyright*by1993
ASTMbyInt'l
FISHER ET AL. ON THE STRUCTURE OF ELECTRORHEOLOGICAL (ER) FLUIDS 373
Experimental
Model ER Fluids
Glass spheres of 7 and 27 ~zm mean diameter were provided by Potter Industries and had
the following nominal chemical composition in percent by weight: 72.5% SiO2, 13.7% Na20,
9.8% CaO, 3.3% MgO, 0.4% A1203, 0.1% K20, and 0.2% F20 and Fe203. Their specific gravity
is ~ 2.5 and dielectric constant 7.2 (1 MHz at 20~ The dielectric liquid employed was Dow
Coming 50 centistoke silicone oil of specific gravity = 0.96 and dielectric constant = 2.76 (10
kHz at 23~ [5]. The volume fraction of glass beads in silicone oil employed in the present
study ranged from 0.15 to 0.90. Following mixing, the dispersion of glass beads in silicone oil
was "conditioned" by heating in a chamber for 30 min at 90~ and 95% relative humidity. It
is estimated from the loss in weight obtained by heating (200~ beads humidified in the same
manner that they contained an adsorbed film of water (H20) of ~ 2 0 0 A thickness, in accord
with results in the literature [6].
Metallography and Statistical Analysis

The ER fluids were examined by transmission optical microscopy at • 50 to X 200 employ-
ing the cell shown in Fig. 1, which consists of a glass slide with two parallel 4 m m wide by 50
um thick copper strips spaced 1.2 mm apart connected to a d-c high-voltage power supply.
The dispersion of glass beads in silicone oil was placed carefully onto the glass slide by means
of a syringe, filling the gap between the electrodes. Care was taken to ensure that there occurred
only one layer of beads on the slide. A photo was first taken of the arrangement of the glass
beads with no field applied. A voltage was then applied (generally taking ~ 50 ms to reach the
desired value) to the electrodes, corresponding to an electric field, E, in the range of 0.5 to 3.0
kV/mm, and the resulting structure photographed within a period of about 30 s while the field
was still on. The main features of the structure developed faster than the eye could follow;
however, adjustments and rearrangements of the beads continued for periods of minutes and
FIG. 1--Schematic of the cell employedfor optical observation.

longer A fresh E R fluid sample was e m p l o y e d for each variation in field strength or v o l u m e
fraction o f beads investigated, to avoid any history effects
Stereologlcal features that were considered to be i m p o r t a n t pertaining to the initial disper-
sion structure at zero field and after application o f the electric field are listed in Table 1, some
are illustrated in Fig 2 T h e parameters were measured directly from the photomicrographs
using standard procedures [ 7-9] However, s o m e adaptations o f these procedures were nec-
essary for features not typical in other microstructures The data were plotted in hlstograph
format, and for each data set the m e a n and m e d i a n values and the standard devmtion were
d e t e r m i n e d Further, the data were analyzed to ascertain whether a given parameter was dis-
tributed In a normal (gaussian) or log-normal form This was accomplished by comparing the
m e a s u r e d (observed) data with computer-generated (expected) values. The expected data sets
were generated using a distribution function with the m e a n and standard deviation o f the mea-
sured data The fit o f the distribution was determined by the chl-squared, x 2, parameter that
gives a measure of the deviation between the observed and expected data [10]
x2 = ~ (observed - expected) 2
expected ( 1)
Chl-squared tables are based on a m i n i m u m o f 33 data values per set Since some of the
m e d i a n values were d e t e r m i n e d from less than 33 values, the standard chl-squared tables could
not be used for these cases T h e expected values were then determined by the possibility of the
data o c c u m n g over a given range when the m e a n and standard deviation are known For the
n o r m a l distribution, the expected probability o f the value being in the range o f x l to x2 is given
by the following distribution function [10]
expected- ~
1 .x2
~,xl x e (l/2)[(x-u)/~]2 d x (2)
where u and ~ are the m e a n and standard deviation With the use o f a computer, the median
and standard deviation were used to generate 1000 normal and log-normal distributions with
an equivalent n u m b e r of data points These distributions were then employed to develop a x 2
table that could be used for hypothesis testing The null hypothesis, H0, was used in the test to
d e t e r m i n e whether the data were distributed in the form o f the comparison [ 10]
TABLE 1--Stereologtcal parameters measured on the ER flutds
Symbol Defimtlon
AA The area fraction of glass beads that is proportional to volume fraction, V~

~c Center-to-center spacing of the beads m the initial structure
Inn Nearest-neighbor spacing of the beads in the lnmal structure
), Free spacing between the beads m the initial structure
C Contiguity ~s the fraction of particles contacting other particles in the mltml structure
C = 2 N~a/NA, Naa is number of contacts per umt area, N~ the number of beads
per unit area
lo(• The spacing between chain centers taken perpendicular to E
Xc(• The free spacing between chains taken perpendicular to E
xc(• The thickness of the chains taken perpendicular to E
xc(ll) The spacing taken parallel to E of the cells formed by cross hnks between chains
& Number of points of the feature of interest per umt length, parallel PL (]P) and
perpendicular Pz (Z) to E
ill2 The degree of orientation or anlsotrop~c arrangement of the particles ftl2 = [PL ( l )
- PL (]])]/[PL ( • - 0 571 PL (]l)] for the two-dimensional case [8]
FIG. 2 - - T h e structure prior to (a) and after (b) the application o f an eleetric Jield E = 1.5 k V/mm to
the model ER fluid consisting of O.40 volume fraction of 27-um diameter glass beads in silicone oil. Illus-
trated are some o f the stereological parameters that were measured.
0.3
Glass Beads
= 27(l.Lm)
>- 0.2
0
Z
LU
0
LU
n"
LL
0.1
0 10 20 30 40 50
Sphere dia., d (l~m)
(a)
0.6
Glass Beads
d=7j~m
0.4 N=IO0
0"
14.
0.2
0 5 o is 20 25 30 3s, 40 4s 50
Sphere dla., d (~m)

(b)
FIG 3 - - T h e s t z e dt ~trtbutlon o f t h e g l a s s h e a d s (a) ~r = 2 7 u m , a = 8 2 l~m, a n d (b) ~l = 7 u m , cr =
5 8um N = l O O m each c a s e
FISHER ET AL ON THE STRUCTURE OF ELECTRORHEOLOGICAL (ER) FLUIDS 377
FIG 4--The structure prtor to (a) and after (b) apphcatton of an electrtc field, E = 1 5 kV/mm, to the
model ER flutd eonststmg of O 44 volume fractton of 7-um diameter glass beads m slhcone otl
1.0 i - i 9 i 9 i 9 i - i 9 i
0.8
0
0.6
0.4
, ~ , d=' 7p.m
"0
e-
0
0,2
0.0 U []
II 9
D ~12, d'=27~ m
n 9
-0.2
9 9 9
9 Q12'
d'=7~.m
,~,4 I I ! I I I i i
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8
AA
FIG 5--The contlgutty, C, and the ortentatton parameter, ~212,versus area fraction, AA,for 7-lzm and
27-#m dtameter glass beads In slhcone oll prlor to the apphcanon of an electrtc field

Glass Beads
The size dlstnbutlons of the glass beads are shown in Fig. 3. The larger beads have a normal
size d~stnbutlon with a mean diameter of 27 #m and a standard devmtlon of 8 2 #m The
smaller beads have a log-normal dlstnbuUon with a mean of 7 #m and a standard deviation
of 5 8 #m.
Structure at Zero Fteld

The structure that exists when the beads are first d~spersed onto the glass shde with E = 0
is here termed the "initial structure." For th~s condmon, the glass beads exhibited no clear
pattern or arrangement, see for example, Figs. 3a and 4a That the beads are relatively non-
oriented with respect to the electrodes ~s indicated by the low values of the onentaUon param-
eter, fl~2, found for all area fractions, AA, of beads, see Fig 5. The slightly negative values offl~2
for the 7-urn beads (indicating a tendency to be onented parallel to the electrodes) may have
resulted from the manner m which the fired was inserted between the electrodes Evident in
F~g 5 is that ~ 1 2 I S relatively independent of AA On the other hand, the cont~gmty, C, increased
FIG. 6--Examples of the histograms for the initial structure ('d = 27 um, AA = 0.42): (a) thefree spac-
ing between particles, ~; (b) the center-to-center spacing between particles, In" and (c) the nearest-neighbor
spacing 1...
200
Glass B e a d s / S i l i c o n e Oil
E=0
8-2rgm
150 LC
e-
l . -= D
"o
e- 100
03
In
0
I_ u
50
~
O
u.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
AA
FIG 7--icc, X, and i.. versus area fractwn, AA, for the lnlttal structure of 27-um glass beads in slhcone
oil
with AA, as might be expected The smaller value of Cfor the 7-um beads probably results from
the smaller surface area per particle available for contacting another parttcle
Examples of the histograms for the measured spacing between particles in the initial struc-
ture are gwen m Fig 6 The dlstnbutlon of the free spacing, ~,, the center-to-center spacing, lcc,
and the nearest-neighbor spacing, l.., were determined to be neither normal nor log-normal,
w~th loc and l.. approximating more a Polsson dastnbutlon The decrease m the mean values,
1.., 7~, and X, with area fraction (volume fraction) of glass beads is shown m Fig 7 The mean
values had a + 5% spread at the 95% confidence level The solid hne drawn m the figure for
IS based on the expression for a random mixture, namely [9]
1-V~
X- (3)
NL
where Vv cx AA and NL is the number of intercepts per unit length, the intercepting features
being the glass beads Equation 3 gives values that plot as a loganthmlc curve Therefore, a
logarithmic curve was used to fit (least squares) the data for lcc and ~ gwmg
FISHER ET AL ON THE STRUCTURE OF ELECTRORHEOLOGtCAL (ER) FLUIDS 381
F I G 8--Development of the chain structure wtth mcreasmg field m the flutd contammg 0 4 volume
fractzon of 27-um beads (a) E = O, (b) E = 0 15 kV/mm, (c) E = 0 3 kV/mm, (d) E --- 0 5 kV/mm, (e)
E = 1 5 kV/mm, and (f) E = 3 0 k V / m m
X = 11AA'2 (#m) R2=084 (4)
and
7~ = 33 Aj~ (#m) R z = 092 (5)
However, a better fit was obtained with a hnear plot gwmg
X = 115- 163AA(um) R 2 = 097 (4a)
and
1r = 142 - 165 AA (#m) R z = 0.97 (5a)
The reason for the better fit to Eqs 4a and 5a may reside m the large contlgmty that existed,
especmlly at low area fractions, thereby reducing the averaging spacing between particles
1.0
0.8 o AA= 0 . 20
J o
0.40
0.6 A 0.70
r
t- Glass Beads/Silicone Oil
d=27txm
0.4
0.2
0.0
. 0 2t , , , , , , i ,
0 1 2 3 4
E(kV/mm)
FIG 9--The degree of ortentatton, ~12, versus electrlc field, E, for three concentrattons of glass beads
Structure Upon Application o f Electric Field

The manner in which the chain-like structure developed as the field was gradually increased
is illustrated in Fig. 8 for a fluid containing 0.4 volume fraction of glass beads. At low fields (E
= 0.15 kV/mm), the beads begin to form chain segments aligned in the direction of the electric
field. With increase in field to 0.3 kV/mm, the chain segments lengthen by attachment of avail-
able free beads and by joining of segments. At this field strength, some segments have attained
sufficient length to bridge the electrode gap. At E = 0.5 kV/mm, most chains now extend from
one electrode to the other, giving a clearly-defined chain structure. Further increase in field to
3.0 kV/mm produces some thickening and cross linking of the chains, but otherwise no dra-
matic change in the general appearance of the structure. Similar behavior was noted for all
concentrations of beads investigated and both sizes of beads.
The degree of alignment of the beads along the direction of the field is described by the ori-
entation parameter, ~2. Figure 9 shows the variation of ~212with field strength and concentra-
FIG. lO--Examples of the histograms for the structure (d = 27 um, AA = 0.38) obtained with E = 1.5
k V/mm: (a) the free spacing between chains, Xc ( I ) , and (b) the thickness of the chains, Xc (I).
tlon of beads It is evident that fl~z increases with E to about 1 k V / m m and then remains rel-
atively constant for further increase in E However, fl~2 decreases slightly as the volume
fraction of glass beads is Increased This results mainly from the fact that the amount of cross
linking between chains increased as the concentration of beads increased Worthy of mention
is that the saturation of ft~2with respect to E occurs at a similar value of E as did the activation
energy, Q,t. associated with the structure term in rheological measurements on slhca/slhcone
oil ER fluids [ 11 ] Also, a saturation of the structure at E = 1 to 2 k V / m m was found by optical
measurements (birefnngence and dichroism) on ER fluids consisting of 130 and 49 nm silica
particles in cyclohexane [ 12]
Since in the present studies a well-defined chain structure first formed at E ~ 0 5 k V / m m ,
the pertinent parameters,/c ('L) (center-to-center spacing between chains), Xr (-L) (free spacing
between chains), and Xc (-L) (thickness of the chains), could only be determined for fields
400
Glass beads/Silic0ne O=1
t 7=0
E= 0.5-3.0kV/mm
320
E
o 240
IX
c-
-H
o
A 160
-H
v
o
2c(-L)
80 7c(-L)
=27p.m
0 0.2 0.4 0.6 0.8 1.0
AA
FIG 11-- Variation o]'the mean parameters lc (I), Xc (3_), and Xc ( J_) wtth area fractton, AA, of 2 7-~m
glass beads
FISHER ET AL ON THE STRUCTUREOF ELECTRORHEOLOGICAL(ER) FLUIDS 385
greater than this value An example of the dlstnbutlon in the values o f Xc(-L) and of Xc ( _L) is
given in Fig. 10. The • test was employed to compare such distributions with the normal
(gausslan) and log-normal forms. Moreover, the Wllcoxon ranked sums test [10,11 ] was used
to ascertain the effect of the field strength on the distribution for a constant volume fraction
of beads. In the case of Xr (_k), half of the distributions accepted the null hypothesis, H0, for
the normal form, while the other half accepted it for the log-normal form A larger fraction of
the distributions accepted H0 for the normal form as the field strength increased. In the case
of Xc (d-), all of the distnbutions accepted H0 for the log-normal form.
In the Wllcoxon ranked sum test, H0 was used to determine whether distributions were sim-
ilar, that is, indistinguishable. For AA ~ 0.2, the distributions of Xr ( l ) and Xc ( / ) could be
distinguished between E = 0 5 k V / m m and E > 1.5 kV/mm, that IS, H0 at the a = 0 05
confidence level was rejected However, the distributions for E = 1.5 k V / m m and E = 3 0
k V / m m were not distinguishable. For AA > 0.4, the distribution for E = 0 5 to 3.0 k V / m m
could not be distinguished, that is, they were independent of electric field in this range Thus,
forAA > 0 2, the structure is essentially independent of the electric field for E > 0 5 kV/mm,
in accord with the results for fh2 in Fig. 9.
In keeping with the preceding points, the mean values oflc ( 1 ) , ~r ( / ) , and X~ ( • (which
exhibited a _ 10% spread at the 95% confidence level) were relatively independent of E in the
range of 0.5 to 3 0 kV/mm. Their variation with AMis shown in Fig. 1 l, where it is seen that
7c( 1 ) and Xr (_l_) decrease with AA, while X-r (d_) increases. The largest AA values in Fig. I l are
in excess of that for the packing of equi-slzed spheres (for which AA ----0.78) This is believed
300
GlassBeads/SiliconeOil
E=1.5kV/mm
250
E
200 ~\ [c(• d-=27~m
o
IX Xc(-L) k ~'=271J.m
. ~ 150
d'---7~m X'c(•
--- 100
O ,o O
Xc(•
d=7,u.m
50
0.0 0.2 0.4 0.6 0.8 1.0

AA
FIG 12--Comparison of the mean parameters Xc (_L) and Xc (_L) versus area fractton, AA, for the two
bead stzes
to be due to the spread in the size distribution of the spheres and the accidental occurrence of
some second-layer particles dunng placement of the particles on the glass slide Figure 12
shows that the variation ofXc ( _L) and X-c (-L) with AAis similar for the two sizes of glass beads.
An area fraction greater than t 0 45 was difficult to obtain for the smaller beads, because there
occurred an appreciable second-layer effect when larger concentrations were employed
An additional feature of interest in the structure produced by the field is the cross hnking
between the chains that extend from one electrode to the other, whereby the structure develops
into one of elongated cells Figure 13 shows that the mean free spacing between cross-links,
Xc (11), is proporhonal to the mean free spacing between chains, ~c (J-), the proportlonahty
constant being ~ 2 . This leads to a decrease In the area bounded by the cells with increase in
AA, the cell area approaching the glass bead cross-section area at largest values of Aa
One expects a correlation between the mean spacing between chains, lc ( / ) , and the mean
thickness of the chains, X-c (_t_). For equl-sized spheres of diameter, d, and assuming that they
700
9 / -
600
500 ".7
SJ.
E
9-~ 400
I~ ~ 300
G l a s s Beads/Silicone Oil
E=0.5-3.0 kV/mm
200
d=27~tm
100 A A : 0.2
|
O
0 100 200 300
FIG 13--Mean free spacing between cross hnks, -~c (11). versus mean free spacing between chams. Xc
( I ) , for the flutd wtth 27-urn partmles
all align into chains of equal spacing and thickness, one obtains from the conservation of
spheres
7~(_L)/X-<(J-) = 7r/(4A.) (6)
A plot of the measured values of the rauo lc (-L)/X-c ( l ) versus 1/AA for the 27-#m beads is
presented in Fig 14 Except for the smallest values ofAA, where the chains were not well devel-
oped, the measured ratio is proportional to 1/AA In accord with Eq 6. The slope of the line for
the measured values is, however, ~ 1, which is 4 / r larger than for the ideal case. The difference
xs considered to be due to the fact that the glass beads are not all of the same size and to
the occurrence of cross hnks and isolated beads and chain segments. The slope of a similar
plot for the 7-um beads was ,~ 1.5 m keeping with the broader distnbution of sizes for these
beads
F~gure 15 shows that ~ (J_) is about twice the initial mean free spacing between the beads,
X, p n o r to the application of the field This suggests that the chains form by the movement on
the average of one-half of the beads towards one set of their nearest neighbors and the other
half m the opposite direction to their other nearest neighbors [4]
Glass beads/Silicone Otl / p

a=27~m /p /
E= 0.5-3.0kV/mm
6
IX
-- 4
// ~e/Xo =n/4AA
v
Slope//=1// - / ~~r.(_L)
2
, i Xc(_L)
0 2 4 6 8
1/A A
FI G 14--The ratto ]c ( l ) / ~ c ( I ) versus the rectprocal of AAfor the fluld wtth 27-urn particles The
dashed hne isfor the tdeal case of equt-stzed spheresformmg equt-spaeedehams parallel to the electrtcfieM
as shown tn the msert
300
Glass Beads/Silicone Oil

d=271~m
200
-%
100
9 9
i I I i
0
20 40 60 80 100
~, (gin)
FIG 15--The mean free spacmg of the chams, Xc (1), versus the mean free spacmg of the beads m the
mlttal structure, -X,for the flutd with 27-~tm beads
Summary and Conclusions

Inttlal Structure
The glass beads dispersed onto the observation cell were essentially non-oriented, thereby
providing no bias to the chain structure that formed upon apphcatlon of the electric field
The observed high degree of contiguity m the initial structure could be due to the water
adsorbed on the glass beads providing an attractive surface tension force between the particles
The d~stnbut~on function of the spacing between nearest neighbors m the mltlal structure
was neither normal nor log-normal m form, being more nearly Polsson.
Structure Upon Apphcatzon o f an Electric FleM

The orientation of the glass beads, which leads to the chain structure, increased rapidly with
electric field to ~ 1 k V / m m and then remained constant with further Increase to 3 kV/mm A
distinct chain structure whereby most chains extended completely across the electrode gap first
occurred at E = 0 5 k V / m m
The dlstnbutlon of the free spacing between chains, ~r (_1_), tended to be normal, whereas
that of the thickness of the chains, Xc ( l ) , tended to be log-normal
The mean free spacing between chains, Xc (.1_), and their mean center-to-center spacing, 7c
( l ) , decreased m an approximately hnear fashion with volume fraction of beads m the range
of 0 2 to 0 9, and their mean thickness, X c ( l ) , increased hneanly
The mean free spacing between cross links, ~c ([I), m the chain structure was about twice the
mean free spacing between chains, ~ ( l ) .
The ratio oflc (-[-)/X-c ( l ) was directly proportional to the reciprocal of the volume fracUon
of glass beads Th~s ratio is 417r greater than that expected for eqm-s~zed beads giving equi-
spaced chains
Xc ( l ) is about twice the lmtlal free spacing between beads, ~, p n o r to the apphcatlon oftbe
field Th~s suggests that the chains form by the movement on the average of one-half of the
beads towards one set of their nearest neighbors and the other halfm the opposite direction to
their other neighbors
Acknowledgments
The authors gratefully acknowledge support of their work on ER fluids by the Nahonal Sci-
ence Foundation under NSF award No CBT-8714515, the Ford Motor Company, and the
North Carolina State University (NCSU) University/Industry Consortium on ER Fluids
References
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Applications II
Richard N. GrugeP and Rohit Trivedi 2
Interpreting Solidification Phenomena and

Microstructural Evolution in Metals Through
the Use of Transparent Model Alloy Systems
REFERENCE: Grugel, R N and Trlvedi, R , "Interpreting Solidification Phenomena and
Microstrnctural Evolution in Metals Through the Use of Transparent Model Alloy Systems,"
Metallography Past. Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F
and Materials, Philadelphia, 1993, pp 393-413
ABSTRACT" It is well estabhshed that the material properties of alloys are directly related to the
scale and distribution of their microstructural constituents The advances and applications of
metallographlc techniques for the examination ofsohdlfied mlcrostructures have proven invalu-
able in ascertaining these structure-property relationships Unfortunately, many aspects of
microstructural evolution can only be inferred from a post-sohdification examination The use
of transparent compounds that freeze in a manner analogous to metals circumvents this problem
by allowing direct and continual observation of solidification events dunng both transient and
steady-state growth This paper discusses the role of these compounds in promoting understand-
mg of sohdlfication phenomena Examples of dendritic, eutectlc, and monotectlc microstruc-
tural development, pertinent to theory and practice, are presented and compared with their
metal counterparts
KEY WORDS. sohdificatlon, dendritic systems, eutectlc systems, monotectlc systems, casting,
microstructure, interface stability, composite materials, float-zoning, metallography, metallur-
gical specimens, metallographlc techniques
Solidification o f liquid alloys can be viewed as the initial processing step toward fabricating
virtually all c o m m e r c i a l metal products This encompasses sohdlfiCatlon o f bulk ingots weigh-
ing several tons, production o f sub-micron size powders by atomizing llqmds, casting of intri-
cate net shapes by the lost wax technique, and the crystal perfection sought by float zoning
SohdlfiCatlon times can vary from microseconds to weeks, with compositions ranging from
essentially pure materials to alloys consisting o f ten or m o r e elements While this only offers
the briefest of an introduction to solidification processing, the extent that it encompasses can
be appreciated Yet, in spite of these processing extremes, the mlcrostructures will often appear
very similar, differing only in the scale.
Thus, while the composition and processing technique will determine the scale and distri-
bution of the mlcrostructure, it Is reasonable to assume that constituents such as dendritic and
eutectlc phases will always be present As the direct correlation between mlcrostructure and
material p e r f o r m a n c e is well d o c u m e n t e d [ 1-3], it follows that the relationship between pro-
Research assistant professor, VanderNlt Umverslty, Department of Materials Science and Engineer-
ing, Center for Mlcrogravlty Research and Apphcatlons, Nashville, TN 37235
2 Senior scientist and Anson Marston distinguished professor in Englneenng, Ames Laboratory, U S
Department of Energy and the Department of Matenals Science and Engmeenng, Iowa State University,
Ames, IA 50011
393
Copyright9
Copyright by ASTM
1993 Int'l (all
by ASTM rights reserved);Www.astIII.OI'g
International Thu Dec 29 00:42:12 EST 2011
cessmg conditions and mlcrostructural evolution must be understood in order to optimize the
properties To this end, Innumerable lnvestlgahons have been undertaken While many dif-
ferent experimental techmques were utilized, they inevitably included sectioning and metal-
lographically preparing the solidified alloy for microscopic examination and evaluation The
subsequent analyses provided a great wealth o f reformation regarding mlcrostructure-pro-
cesslng relationships, particularly with regard to primary dendrite, secondary dendrite, and
eutechc spacings as functions of growth velocity, temperature gradient, and composlhon The
results, however, gave httle, if any, reformation into the initiation and evolution of the
observed mlcrostructure This was particularly true with regard to understanding dynamic
effects such as planar-cellular-dendrite transitions, dendrite arm initiation, mechamsms of
changing dendrite and eutectlc spacings, coarsening mechanisms, fired flow, and their overall
contributions to defining the mlcrostructure To investigate these phenomena, techmques
such as rapid quenching or decanting of the growing sohd-hquid interface were employed
Unfortunately, accompanying these procedures are transient effects attributed to quenching
and residual hqmds that mask the true structure So although some insight has been gamed,
the dynamic mlcrostructural development is still subject to a highly referred interpretation
The obstacle to overcome when conducting research in this field is the inherent opaqueness of
metals, a concern convemently remedied by use of appropriate transparent model alloy
systems
Model Alloy Systems

Hlstortcal Review
Perhaps the first study of transparent matenals to model the sohdification behavior of metals
was that of Papapetrou [4], who in 1935 directly observed, photographically recorded, and
reported on their dendritic growth and facet development In 1950, Kofler [5] investigated the
nature of coupled-zones by comparing organic eutectlc systems to metallic ones In 1958,
Jackson [6] introduced the "a-factor" and showed an example of salol growing in a faceted
manner from its undercooled liquid, and the dendritic growth of ice in water In his 1961
paper, Txmmermans [ 7] wrote of"plastic crystals" and, based on physical propemes, classified
organic compounds as "globular" and "non-globular," noting that the former had cubic-type
structures Jackson and Hunt [8] (1965) noted several compounds that freeze in a manner
analogous to metals and suggested using them to observe solidification phenomena directly
Their subsequent work with organic eutectic systems [9,10] is fundamental to our present
understanding of behavior in metal systems, and experiments utilizing ammonium chloride-
water solutions [11] have provided considerable insight regarding structural development in
bulk or ingot castings In view of this pioneering work, researchers have realized the advantage
of organic analogues in explaining solidification phenomena as is evident in subsequent stud-
les of dendritic [12-49], eutectlc [50-52], and monotectlc [53-62] systems, as well as bulk
castings [63- 75 ], floating zones [ 76-85], interface stability [86-96], and solid-liquid interface
Interactions [97-105]
Purpose, Characterlsttcs, and Examples

The purpose of a model system is to facilitate the direct and continued observation ofsohd-
ification phenomena as it occurs in a metal system Consequently, the components of the
model system, usually organic compounds or salts, must meet certain cntena Whereas the
phenomenon to be investigated will dictate selection of the appropnate matenals, there are
some fundamental reqmrements that are noted ln Table 1 T a b l e 2 h s t s a n u m b e r o f m a t e n a l s
GRUGEL AND TRIVEDI ON SOLIDIFICATION 395
TABLE l--Some fundamental requtrements desired in orgamc

analogues
I Transparency
2 Convement melting temperature, 0 to 100~
3 Chemically stable
4 Nonreactive
5 Preferably nontoxic
6 Crystallographic structure of interest
that m general, satisfy the preceding reqmrements Although these are routinely used, they
represent only a fraction of possible candidates
Figure 1 compares the dendritic growth seen from the quenched interface of a d~rectlonally
solidified magnesium alloy [103] with that directly observed in a succInonltrlle-watermixture
Not only as the likeness striking, but such compansons are common However, upon closer
examination, the orgamc analogue presents a number of advantages For example
1 There are no anomahes from quench effects, each dendnte arm, and ~ts constituents, ~s
d~stlnct
2 Mlcrostructural characteristics such as the dendnte tip radius, primary, and secondary
dendrite arm spacings can be directly measured
3 Dynamic effects such as secondary arm development along the trunk and their changes
in growth velocity as they begin to "sense" nelghbonng arms can be recorded and ana-
lyzed in real time
4 The mechanisms by which changes m spacing, for example, dendrite and eutectIc, occur
can be d~rectly observed
Experimental Methods and Examples

The ways and means of utlhzmg transparent analogues to study solidification phenomena
are essentially hmlted only by the ~maglnatlon of the investigator The following three exam-
ples represent procedures employed m the majority of studies conducted p n m a n l y , but cer-
tainly not exclusively, by the metals and alloys community Bear in mind that the methods
described here are generic in nature and subject to considerable variaUon depending on the
information sought
TABLE 2--Compounds havmg solldtficatton behavtor similar to metals Note that although some of
the melting pomts appear excessive, mtxmg with other compounds will lower them stgmficantly
Compound Structure Melting Point, ~
Succlnomtnle bcca 58
Camphor fccb 175
Carbon tetrabromlde fcc 90 1
Hexachloroethane cubic 184 5
Plvahc acid fcc 35 4
Ammonmm chloride fcc subhme 340
a Body centered cubic
b Face centered cubic
E I
II II
Temperature Gradient Stage Investtgatlons--The temperature gradient stage, introduced

in 1966 [104], is a powerful tool that allows for direct observation of a solidification interface
that is growing under controlled, steady-state conditions Basically, this procedure requires
three components, (a) a thin cell, (b) the temperature gradient stage, and (c) a microscope in
the transmitted light mode. The organic analogue shown in Fig 1b is an example of this
technique
(a) The thin cell, Fig 2a, essentially consists of two thin (0 1 to l mm) glass sheets (25 by
60 mm) that are separated by a fine gap The gap height is determined by the spacer
used and should, in general, be from 50 to 300 #m The cell is sealed along the edges,
often with an epoxy, with the exception of a small port at each end. The transparent
pure material or mixture of Interest is then melted and introduced at one of the ports
The cell then fills by capillary action, which may be facilitated by use of pressure or a
vacuum, after which the ports are sealed. It is desirable to include fine chromel-alumel
thermocouples within the cell for ln-sItu temperature measurements
(b) The thin cell is then placed on the temperature gradient stage, Fig. 2b, where it straddles
a "hot" and "cold" plate The temperatures of the respective plates are set such that a
sohd-hquld interface develops and is maintained between them After an equihbnum
period, the thin cell is drawn across the stage, usually toward the cold end whereupon
the sohdlfiCatlon proceeds in a directional manner Note that as the growing solid-liquid
interface is constrained by the temperature gradient imposed between the hot and cold
blocks, it maintains the same position under steady-state conditions
(c) Lastly, the gradient stage assembly rests on a microscope stage, Fig 2c, such that the
breech between the hot and cold blocks is directly over the transmitted light source
Consequently, the sohd-hquld interface that develops in the cell IS in line with the objec-
tive lens and may then be directly observed, photographed, or otherwise recorded The
observed mlcrostructure can then be directly related to the processing parameters of
growth velocity (V), temperature gradient (G), and composition (Co).
Use of the temperature gradient stage has proved invaluable in promoting our knowledge
of solidification behavior in dendritic, eutectlc, and monotectlc systems. This includes micro-
structure-processing parameter relationships, dynamic developments, lnterfaclal interactions,
and theoretical considerations
An example of dynamic development is given in Fig 3 [30] where evolution of the solid/
liquid interface has been directly observed and recorded Included in this series ofmlcrographs
is information regarding breakdown (instability) of the initially planar solid/liquid Interface,
Initiation of cells, transition to mixed cells and dendrites, and finally to steady-state dendritic
growth Not only is the scale of these developments observable, but also the mechanisms by
which they occur, this can then be related to the well-controlled solidification parameters of
V, G, and Co As seen in Fig 4 [52], comparable conclusions can be drawn regarding the ini-
tiation and development of eutectic growth Organic analogues have also been used to inter-
pret the mlcrostructure found in monotectlc systems For example, Figs 5a [105] and b [56]
are mlcrographs of dlrectlonally solidified Al-17 5In alloys In Fig. 5a, the indium phase
assumes an aligned rod-hke morphology as expected, however in Fig 5b, having a faster
growth rate, the indium phase is seen to consist of randomly dispersed spheres and dumbbell
shapes This latter structure was attributed to the indiscriminate Incorporation of the liquid
indium phase that accumulated and coalesced at the Llquld~/Solld~ + Llquldn reaction inter-
face Comparable to the Al-In mlcrostructure in Fig. 6a, rod-hke growth of the LlquldH phase
(glycerol) is seen in the analogous, organic, succlnonitrile-7 5% by weight glycerol system, the
mlcrostructure of Fig 5b is also similar to that seen in Fig 6b Note, however, the section
o ~
~___}
U~ ~~
j ~ ~~
!
| ~
8 ._g
~ i"6
g~
FIG. 3--Development o f solid-liquid interface shapes with change in growth rate from zero to 3.4 um
s i at a temperature gradient o f 6.7 K m m -1. (a) 50 s, (b) 55 s, (c) 65 s, (d) 80 s, (e) 135 s, and (f) 740 s
(from R e f 30).
represented in Fig. 6b is that of Fig. 6a, only a short time later. The conclusion must then be
that at "fast" growth rates the LiquidH is indeed incorporated in a rod-like manner, but that
the close spacing and liquid nature of the rods promotes rapid coarsening.
Finally, measurement of microstructural features from directionally solidified organic sys-
tems has also proved invaluable in ascertaining theory. Figure 7, for example, compares the
experimentally measured primary dendrite arm spacing to that theoretically predicted [26].
Analogue materials are well suited for studies like these due to the thorough knowledge of their
FIG 4--Evolutwn of lamellar structures durmg the dwectlonal ~ohd~catlon oJ a carbon tetrabromlde-
hexachloroethane eutectw at a growth veloctty of O 5 u m s i The ttmes measured from the mstant at whwh
the velocity was changed from zero to 0 5 u m s -I are (a) 11 33 ram, (b) 11 67 mm, (c) 12 33 mm, and (d)
16 m m (from Ref52)
II
\
=L
II
II
| 0 "l~i ' ! 1 ' 111'1 I ' I I I IIII I | ! ~1 ' I
E::L
- i0 z
* CELLS
9 DENDRITES
THEORY
i0{~ I . . . . . . . . , ,a ....... IC) . . . . . .

b . I V, / ~ m / s
FIG 7--(a) Dtrecttonally sohdtfied succmonttrtle-5 5 molecular percent acetone, growth velocity =
1 17 #m s - ~and temperature gradtent= 6 7 K ram- 1 and (b) comparison ofexpertment wtth theory (from
Ref26)
material properties and because of the experimental procedure that rigidly controls and accu-
rately measures the sohdlficatlon processing parameters
Bulk Casting Slmulattons--Solldlfication of, for example, large steel ingots invariably
results in " A " and "V" segregates and, subsequently, severe composmonal differences Th~s
results in a very inhomogeneous structure, the evolution of which can only be referred. As
demonstrated by Jackson et al [11] m 1966, such casting can be convemently simulated using
analogue systems that not only allow direct observation of dendrite growth and distribution,
but also the effect of convection, particularly in regard to plume ruination and development
A typical experimental setup, schematically depicted in Fig. 8, consists of two transparent
sheets, perhaps 15 cm square, separated by 2.5 cm These sheets are connected on the sides
and bottom by a copper bar, the top left open The bottom of the copper bar is then immersed
in llqmd mtrogen or some other coolant The model solution, often an a m m o n i u m chloride-
water mixture, is poured into the top after which solidification commences The extent of the
solute-rich plumes that exit the channels that develop in these "castings" ~s clearly seen in Fig
9 [63] by the slight a d d m o n of an appropriate dye
Dendrtte Growth Into Undercooled Melts--In contrast to the bulk casting simulations just
described, this techmque is specifically utlhzed to investigate dendritic growth phenomena on
a m~croscoplc level under very exacting condmons into pure or only slightly adulterated
undercooled hqmds A schematic typical of the apparatus used in these studies is shown m Fig.
10 The liquid m the flask is undercooled to the desired temperature and precisely maintained
by the surrounding bath. Nucleation is then lmtlated at some point away from the bulk of the
undercooled hquld with the sohd phase proceeding down a capillary tube A free, usually sin-
gle, dendrite then exits the capillary tube and grows into the bulk hquld such as seen in Fig. 11
[21] Evaluations of the microphotographs taken dunng growth have shown that not only do
unique and predictable relaUonshlps exist between undercoohng, growth velocity, and com-
posmon, but that constant scahng factors, for example, the dendrite tip radms to lnmal sec-
ondary arm spacing raUo, also exist, such information gwes us insight into pattern selection
and formation
r
t"-
~
I
15 cm
-- Copper
Framd I: Liquid
Nitrogen
FIG 8--Schemattc drawmg of a typtcal "bulk"castmg cell
FIG 9--Sohdlfcatzon of an ammomum chloride-water casting s'howmg colored solution pouring out
from behind the dendnuc front (from Ref 63)
Mlcrogravlty S t u d w s - - I n addition to the sohdxficatlon parameters of V, G, and Co men-

tloned earlier, gravity (or lack of) is continuing to nghtfully receive more and more recognition
as a processing variable Again, organic analogues have played an important role in ascertain-
ing the effect of gravity on solidification structure For example, dendritic growth of ammo-
m u m chloride crystals in a water solution was directly observed, that is, filmed, in the micro-
gravity environment afforded by a sounding rocket [69,70] The environment of space,
however, is not necessanly required to begin understanding the implications of solidification
phenomena in mlcrogravlty G h c k s m a n e t a l [19,23,36] have clearly shownthe effect ofcon-
Constant
Temperature
Bath
I I
-4 cm
FIG lO--Schematw drawing of an apparatus used to study dendritic sohdtficatton In undercooled
melts
vectlve heat transfer on the structure of pure succlnonltnle dendrites growing at different ori-
entations with respect to earth's gravity vector The two-dimensional nature of the thin cells
discussed earher effectively serve to suppress convection in the liquid [20,40,44,48] and thus
promote the experimental conditions one might expect in space It is also convenient to mix
organic solutions in proportions such that the liquid components of immiscible systems essen-
tially have the same density, which in essence eliminates phase separation, coalescence, and
segregation due to buoyancy forces This technique has been employed to investigate solidi-
fication phenomena in hypermonotectIc systems [60] Figure 12 is an example that shows liq-
uid-liquid phase separation and distribution in an isodense system Admittedly, the conditions
are far from Ideal, however, the insight gained was sufficient to conclude that gravity "inde-
pendent" effects of coalescence and preferential surface wetting are key factors leading to mas-
sively lnhomogeneous structures This has since led to a novel means of processing hyper-
monotectlc alloys, which, incidentally, was demonstrated using an organic analogue in
conjunction with a temperature gradient stage [62]
Addmonal Considerations When Usmg Analogue Systems

Although the earlier examples show the value of organic analogue systems toward the inter-
pretation of solidification mlcrostructures, It must also be realized that there are, beside the
obvious, a number of differences between them and metals For analogue materials
1 Heat conductivity in the solid is similar to that of the liquid

2 The liquid diffusion coefficient, De, is 1 or 2 orders of magnitude less than metals
FIG. 1l--Superimposition ~f time-lapsed photographs ~fa growing dendritic crystal, showing the side
branch evolution process on the {100} branching sheets ([?om Ref 21).
3. The Prandtl Number, Pr = viscous diffusivity/heat diffusivity, is 2 orders higher than

that in metals.
For comparison to metals, the earlier considerations imply using much slower rates during
constrained growth experiments, and a cautious interpretation of fluid flow effects in bulk
studies.
FIG 12--Photogtaphtc sequence of the hqutd-hquld phase separatwn and coalescence process m a
hypermonotectlc succmomtrtle-(water + ethanol) rmxture (from Ref 60)
Direct Observation of Solldlficatlon in Opaque (Metal) Systems

A number of methods for examining solld/hqu~d interfaces that are then inferred to account
for what occurs m an opaque metalhc system have been presented These studies have con-
tnbuted considerably to our knowledge of sohdlficatlon phenomena, but m rawness, tech-
tuques also exist that allow "d~rect" observation m metal systems These techmques and mves-
Ugatlons have been well discussed by Ghcksman [106] Examples include studymg eutectlc
growth phenomena with polarized hght [ 107,108 ], dendrite growth and remeltmg [109,110],
and solute redistribution using radlographxc techmques [111] High-resolution transmission
electron microscopy (TEM) studies have also been conducted [112], and high-speed photog-
raphy has been used to measure solld/hqu~d interface growth velocmes [113,114]
Conclusions
A bnef overwew has been presented on the use of transparent matenals that sohdlfy m a
manner analogous to metals In view of the examples gwen here, it is concluded that their use
not only allows for the dwect observation and recording of dynamic solidification processes,
but permits highly accurate measurements of mlcrostructural constituents, under well-con-
trolled conditions, that would otherwxse have to be referred from quenched-m sohd/hquld
interfaces of metals This reformation furthers our knowledge of sohdlficahon phenomena
and processing
Acknowledgments
This work was sponsored by the NASA Office of Space Science and Apphcatxons, and by
Ames Laboratory, which ~s operated for the U S Department of Energy by Iowa State Urn-
verslty under Contract No W-7405-ENG-82, Office of Basic Energy Sciences, Division of

Materials Science
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Edward Larkin I and Mehrooz Zamanzadeh
Some Failure Analysis Case Histories in

Galvanized Steel Products
REFERENCE: Larkln, E and Zamanzadeh, M , "Some Failure Analysis Case Histories in Gal-
vanized Steel Products," Metagography Past, Present, and Future (75th Anmversary Volume),
ASTMSTPl165, G F VanderVoort, F J Warmuth, S M Purdy, a n d A Szlrmae, Eds,Amer-
ican Society for Testing and Materials, Philadelphia, 1993, pp 414-428
ABSTRACT: The three case histories presented in this paper concern defects and causes of fail-
ure associated with galvanized steel sheet material Optical metallography and mlcroindentatlon
hardness testing were the principal methods employed in determining the cause of failure but
were supplemented as necessary by scanning electron microscopy and energy-dispersive X-ray
spectrometry
One of the case histories presents defects associated with the actual hot-dip galvanizing process
itself In one instance, tiny hydrogen bhsters were observed to have occurred at oxide scale depos-
its at the interface between the steel and galvanized coatings
When galvanized sheet steel cracks in bending dunng formingoperations, most end users tend
to place the blame on the galvanized material However, several separate investigations of
formed and cracked galvanized steel parts have revealed that the cracking often Initiates at the
sheared edges of the part where plastic deformation has produced a local increase in hardness
and a corresponding decrease in ductility Ductlhty is the property of steel required to success-
fully withstand forming operations
The final case history presents some observations made dunng failure analysis of corroded
galvanized and painted panels at a utility plant The coating system was composed of a galva-
nized layer, a thin primer, and a final top coat, The problem was identified as localized devel-
opment of white rust The problem was found to be caused by the presence of a second-phase
precipitate in the galvanized layer that adversely affected Its ductlhty allowing it to crack dunng
forming This produced localized stress in the paint layer that then cracked permitting moisture
to come into direct contact with the zinc, resulting in white rust formation
KEY WORDS: galvanized steel, failures (materials), lntergranular precipitation, hydrogen blis-
ters, forming problems, metallography, metallurgical specimens, mlcrostructure, metallographlc
techniques
Historical Background
C e n t u r i e s before zinc was discovered i n t h e metallic form, its ores were used for m a k i n g
brass. A n c i e n t metallurgists p r o b a b l y lost this volatile m e t a l as v a p o r because t h e i r a p p a r a t u s
was n o t designed for c o n d e n s i n g it [1] Metallic zinc is n o t a n easy m e t a l to p r o d u c e Z i n c
oxide c a n n o t be r e d u c e d b y charcoal at t e m p e r a t u r e s below 100~ However, zinc bolls at
923~ a n d t h e m e t a l is, therefore, p r o d u c e d as a v a p o r t h a t m u s t be collected a n d c o n d e n s e d
It is c l a i m e d t h a t C h i n a first p r o d u c e d zinc in the p e r i o d 200 B C. to 100 A D As far as C h i n a
is c o n c e r n e d , t h e r e is a reference in a t e x t b o o k o n metallurgy, d a t e d to 1637, for the p r o d u c t i o n
o f zinc in sealed c r u o b l e s [2] Z i n c was e v e n used for coinage d u n n g the M l n g dynasty (1368
to 1644)
Metallurgical engineer and manager, respectively, Metallurgy Division, Professional Service Indus-
tries, Inc, Pittsburgh Testing Laboratory Division, Pittsburgh, PA 15220
414
Copyright
Copyright*by1993
ASTMbyInt'l
LARKIN AND ZAMANZADEH ON GALVANIZED STEEL PRODUCTS 415
There is considerable evidence of the production of zinc in India between the tenth and
sixteenth centuries At Zawar, near Udiapur in Rajasthan, great heaps and walls of small
retorts have been found recently It is estimated that the elhptlcal retorts found at Zawar rep-
resent the extraction of 100 000 tons of metalhc zinc [3].
Long before zinc was smelted in Europe, it was being sold there by Portuguese and English
traders who brought it from the Orient Zinc was being imported by the East India Company
from about 1605 onwards At this time, the zinc was added to copper to make brass [1]
Lead ores are often contaminated with zinc because the two metals occur together Small
amounts of metallic zinc were obtained as a by-product of the lead industry and Agrlcola men-
tloned the formation o f " z l n c u m " in the furnaces of Silesia This is probably the first Indica-
tion we have in the West of any attempt to recover metallic zinc The credit for the first mten-
tlonal production of metallic zinc in the West is given usually to Wllham Champion who
developed a vertical retort method in 1738 Rows of horizontal retorts, which are more ther-
mally efficient and, therefore, more economical, were installed by the Abbe Dony at Liege,
Belgium, in 1807 [2]
The first recorded experiments for producing zinc coatings by the dipping process are those
of a French chemist, Melouin, in 1741 [4] Tinned iron was already known at that time and
Melouln attempted to zinc coat iron sheets in a similar manner by immersion In a bath of
molten zinc The results of his experiments formed the basis of a report to the Academ~e Roy-
ale in 1742. Interest in Melouin's discovery spread through the scientific circles in Pans The
first application that was attempted was to use molten zinc as a cheap protective coating for
household utensils Zinc was used to replace tin, which had become too expensive for the poor.
In 1742, Jean-BaptIste Kemerhn applied this process for coating iron kitchen utensils and
these products were fairly well known in parts of France during the second half of the eigh-
teenth century [4] In 1778, however, it was discovered that the zinc became corroded by
orgamc acids and that the salts found on the zinc were poisonous Interest in hot dipped zinc
coatings then dechned
In 1780, the Italian, Lulgl Galvani, discovered the electncal phenomenon of the twitching
of a frog's leg muscles when contacted by two dissimilar metals, namely, copper and iron. Gal-
vain incorrectly concluded that the source of the electricity was in the frog's leg. Expenments
with dissimilar metals were further pursued by another Italian, Alessandro Volta, who came
to believe that the flow of electrical current was caused by the contact of the dissimilar metals
themselves. In 1800, Volta was able to prove this by constructing a stack of alternating zinc
and silver plates with a piece of cloth soaked in a salt solution between the individual plates.
This device, known as a Voltaic pile, was the world's first battery
Electrodeposmon of zinc in the laboratory occurred in 1800, the same year that Volta devel-
oped the voltaic pile. In September of that year, the German physiost, Johann Rltter, used
Volta's battery to deposit zinc on iron [5 ]. In 1805, an early Bnhsh patent was issued to Charles
Hobson, Charles Sylvester, and John Moorhouse for a method of coating nails and bolts by
placing them in a galvamc pile with zinc and seawater [5] Full commercial utihzation of zinc
plating processes had to walt until the end of the nineteenth century until electric dynamos
and generators became available.
In 1824, Sir Humphrey Davy showed that when two dissimilar metals were connected elec-
trically and Immersed in water, the corrosion of one was accelerated while the other received
a degree of protection From this work he suggested that the copper bottoms of wooden naval
ships could be protected by attaching iron or zinc plates to them, the earliest example of prac-
tical cathodic protection When wooden hulls were superseded by iron and steel, zinc anodes
were still used
In 1836, Sorel in France took out the first of numerous patents for a process of coating steel
by dipping it in molten zinc after first cleaning it with 9% sulfuric acid and fluxing it with
a m m o n i u m chloride He provided the process with its name "galvanizing." It is interesting to

note that Sorel was aware of the electrochemical nature of corrosion and the sacnficlal role of
the zinc coating on the iron. Originally, the word galvanizing did not refer to the process of
coating but to the fundamental property offered by this coating [4].
In addition to Sorel's patent of 1836, a British patent for a similar process was granted in
1837 to Wllham Crawford By 1850, the Brltlshgalvanizlnglndustrywasusing l0 0 0 0 t o n s o f
zinc a year for the protection of steel [6] Early corrugated galvanized steel, used as a roofing
material, found its way to both Australia and California dunng the gold rush of 1849
In the beginning, individual sheets of iron had to be hot-dipped by hand The Sendzlmir
coating process was the first to attain commercial success by fulfilling the basic coating require-
ments in a continuous galvanizing operaUon A coating line was installed by the Armco Steel
Corporation at Butler, Pennsylvania, in 1936 and proved the soundness of the process [3]
Metallurgically, this process suppresses the formation of the bnttle iron-zinc alloy layers at the
steel/coating interface by the addition of 0 2% aluminum to the bath By minimizing the thick-
ness of the bnttle iron-zinc alloy layers, the ductility of the coating is improved The beneficial
effects of aluminum alloy additions to the zinc bath were first discovered in the early twentieth
century, and research in this area was later performed by Babhk and others
Case History 1
Several pieces of galvanized steel strip were experiencing a problem with the galvanized
coating Small blisters were observed on both sides of the sheet The strip was first passed
through a furnace to oxidize and remove any oil residues The stnp was then annealed in a
furnace containing a hydrogen atmosphere and finally hot-dip galvanized
Visual Inspection
The hot-dipped galvanized coating on both sides of the steel strip possessed numerous very
small blisters The blisters were distinguishable by an increase in reflectivity caused by their
raised surfaces It was found that rubbing the blisters with a fingernail or other object would
flatten the zinc coating over the bhster and so eliminate it
Metallographlc Inspection
Transverse sections through the galvanized steel in the bhstered areas were prepared for sub-
sequent metallographlc inspection In the as-polished condition, the bhsters were observed as
small arches in the coating with complete separation occurring at the zinc/steel interface (Fig
1) At high magnifications, small gray inclusions were observed on the steel surface within the
cavity (Fig 2) The inclusions were examined using a scanning electron microscope equipped
with an energy-dispersive X-ray spectrometer Only iron was observed The equipment cannot
detect the presence of elements in the first row of the periodic table such as carbon, oxygen,
nitrogen, etc Based upon the appearance of the inclusions, and the absence of any elements
other than iron, the inclusions are most hkely iron oxide
Results
The blisters in the galvanized coating appear to have been caused by gas accumulation at
the interface between the steel and the zinc coating Iron oxide inclusions were observed within
the blister cavities The following mechanism is responsible for the bhstenng problem ( 1) the
as-received steel strip probably was incompletely pickled, which left iron-oxide scale at small
FIG 1--Pholograph at X 200 showing a bhster under the galvamzed coating, as-pohshed
isolated locations, (2) dunng plckhng and later anneahng, hydrogen was absorbed by the steel,
(3) during galvamzmg, the heat from the molten zinc caused the hydrogen to diffuse out of the
steel, and (4) at locations where surface oxides existed, the atomic hydrogen was able to recom-
bine to form diatomlc molecular hydrogen gas that raised the surface of the coating, forming
the observed bhsters
FIG 2--Photograph at X 500 showmg scale parttcles within a bhster, as-pohshed
To eliminate this problem, it was suggested that the surface oxides be ehmlnated completely.
Thin will not prevent hydrogen absorption but should prevent the formation of gas blisters
when the hydrogen diffuses out of the steel during galvanizing.
Case History 2
One section of a formed (bent) galvanized steel sheet cracked during bending. The objective
o f the investigation was to determine the cause of the cracking
Visual Exammatlon
The cracked part was observed to have been bent in two perpendicular directions as indi-
cated by arrows (Fig 3) A large crack is visible that had lmtlated at the thin edge (steel sheet
thickness) The crack occurred at the outside diameter surface ofthe second bend where tensile
stresses dunng forming would be expected to be greatest The fracture surfaces of the large
crack were examined with the aid of a scanning electron microscope and were observed to
possess a dimpled structure that is indicative of a ductile mode of failure resulting from a ten-
slle overload (Fig 4)
Numerous small cracks, parallel to the p n m a r y crack, were also observed along the thin edge
of the sheet (Fig 5) This edge of the steel sheet appears to have been produced by sheanng.
Metallographtc Exammatlon
Transverse and longitudinal sections through the galvamzed steel sheet were prepared for
subsequent metallographlc examination In the as-polished condmon, some sulfide inclusions
were observed Most of the cracks appear to have lnmated at the surface of the material (Fig.
FIG 3--Photograph at • 1 8 showmg the locatton of the cracks m theformed part
FIG 4--Photograph at X 400 showmg the fracture surface of the larges't crack
FIG 5--Photograph at X 20 ~howmg smaller cracks m the sheared edge of the part
FIG 6--Photograph at X 200 ~howmg a crack m the sheared edge o f the material, 2% total
6), but a few small cracks were observed to have originated at subsurface sulfide Inclusions (Fig
7)
Etching with a 2% nltal solution revealed the existing microstructure of the steel sheet that
was found to consist of spheroldlzed carbide particles in a matrix of equlaxed grams of white
etching ferrlte The mlcrostructure adjacent to the edge where the cracking mmated was
observed to possess highly elongated ferrlte grains, indicative of the plastic tensile deformation
that was produced during the shearing operation (Fig 8)
Mwromdentat~on Hardness
A Knoop microlndentation hardness survey, using a 200-g load, was performed on one of
the metallograph~c specimens and the results are presented m Table 1 The hardness of the
sheared surface was found to be significantly higher than the material at an undeformed
location
Results
The formed galvanized steel part was found to have failed as a result of cracking that had
mitmted at the thin edge (sheet thickness) of the sheet that was located at the outside diameter
surface of a bend The edge where the cracking initiated had been produced by shearing and
possessed a plastically deformed m~crostructure with a hardness s~gnlficantly greater than that
of the undeformed base metal The fracture surface of the large primary crack indicated that
failure occurred as a result of a tensile overload
For a ferrltlC steel to successfully withstand forming operations, good ductility IS required
FIG 7--Photograph at • 500 showmg a crack orzgmatmg at a subsurface sulfide mcluswn, as-pohshed
FIG 8--Photograph at • 200 showmg the mwrostructure o f the sheared edge, 2% nttal
TABLE 1--Mtcromdentatlon hardness of sheared edge
Location
(mdhmetres from surface) HK Approximate HRB
Sheared edge, 0 05 253 100 4

Sheared edge, 0 10 253 100 4
Sheared edge, 0 15 234 96 6
Base metal 111 54 0
Base metal 111 54 0
Base metal 107 50 0
Good ductlhty occurs in the softer tempers of steel The shearing, which was performed to
produce the edge of the sheet, has locally cold-worked and hardened the steel This harder
material at the surface did not possess sufficient ductility to withstand the subsequent forming
operations and therefore cracked
Case History 3
Sections of two corrugated, galvanized, and painted sheet steel panels were examined One
of the panels had detenorated in service developing both white and red rust under the paint
primarily at the locations of the bends in the corrugation The second panel was reported to
be a spare panel from the original project that had never been placed m service and had been
kept in an indoor environment The material was used m an outdoor environment as roofing
material for a building The material was designed to give 20 years of service life but had begun
to deteriorate after only one year
Visual Inspectton
The deterioration of the paint on the exposed panel was found to have occurred on the exte-
rior side of the panels only at the locations of the bends in the corrugation Furthermore, the
corrosion occurred only where the bends in the corrugation placed the coating system in ten-
sion No detenoraUon was observed along the flat portions of the steel sheet or where the bends
in the corrugation placed the system in compression The detenoratmn of the exposed panels
consisted mostly, at th~s time, of white rust that caused the overlying paint to peel and have a
bllstered appearance (Fig 9) Red rustlng ofthe steel was observed at a few locatlons (Fig 10)
The angle of the corrugation was found to be approximately 120 ~ and the angles were not
sharp
The surfaces of the paint, at the location of the bends, were further examined using a scan-
ning electron microscope The surface of the paint in nonbllstered areas was observed to pos-
sess a wrinkled appearance with numerous shallow, parallel furrows (Fig 11) At locations
close to where white rusting had occurred, numerous small cracks in the paint were found (Fig
12)
FIG 9--Photograph at X 2 +howtngpatnt bhstermg and whzte rust
FIG lO--Photograph at ><2showmg palnt bhstermg and red rustmg of the steel substrate
FIG 1 l--Photograph at X 5 5 showmg wrinkles m the pamt at the bend locatton
FIG 12--Photograph at X 110 s'howmg cracks m the pamt at the bend locatton
Metallographlc E.~amtnatton
Cross secUons through both the exposed and unexposed panels at the location of the bends
and at undeformed areas of the panels were prepared for metallographlc examination For
both panels, the steel substrate thickness was measured to be 0 864 m m (0 034 in ) with a gal-
vanized coating 0 020 m m (0 0008 in ) thick The p n m e r coating was measured to be 0 005
m m (0 0002 in ) thick and the polyvlnyhdene fluoride (PVDF) top coat was measured to be
0 028 m m (0 0011 in ) thick Energy dispersive spectrometer (EDS) analysis ofa delamlnated
section of the paint indicated that a chromate wash p n m e r had been applied to the zinc pnor
to painting
Etching with a 1% nltal solution revealed the presence of a very thin iron-zinc alloy layer
The remainder of the galvanized coating consisted of free zinc with a hardness of approxi-
mately 54 HV However, at all locations within the galvanized layer of the two panels, dark
grain boundary precipitates were observed (Fig 13) Away from the bend areas, the lntergran-
ular precipitates were very thin in appearance while close to the bend areas, these precipitates
have a wider appearance that is attributed to internal cracking along these gram boundary
films
Immediately above some of the cracks in the galvanizing, localized plastic deformation of
the paint layer was observed (Fig 14) This locahzed deformation of the paint was responsible
for the observed w n n k h n g At other locations, cracking of the paint and intergranular cracking
ofthe zlnc were observed (Fig 15) Unlform white rust formation was observed to be spreadlng
away from the bend areas underneath the paint layer (Fig 16)
The precipitates were further examined using a scanning electron microscope equipped with
an energy-dispersive X-ray spectrometer The lntergranular precipitate in the zinc coating
were found to contain iron, slhcon, and calcium Based upon the EDS analysis and the gray
color of the precipitate under an optical microscope, we believe the matenal is an oxide impu-
rity in the molten zinc bath that segregated to the grain boundanes d u n n g sohdlfiCatlon No
aluminum, tin, lead, or cadmium were found w~thln these precipitates
Results
The white rusting of the galvanized layer and red rusting of the steel substrate appear to have
been caused by a rupture of the paint film at the location of the bends in the corrugation
However, it appears that lntergranular precipitates in the galvanized layer have reduced its
ductility and it is the galvanized coating that cracked first and then placed stress on the paint
film
Conclusion
The art and science of galvanizing is now 150 years old Modern improvements include
continuous coating and painting of steel sheet and alloying additions, such as aluminum to
improve ductility of the coating by suppressing iron-zinc alloy layer formation However, as
with any h u m a n endeavor, actual practice can deviate from theory and produce a less than
ideal product Two of our case histories deal with such defects Sometimes an end user of a
product will erroneously blame the material for any difficulties encountered d u n n g subse-
quent manufacturing operations as illustrated by our second case history In this paper, we
have shown how metallography can be used to determine the mechanism of failure of zinc-
coated steel products
FIG 13--Pholograph at )<500 shorting mtergranular pre~zpttatlon m the galvamzed coatmg, as

poh~hed
FIG 14--Photograph at • 5 O0 showmg locahzed de/ormauon oj the paint layer, a s'-pohshed
FIG 15--Photograph at X 500 showing cracking along the zmc gram bounda~les, a s'-pohshed
FIG 16--Photograph at • 500 showing whtte rust ]orrnatlon under the paint, as-pohshed
References
[ 1 ] Weeks, M E, "The Discovery of the Elements," Journal of Chemtcal Education, 1933
[2] Tylecote, R F, A Htstory of Metallurgy, The Metals Society, London, 1976
[3] Mathewson, C H , Zinc, The Scwnce and Technology of the Metal, Its Alloys and Compounds, Amer-
scan Chemical Society, New York, 1959
[4] Smith, A, Early Hot Galvantzmg, Product Fmtshmg, May, June, July 1980
[5] Geduld, H , Ztm Plating, Amencan Society for Metals and Metal Finishing Ltd, 1988
[6] Smith, C A , "A Review ofGalvamzmg m the Nineteenth Century," Sheet Metallndustrtes--Annual
Revww, Aug 1978
Herbert J. Muelle/
Characterization of Reaction Between Cast

Titanium and Silica-Containing Investment
Mold
REFERENCE. MueUer, H J , "Characterization of Reaction Between Cast Titanium and Sihca-
Containing Investment Mold," Metallography Past, Present, and Future (75th Anmversary Vol-
ume), ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds,
American Society for Testing and Materials, Philadelphia, 1993, pp 429-445
ABSTRACT. Scanning electron microscopy and energy dispersive spectroscopy analysis were
used to characterize the interracial reaction layer for a system compnsed of commercially pure
titanium cast into an incompatible silica-containing investment mold This layer was compared
to bulk mold material Results of this comparison revealed that cnstobahte was converted into
a vitreous glassy SlhCa phase to a depth of about 500 ~m Both a light and a darker appeanng
vitreous phase was identified The former was associated with coalescence of original cnstobalite
particles and the latter with degradation of the magnesium phosphate matrix The silicon-to-
oxygen ratio of the light phase was significantly higher than that of darker phase Both phases
were contaminated with magnesium, phosphorus, chlorine, calcium, and titanium Slhcon was
detected only short distances within the titanium substrate The lnterfaclal layer formed when
molten titanium was cast into a quartz-containing Investment, which is compatible with t~ta-
mum castings, displayed similar microstructure to the bulk mold material The violent reaction
between crlstobahte and molten titanium could have been due to contamination of cnstoballte,
either occumng naturally or from setting and heating of the phosphate matrix This resulted in
a lowenng of the melting temperature of cnstobahte and inducing the formation of metal slags
and vitreous glassy silica with various Stolchlometncs Molten cnstobahte also emitted its gas-
eous contaminants that reacted with molten titanium both embntthng the metal and providing
the source of the porosity
KEY WORDS. commercially pure titanium, investment casting, silica, quartz, cnstobahte,
phosphate-bonded mold, heat affected zone, vitreous glassy slhca, metal oxide slags, metallog-
raphy, metallurgical specimens, mlcrostructure, metallograph~c techmques
Casting processes for t i t a n i u m net shapes utlhze either a n i n v e s t m e n t shell or r a m m e d

g r a p h i t e m o l d system In t h e i n v e s t m e n t system, a wax p a t t e r n is d i p p e d into a c e r a m i c slurry
After d r y i n g a n d o v e n curing, the i n v e s t m e n t b e c o m e s a rigid shell t h a t will w i t h s t a n d the
stresses o f centrifugal casting a n d will r e m a i n relatively n o n r e a c t i v e to m o l t e n t i t a n i u m T h e
r a m m e d g r a p h i t e system consists o f a m i x t u r e o f g r a p h i t e p o w d e r a n d a b i n d e r t h a t is com-
p a c t e d i n t o a m o l d a r o u n d a rigid p a t t e r n T h e i n v e s t m e n t casting process is preferred for cast-
m g small intricate parts [1] T h e i n v e s t m e n t m o l d system c h o s e n as well as post casting pro-
cessing affect properties o f t h e final casting [2]
In t h e casting o f d e n t a l c o m p o n e n t s , i n c l u d i n g crowns, inlays, a n d onlays, shrinkage of
m e t a l d u r i n g solldlficaUon f r o m the m o l t e n state is c o m p e n s a t e d for by e x p a n s i o n s t h a t o c c u r
1 Research assocmte, Councd on Dental Materials, Instruments and Equipment, Amencan Dental
Association, Chicago, IL 60611
429
Copyright
Copyright*by1993
ASTMbyInt'l
during the setting and heat treatment of the investment mold Constructing oversized patterns
as is done for other commercial apphcations is not done with dental components due to the
complexity of most crown forms A wax pattern is made from a model that duplicates the exact
dimensions of the part to be cast The wax pattern is invested, and the resulting mold space
expands during setting and heating of the investment material This expansion, which is on
the order of 2% of linear dimensions, is used to counterbalance contractions that occur when
molten titanium is cooled A finished dental casting prepared under these conditions will be a
good fitting prosthesis and will resist mlcroleakage between the casting and the walls of the
prepared tooth
Techniques have been developed for the investment casting of gold, mckel-chromium,
cobalt-chromium, and other alloys In these procedures, investment slurries are poured into a
casting ring that surrounds a wax pattern These slurries contain refractory silica particles
together with gypsum, phosphate, or silicate binders These slumes set up in a short time to
form rigid shells with good unfired strength Some expansion occurs during the set-up process
Further expansion occurs during preheating of the invested pattern prior to casting D u n n g
the preheating cycle, the wax pattern is also burned out of the investment
Dental investment casting techniques have been developed for making titanium parts [3]
These methods are similar to those used for shell investment casting but make use of invest-
ment materials that expand upon setting and heating Since molten titanium reacts with silica,
mold materials that do not contain silica refractory have been used These include alumina-
silicates, magnesia, zirconia, and other refractory oxides [4]
Phosphate-bonded molds, which contain refractory silica particles in a matrix of magne-
sium phosphate, have gained some popularity for the casting of dental components Some
phosphate-bonded materials are compatible with the titanium-casting process, even though
the investments contain silica Other investments made from this type of material react vio-
lently with molten titanium It has been recognized [5,6] that the possible reason for this &f-
ference in behavior between phosphate-bonded investment mold materials could be due to
the cristobahte-to-quartz ratio in the sihca refractory
The purpose of this project was to study the interface that forms during the casting of com-
mercially pure titanmm in an incompatible phosphate-bonded investment mold by micro-
scoplc techmques Comparative studies were also made for a phosphate mold material that is
compatible with titanium
Materials and Methods

Sample Preparations
Samples of materials that had been evaluated previously [5] were used These were two com-
mercial phosphate-bonded investment molds, Rema Exakt (Dentaurun, Inc, Newtown,
Pennsylvania) and Blovest (Densply International, York, Pennsylvania) In each sample, a
powder and a colloidal slhca solution were supphed The matenals were mixed according to
the recommended liquid-to-powder (volume/weight) ratios, these being 0 16 and 0 18, respec-
tively Mixing was done mechanically at 430 r/mln for a period of 45 s under a vacuum of 25
m m of mercury The mixture was poured into one end of a metal ring 30 m m diameter by 35
m m long The crucible former containing the prepared wax pattern was secured onto the
opposite end of the n n g that also provided a vacuum seal The wax pattern, simulating the
dental prosthesis to be cast, was prepared on a truncated stainless steel cone, 8 m m m diameter
at the base, 8 m m m height with a total taper of 10* A 10-mm-inner-&ameterrang was secured
concentncally around the base of the cone and provided space for the softened wax to be
inserted under pressure A wetting agent was applied to surfaces of the finished wax pattern
MUELLER ON INVESTMENT CASTING 431
before investing The invested wax pattern was allowed to set for 1 h at 25~ followed by heat-
ing to the burn-out temperature of the wax The investment mold was then heated to the rec-
ommended soak temperature of 860 and 1000~ for the Blovest and Rema materials and held
for 1 h The investment mold was air-cooled to room temperature before casting began Com-
mercially pure titanium was melted by an argon pressure-vacuum arc melting apparatus in a
water-cooled copper crucible and transferred by gravity and vacuum to the investment mold
[3] The cast samples were allowed to air-cool to room temperature A careful examination of
the quality of the castings was made with particular attention being given to the metal-invest-
ment mold interface reaction
Metallographw Preparation
Samples of the bulk Investment mold and sections cut through the investment mold-metal
reaction zones were lmtmlly vacuum impregnated with resin This was done to facihtate gnnd-
lng and polishing to avoid pulhng out investment particles Surfaces used for examinations
were ground successively with 240-, 320-, 400-, and 600-grit silicon-carbon abrasive papers
This was followed by polishing with diamond spray or paste ranging in size from 15, 6, 3, 1
and 0 25 ~m Struers D U R - M O L series of polishing cloths were used with DP blue lubricant
Microscopy
All prepared surfaces for scanning electron microscopy (SEM) were coated with a thin film
of carbon to prevent charging A Cambridge Mk II scanning electron microscope and a Prance-
ton G a m m a Tech energy disperswe spectrometer (EDS) were used for the analysis Both the
secondary electron (SE) and back scattered electron (BSE) modes and combinations thereof
were selected The software programs permitted semiquantitatlve analysis when corrections
for atomic number, absorption, and fluorescence (ZAF) are taken into account A feature of
the software allows compositions to be calculated based upon standardless analysis. Both area
and spot analysis were performed depending upon the size of the area for analysis All spectra
were collected for 500 s
Results
Compatibility of Tltamum-Investment Combmauons
Molten titanium reacted spontaneously with the Blovest investment mold but did not react
with the Rema mold material The casting made with the Biovest mold was bnttle and porous
It was unacceptable for use as a dental prosthesxs The casting did not form the design geometry
required as expected Several mllhmetres of the investment mold remained attached tena-
ciously to the surface of the metal The investment mold appeared to be darkened at the inter-
face around the casting and in the investment mold well away from the casting The titanium
part cast into the Rema investment mold did not show any of the adverse effects shown by the
Biovest mold The Rema mold was defined to be compatible for use in casting titanium parts
Micro vcopy Representattve of Bulk Investments

Figures l a and 2a illustrate BSE images for bulk samples from Rema and Biovest invest-
ment molds, respectively Both microstructures show refractory particles embedded in a
matrix In the Rema investment mold, the refractory particles appear to be composed of ele-
ments with similar atomic weights based on the similar contrast intensities in the photographs
FIGS 1( a - c ) - - S E M photomtcrographs of Rema with back-scattered electron~ (Ftg 1a), and secondary
electrons (Flg~ lb and c) EDS area analysts of Fig la as well as of only a parttcle are presented m
Table I
FIGS 2 ( a - c ) - - S E M photomlcrographs of Blove~t wtth back-scattered electrons (Ftg 2a), and second-
ary electrons (Ftgs 2b and c) EDS area analysis o f Fzg 2a as well as o f only a bright or a darker parttcle
are presented m Table 1
TABLE 1--EDS composztzonalanalysis (atomicpercent)

Sample Fig Region $1 O Mg P CI Ca Tl Zr
Rema a la area 29 19 65 98 2 85 1 33 0 18 0 04 0 0
Rema la particle 33 29 66 67 0 0 04 0 0 0 0
Biovest 2a area 27 34 65 96 3 11 2 78 0,14 0 18 0 05
Blovest 2a bt part b 20 00 66 67 0 0 0 0 0 13 3
Biovest 2a dkpart c 33 20 66 68 0 0 11 0 0 0 0
Blo/TI 4~ (1) 1864 285 1405 d 022 076 767 558
Blo/T~ 5b (2) 33 l0 66 70 0 0 20 0 0 0 0
B~o/T1 5b (3) 27 38 65 13 0 97 1 58 2 18 1 16 1 61 0
Blo/T1 5b (4) 32 88 66 73 0 0 38 0 0 0 0
BIn/T1 5b (5) 6 72 58 56 18 65 6 19 3 92 2 88 3 07 0
BIo/T1 6a (6) 95 72 1 97 0 1 34 0 47 0 30 0 21 0
BIo/T1 6a (7) 95 80 1 90 0 1 39 0 48 0 25 0 18 0
Blo/Tx 6a (8) 9560 202 0 1 30 051 032 026 0
BIo/T~ 6a (9) 45 07 37 92 1 22 1 80 4 81 4 62 4 55 0
Blo/T~ 6a (10) 4446 3086 341 3 10 1277 242 297 0
B~o/T~ 6a (11) 6707 5 39 1005 11 83 1 82 266 1 16 0
B~o/T~ 8a (12) 0 0 0 0 0 0 100 0
Bm/T1 8a (13) 11 22 51 62 0 1 80 0 0 35 35 0
Blo/Ti 8a (14) 3 30 58 11 0 1 26 0 0 37 32 0
Blo/T1 8a (15) 6942 24 13 204 1 09 009 028 295 0
Blo/T1 8a (16) 71 67 24 97 0 1 43 044 0 35 1 14 0
BIo/T1 8a (17) 6760 2302 3 19 506 043 034 037 0
Blo/Ti 8a (18) 21 60 75 97 007 0 0 34 066 1 36 0
BIo/TI 8d (19) 1083 8647 0 16 0 001 086 l 67 0
Blo/T1 8d (20) 57 47 38 06 0 1 91 l 27 0 66 0 64 0
Blo/T1 8e (21) 2991 5892 251 476 131 148 l ll 0
0 43% sulfur also detected but not m any other analysis

b Brighter particles
c Darker particles
d Some phosphorus remained, the exact amount was not determined due to overlapping of Pk and ZrL
X-ray emission energies
T h e Biovest m a t e r i a l was c o m p o s e d o f at least two distract types o f refractory particles as evi-

d e n c e d b y the a p p e a r a n c e o f b o t h bright a n d d a r k e r particles in the m a t r i x Table 1 presents
d a t a f r o m E D S area analysis B o t h i n v e s t m e n t m o l d s were f o u n d to c o n t a i n silicon, m a g n e -
sium, c a l c i u m , p h o s p h o r o u s , a n d c h l o n n e A n e s t i m a t e o f oxide c o n t e n t was possible in the
c o m p u t e r analysis b y t a k i n g i n t o a c c o u n t t h e oxides t h a t f o r m with the e l e m e n t s detected T h e
R e m a i n v e s t m e n t m o l d also c o n t a i n e d low b u t detectable a m o u n t s o f sulfur n o t detected in
t h e Blovest b u l k s a m p l e T h e Blovest s a m p l e c o n t a i n e d slgmficant a m o u n t s o f z i r c o n i u m t h a t
were n o t detected in t h e R e m a sample, E D S spot analysis o f t h e refractory particles are also
s h o w n in T a b l e 1 T h e particles in the R e m a s a m p l e a n d t h e d a r k e r particles (dk part) m the
Blovest s a m p l e were essentially S102, s l h c o n dioxide In t h e b r i g h t e r particles (bt part) f o u n d
m the Blovest sample, z i r c o n i u m h a d replaced a b o u t 13 a t o m i c p e r c e n t o f the silicon present
Porosity was d e t e c t e d in b o t h structures Figures 1b, 1 c, 2b, a n d 2c are higher m a g n i f i c a t i o n
views o f b o t h s u b s t a n c e s p r o d u c e d by using t h e s e c o n d a r y e l e c t r o n m o d e B o t h structures evi-
d e n c e d a d i s t r i b u t i o n o f particle sizes
Investment Mold Degradanon Away from Interface

E v a l u a t i o n o f Biovest b u l k samples s h o w e d d e g r a d a t i o n o f the i n v e s t m e n t m o l d t h a t was
detected occasionally at distances u p to 1 m m or m o r e Figure 3 dlustrates a degraded region
FIG 3--SEM photomzcrograph oJ degraded area m Blovest about 0 5 mmjrom tltamum interface
that was found about 0 5 m m from the interface The abnormal appeanng microstructure In
the center o f the mlcrograph ~s magnesium- and phosphorous-rich but is depleted in silicon
Porosity was also found to be highly concentrated in this area
Mtcroscopy Representattve o f Reacted Interface

Figure 4a shows a low magnification view of the Biovest layer that remained tenaciously
attached to the cast titanium surface Bright refractory particles were easily detected in areas
both near and at some distance away from the tnanlum interface EDS analysis of the bright
particles found in this layer showed results identical to the results presented in Table 1 (Fig
2a) for the bnght particles found in bulk samples of the Blovest investment mold Figures 4b
and c show higher magnification mIcrographs of the bnght particle found directly next to the
titanium interface m the lower center o f Fig 4a EDS analysis o f material located with the
interface region between the particle and the titanium substrate is presented in Table 1 and
labeled as the region or spot analysis ( 1 ) for Fig 4c This was the only analysis where zlrco-
mum was detected except for the bnght refractory particle found in Blovest samples No reac-
tion was noted between particles containing zirconium and the surrounding glassy phase when
the particles containing zirconium were located away from the interface (Fig 4d)
Another obvious mlcrostructural characteristic was found in the investment mold layer
attached to the titanium casting As the interface layer was approached, larger-sized patches
similar to refractory particles were found Figures 5a and b show typical areas EDS analysis
of the larger-sized region to the right of the lnterfaclal zone boundary shown in Fig 5b labeled
(2) identified primarily silicon-dioxide that contained low levels of phosphorous Similarly,
an "island" of material to the left of the boundary labeled (3) analyzed very close to the com-
position of sxhcon-dioxlde A spot located at the interface and labeled (4), showed a greater
deviation from the normal composition of silicon-dioxide This deviation is explained by the
replacement o f silicon by magnesium, phosphorous, chlorine, calcmm, and titanmm in the
FIGS 5(a-b)--SEM photomicrograph at low magn~catlon of a larger partide-hke region (Fig 5a),
and at higher magn~catlon partly showing partzcle separated from surrounding material by boundary
zone (Fig 5b) EDS spot analyszsJor regions labeled (2), (3), (4), and (5) presented in Table 1
lnterfaclal reaction zone Another spot labeled (5), corresponds to another EDS analysis
within the zonal boundary The analysis of this spot showed slgmficant levels of magnesmm,
silicon, calcium, phosphorous, chlorine, and tltamum
Another spot analysis done outside the field of view of the titanium substrate is shown m
Fig 6a Analysis of regions labeled (6), (7), and (8) indicated a very high content ofsihcon
The darker inter-particle material labeled (9), (10), and ( 11 ) displayed lower silicon content
FIGS 6( a-b ) - - S E M photomlcrograph of regton lu.st outs'tale the wew of the tttantum mterjace (bSg 6a)
E D S spot analy~l ~for regtons labeled (6), (7), ( 8 ), ( 9 ), ~10 ), and ( 11 ) are presented m Table 1 Higher
magmficatlon oJ one partl~ ular darker-appearing regton above regton labeled (6) ~hown m Fig 6b
and much greater contents of other elements m the system A higher magmficatlon view of the
darker matnx or inter-particle material located above the region labeled (6) in Fig 6a is shown
in Fig 6b
A view of an area from the titanium-investment mold interface ~s shown in Fig 7 This
mlcrograph clearly reveals the coherency of the attachment of the lighter-appearing glassy
phase to the surface of the metal Mlcrocracks w~thln the mterfacxal layer are also shown These
cracks reveal the brittle nature of the vitreous glassy phase formed
MUELLER ON INVESTMENTCASTING 439
FIG 7 - - S E M photomicrograph o f a regton correspondmg to both titanium substrate and to reacted

mterfacml zone
The last specific region analyzed is shown in the series of micrographs presented in Figs 8a
through d This region represents material located between the titanium casting and the invest-
ment mold Analysis of the region labeled (12) revealed only titanium Analysis of the regions
labeled (13) and (14) Indicated that high levels of titanium can occur in areas seemingly
within the investment mold In these areas that contain higher oxygen levels and low silicon
content, titanium has been oxidized to a Stolchlometry approaching that of tltanluJn-dloxide
Figures 8b and c are elemental maps of titanium and silicon, respectively, for the area shown
in Fig 8a Regions labeled (15), (16), and (17), correspond to the lighter-appeanng glassy
phase and display low but significant contributions from magnesium, phosphorous, calcium,
chloride, and titanium Figure 8d shows the network of dark "Inter-island" material near the
interface Regions labeled (18) (Fig 7a) and (19), (20), and (21) in Fig 7d all correspond
to darker inter-particle material Data from the analysis of these regions confirmed the large
variations in composition and the lower silicon to oxygen ratios when compared with the
lighter-appearing glassy phase
Discussion
Phosphate-Bonded Investment Molds
Magnesium-oxide and ammonlum-dlhydrogen phosphate particles, which are dispersed

with the silica refractory particles, react after being mixed with a colloidal silica solution
Ammonium-magnesium-phosphate hexahydrate is an amorphous phase that initially forms
Upon heating, the water of hydration and the ammonmia are driven off as gaseous by-prod-
ucts An amorphous magneslum-pyrophosphate phase, MgzP207, forms above 200~ which
subsequently becomes crystallized above 600~ The pyrophosphate also reacts with
unreacted magnesium-oxide to form magneslum-orthophosphate, Mg3(PO4)2 [ 7]
,4~v
~v
~v
~rN
Slhca
There are at least three polymorphs of sd~ca, including quartz, trldymite, and cnstobahte
[8] Thermodynamically, quartz is the most stable form and cnstobahte the least stable form,
with heats of formation [9] being 2 3 and 1 2 kg cal/mol, respectively Quartz is stable below
870, tndymlte below 1470, and cnstobahte below 1700*C Since the transformation of one
polymorphlc form to another requires a marked change m the linking of the S104 tetrahedrons
[10], the transformations are extremely slow resulting m the existence of metastable states.
The conversion ofquartz to cnstobalite is both time and temperature dependent [11 ] Melting
temperatures vary, being 1610~ for quartz, 1703"C for tndym~te, and 1713~ for cnstobahte
[12] In addmon, each polymorph has a high- and a low-temperature modification Vitreous
silica, an amorphous form, can also exist in the supercooled or metastable condition at all
temperatures below its melting temperature
Slag Formatton
The reason that the Blovest investment mold reacted with tltamum was due to the hque-
faction of silica that subsequently converted to a glassy vitreous slag. These slags have a wide
range of oxygen stolchlometry varying from the expected ratio of I 2 for pure silicon-dioxide
that exists m unreacted material Both sd~con-nch and slhcon-depleted ratios were detected.
These areas ranged from a high of 95 8 to a low of 3 3% silicon that corresponds to silicon-to-
oxygen (SI O) ratios of 50 4" 1 and 1 17 6 The pure s~hcon-dloxlde material was converted
into a v~treous slag form that contained other investment elements, including magnesmm,
phosphorus, chloride, calcmm, as well as titanium. The concentrations of these contaminants
as compared to bulk control material increased enormously m selected instances. The
X(contammant):Sl ratios changed from a normal ratio of 0 33 to ratios of 2 8, 0 9, 0 6, 0 4,
and 11.3 for magnesium, phosphorous, calcium, chloride, and Utanium, respectively. Inspec-
non of the S102-MgO, S102-P205, S102-CaO, and SIO2-TIO2 phase diagrams [ 13] reveal eutec-
tic reactions occurring at 1543,975, 1436, and 1550~ respectively (Table 2), which are below
1670~ the melting temperature oftitamum Additional binary systems capable of hquefying
components at or below the melting temperature of titanium include MgO-P2Os (600~
CaO-P205 (500~ P2Os-MgO (1543~ MgO~T102 (1600~ and CaO-T102 (1475~
Vitreous silica within the mterfacml region included both lighter- and darker-appeanng
material The hghter-appeanng form occupied most of the area fraction This form appeared
to coalesce silica particles The darker form appeared to be remnants of the magnesium-phos-
phate matnx The darker-appearing form, m most instances, was detected to contain lower
SI O ratios It also appeared that this form had a lower melting temperature range, since it
appeared to have flowed between lighter-appearing regions
TABLE 2--Lowest eutecttc temperatures (~

Binary System
Binary
System SIO2 MgO P205 CaO TlOz ZrO2
SIO2 1723 1543 ~975 1436 1550 1675
MgO 2800 1543 2370 1600 2100
P205 ~-600 ~500
CaO 2570 1475 2260
TIO2 1825 1760
ZrO2 2700
Ztrcomum-Contammg Refractory
One apparent difference in mlcrostructure between Blovest and Rema shown in Figs 1 and
2 IS the bnght-appeanng zirconium containing refractory particles present m the Blovest sam-
ple These particles did not appear to react with molten titanium with the same spontaneity
shown by the darker-appeanng particles In fact, zirconium-containingparticles were detected
throughout the lnterfacial region and with no evidence for any apparent conversion in form
Only a selected few particles found exactly at the interface between the investment mold and
the titanium substrate showed any indication of reaction This IS shown m Fig 4c where indi-
cations exist that some diffusion may have occurred between the titanium substrate and a zir-
conium-containing particle High contents of zirconium, magnesium, titanium, and silicon
were detected in this area
1.2
o
D
z
"' I.(3"
-ft.8
CO
fl /// BASELINE
ii // ..-
II / / o~
!i/," .-""
~176176176
J"// J'- ... o . . . ..",. oO'~

,,,.4
"r" ff ~176
~' ~176
/ ~ ~
~176
~176
.~
o.2
X
~176176
IJJ ~176176
~176176176
~176176
~
~176176
I I I
0 200 400 600
TEMPERATURE(*(])
FIG 9--Thermograms from dlfferentlal scannmg calorlmetryfor Rema and Btovest (from Ref 5)
Quartz and Crtstobahte

Thermal analysis previously obtained for both Rema and Blovest investment materials are
shown in Figs 9 and 10 These graphs include differential scanning calorimetry and thermo-
mechamcal data compiled in previous work [5] These results show that BIovest and Rema
investment molds contain silica In the form of cnstobalite and quartz, respectively Since the
Biovest investment mold reacted w~th t~tamum while the Rema investment mold did not
react, it follows that differences m reactivity between cnstobahte and quartz with molten tita-
nium was the hkely reason for this behavior
One explanation may be due to differences in purity between quartz and cnstobahte Quartz
is remarkably pure with a specific gravity of 2 65 to 2 66, while cnstobahte contains an
increased number of lmpunties, both substxtutional and interstitial Ions, as shown by the
greater variation in specific gravity usually between 2 27 to 2 32 [10] Some impurities are
thought to be trapped at imperfections such as strained and broken bonds [ 14] These imper-
fections anse in cnstobahte due likely to the larger SI-O-SI angle (180 ~ versus 144 ~ for quartz)
between nelghbonng SIO4 tetrahedra [15] Bond angle difference also affects impurity centers,
such as the aluminum center, germanium centers, stable mulhp[e-alkah centers, and others
The presence of ampurmes in cristobahte should accelerate the formation of metal slags that
are more reactive with titanium to form TIO2 and SIOx Even the lower melting temperature
of quartz by 93~ below that of cnstobalite [ 12] appears not as important as the greater reac-
tivity of cnstobahte induced by its impurities and greater number of structural imperfections
y /
/
/
/
I
Z /
/
0
CO BIOVEST / REMA
/
Z /
<~ /
/
G. 0.6 /
X /
/
LIJ /
/
/
<I /
/
LU 1,
Z /
_.,.I
i i i I i I
25 200 4O0 60O 800

TEMPERATURE(~
FIG l O--Percent expanston versus temperature plots for Rerna and Btovest (from Ref 5)
(PDVSA Los Teques) pursuant to License Agreement. No further reproductions authori
Furthermore, bandgap &fferences in their electronic structures, 9 2 eV for quartz and 6 9 eV

for crlstobahte [ 15], most likely contribute to &fferences in their reactlvlt]es
Besides naturally occurnng impurities with cristobahte, impurities can be also reduced via
contamination during the setting and heating of the magneslum-ammomum-phosphate
binder Hydrogen, oxygen, nitrogen, phosphorous-pentoxlde, and other gases are very likely
to be taken-up by the cristobahte This contammaUon lowers the melting temperature ofcris-
tobahte During casting with molten tltamum, these gases are outgassed from the liquefied
cristobahte and wolently react with the molten titamum both embritthng the metal and pro-
viding a source for the porosity
Conclusions
1 Crlstobahte reacted violently with molten titanium probably due to its increased level of
impurities either occurring naturally or from gaseous contamination dunng the setting and
firing of the phosphate matrix
2 Microscopy and energy &sperslve spectroscopy revealed transformation of crlstobahte
into a vitreous glassy slag in a phosphate-bonded investment mold that contained silica in the
form of both crlstoballte and quartz
3 The coalescence ofcnstobahte particles and the degradation of the magnesium-phosphate
matrix formed two &stlnct types of vitreous glassy slags Silicon-to-oxygen ratios were higher
m the former type
4 ContamlnaUon of the vitreous glassy slags by magnesmm, phosphorous, calcmm, chlo-
ride, as well as tltamum occurred
Acknowledgments
A portion of this project was supported by a grant from the National Institutes of Health,
No DE 05761 John Lenke provided SEM-EDS expertise and support
References
[1] Wllhams, R D and Dlppel, J, "Comparison of Titanium Investment and Rammed Graphite Cast-
ings," Tltamum Net Shape Technologies, F H Froes and D Eylon, Eds, The Metallurgical Society,
American Institute of Mining, Metallurgical, and Petroleum Engineers, New York, 1984, pp 193-
199
[2] Teifke, F C, Marshall, N H, Eylon, D, and Froes, F H , "Effect of Processing on Fatigue Life of
T1-6AI-4V Castings," AdvancedProcessingMethodsfor Titamum, D F Hasson and C H Hamil-
ton, Eds, The Metallurgical Society, American Institute of Mining, Metallurgical, and Petroleum
Engineers, New York, 1982, pp 147-159
[3] Waterstrat, R M and Gmseppetti, A A, "Casting Apparatus and Investment Mold Material for
Metals which Melt at Very High Temperatures," Journal of Dental Research, Vol 64, Abstract No
1278, 1985, p 317
[4] Mueller, H J, "Microscopy Analysis of Dental Tltamum Casting Investment Materials," Scanmng
Microscopy, Vol 3, No 3, 1989, pp 837-842
[5] Mueller, H J, Gmseppettl, A A, and Waterstrat, R M, "Phosphate-Bonded Investment Materials
for Titanium Casting," Journal of Dental Research, Vol 69, Abstract No 2072, 1990, p 367
[6] Takahashl, J, Kamura, H, Lautenschlager, E P, Chern Lm, J H, Moser, J B, and Greener, E H,
"Casting Pure Titanium into Commercial Phosphate-bonded $102 Investment Molds," Journal of
DentalResearch, Vol 69, 1990, pp 1800-1805
[7] H1guch~,H , Matsuya, S, and Yamane, M, "Thermal Behavior ofPhosphate-Bonded Investment,"
ShtkaRlkogakuZassht, Vol 23, No 61, 1982, pp 6-11
[8] Wnedt, H A , "O-SI (Oxygen-Slhcon)," BlnaryAlloy Phase Diagrams, T B Massakskl, Ed, 2nd
ed, Vol 3, ASM International, Metals Park, OH, 1990, pp 2915-2918
MUELLER ON INVESTMENTCASTING 445
[9] Iler, R K, The Colloid Chernzstry ofSthca andSlhcates, Cornell Umverslty Press, Ithaca, NY, 1955,
pp 3-17
[10] Norton, F H, Refractortes, 4th ed, McGraw-Hall,New York, 1968, pp 171-173
[11] Stevens, L and Kuhn, A T , "Dlatomlte as a Source of Cnstobahte for Dental Investments a Dif-
ferential Thermal Analysis Study," Austrahan Dental Journal, Vol 27, 1982, pp 238-242
[12] Handbook of Physicsand Chemistry, 46th ed, R C Weast, Ed, The Chemical Rubber Co, Cleve-
land, OH, 1965, p B-218
[13] Levm, E M, Robbms, C R, and McMur&e, H F, Phase Dtagrams for Ceramtsts, Vol 1, The
American Ceramic Society, Columbus, OH, 1964, pp 69, 85 (Vol 4), 102, 104, 105, 112, 113, 141-
143
[14] Grlscom, D L, "Defects and Impunues m a-Quartz and Fused SdlCa," The Phystcs of StO2 and Its
Interfaces, S T Pantehdes, Ed, Pergamon Press, New York, 1978, pp 232-252
[15] Cha&, D J, Laughhn, R B, and Joannopoulos, J D, "Electromc Structure and Spectra of Crys-
talhne and Amorphous S102," The Physics of Sl02 and Its Interfaces, S T Pantehdes, Ed, Perga-
mon Press, New York, 1978, pp 55-59
Author Index
A K
Alberts, F E , 109 Koss, D A, 363

Anderson, I E , 363
L
B
Larkm, E., 414
Bartoslewlcz, L , 109
Bell, D E, 327
Benner, R L, 139 M
Bitler, W R , 212
Blum, S T , 254 Marder, A R , 167,254
Marslco, T A, 327
C Mueller, H , 429
Chou, Y T , 167 N
Cole, G S, 109
Conrad, H , 372 Nelson, J A , 313
Notls, M R , 167
D
P
Denney, P E , 327
Drury, W, 295 Petroloms, K , 327
Plckenng, H W , 212
F Prestndge, E B, 243
Purdy, S M, l, 184
Fisher, M D , 372
Fowler, D B ~235
R
Fncke, W G , Jr, 88
Fnel, J J , 243
Ramam, A S, 189
Rochow, T G , 83
G
Glannuzzl, L A , 212
Gogglns, K M , 254
Gokhale, A M , 295 Saenz, N T , 155
Grugel, R N , 393 Shaw, W J D , 344
Smith, B J , 254
H Sprecher, A F, 372
Szlrmae, A, 1
Hemnch, K F J , 177
Hllller, J , 224 T
Howell, P R , 189, 199, 212, 327,
363 Tnvedl, R , 393
447
Copyright
Copyright*by ASTM Int'lASTM
1993 by (all rightsInternational
reserved); Thu Dec 29 00:42:12 EST 2011
www.astm.org
V Z
Vander Voort, G F , 1, 3, 266 Zamanzadeh, M , 414

Varughese, R , 199 Zelk, L K , 363
Zwell, L , 184
W
Warnmuth F J , 1
Subject Index
A Auger spectroscopy, 88
Automotive matenals, 109
Abrasives Axle shafts, automotive, 109
for advanced materials, 313
development, 313 B
diamond, 139
Advanced materials, mlcrostructural Balnlte, granular, in HSLA-100, 199
analysis, 313 Body structures, automotive, 109
Aging, AL 9021,344 Brittle materials, ultrathln sectmn
AI (artlfiCml intelligence), twin band techniques, 155
identification, 243
Aluminum C
AL 9021, mlcrostructure and
mechanical alloying, 344 Cast iron, in automotive materials, 109
in automotive materials, 109 Ceramic composites, ultrathln section
Analytical transmission microscopes, techniques, 155
development, 177 Ceramics
Artificial intelligence, twin band m automotive materials, 109
identification, 243 mlcrostructure analysis, 313
ASTM Committee E4 surface preparation, 139
award winners, 23 ultrathln section techniques, 155
chairmen, 34 Chain structure, of electrorheological
history, 3, 83 flmds, 372
officers, 4, 17 Chipping, lnterfaoal, 139
standards, 27 Chromized coatings, quantitative ~mage
subcommittee chairmen, 19 analysis, 254
subcommittees, 6 Cloud-piercing telescope, 88
technical publications, 33 Coatings, corrosion-resistant, quantitative
ASTM standards image analysis, 254
Committee E4 Composite materials
history, 3 mlcrostructure analysis, 313
overview, 27 mlerostructure development,
roles of, 83 transparent model alloy system,
E 15, 184 393
E 15-26T, 184 Copper-niobium alloy, powders,
E 43, 184 mlcrostructure, 363
E 43-42T, 184 Copper precipitates, HSLA- 100, TEM,
E 81, 184 199
E 81-49, 184 Corrosion-resistant coatings,
E 81-77, 184 characterization with ~mage
E 82-63, 184 analysis, 254
E 112, 254 Creep, Nb-2Y composites, 189
E 112-88,243, 254 Cnstobahte, reaction with titanium, 429
E 1181-87, 254 Crystal data, 184
E 1382, 243 Cubic boron mtride, 139
449
D G
Decarburization, subcommittee, 6 Galvanneal coatings, quantitative image

Deformation, reduction in advanced analysis, 254
materials, 313 Glass, in automotive materials, 109
Dendritic systems, development, Glass beads, for electrorheologlcal fluid
transparent model alloy system, model, 372
393 Grain boundaries, twin band
Diamond grinding disks, 139 identification, 243
Diffraction Grain size
patterns, "d" spacings, 184 E4 subcommittee, 6
X-ray, 184 measurement, 254
Disks, grinding, 139 mechanically alloyed aluminum, 344
Distribution function, in Granular bamlte, in HSLA-100, 199
electrorheologlcal fluids, 372 Granular femte, in HSLA-100, 199
Grinding
E diamond disks for, 139
for ultrathm sectioning, 155
Edge rounding, 139
Electrical system, automotive, 109 H
Electrodes, automotive, 109
Electron microprobe analysis, early Heat-affected zone
development, 224 cast titanium in incompatible
Electron microprobes, 88 investment mold, 429
Electron Microscope Micro Analyzer, HSLA-100, 199
167 laser-welded nickel-aluminum bronze,
Electron microscopy, early development, 327
224 Heyn intercept method, 254
Electron Mlcrostructure of Steels, High-pressure inert gas atomization, Cu-
subcommittee, 6 Nb powders, 363
Electron probe mlcroanalyzer, 177 History
Electron probes, static-beam, 167 electron microscopy, 224
Electrorheolog~cal fluids, mlcrostructure, metallography, E4 committee and, 3,
372 83
Emission microscopy, E4 subcommittee, mlcroanalysis, 224
6 mlcrostructure analysis, 313
Energy dispersive spectroscopy, cast phase transformation in iron-carbon
titanium in sdica-contaming alloys, 167
investment mold, 429 Hot-dip galvannealed coatings,
Eta phase, Fe-Zn couples, 212 quantitative image analysis, 254
Etchants, for AL 902 l, 344 Hot isotatlc pressing, Nb-2Y composite,
Eutectxc systems, development, 189
transparent model alloy system, HSLA-100, TEM, 199
393 Hydrogen blisters, galvamzed steels, 414
Exhaust system, automotive, 109
Image analysis, 88
Failure analysis, galvanized steel products, corrosion-resistant coatings, 254
414 microscopes, 88
Femte, granular, in HSLA-100, 199 quantitative, 254
Forming problems, galvanized steels, 414 twin band identification, 243
Ford Model T, 109 Image processing, twin band
Fractal dimension, fracture surface, 295 identification, 243
Fracture surfaces, fractal dimension, 295 Inclusions, subcommittee, 6
INDEXES 451
Interface reactions, cast titanium in silica- electron microscopy, early

containing mold, 429 development, 224
Interface stability, transparent model alloy failure analysis, galvamzed steels, 414
system for, 393 fracture surface fractal dimension
Intergranular preop~tahon, galvanized measurement, 295
steels, 414 high-pressure inert gas atomization, 363
Internal cracking, AL 9021,344 for laser-welded mckel-alummum
Investment casting, commercmlly pure bronze, 327
titanium, 429 mercury quench method, 167
Investment molds, slhca-contalnlng, 429 mIcroanalysls, early development, 224
Ion mllhng, hqmd mtrogen, 212 mlcrostructural analysis (see
Iron-carbon alloys, Wldmanstatten Mlcrostructure)
structure and martens~te, 167 quant~taUve metallography, 235
Iron-zinc couples, mterdlffUSlOn regions, for solidified mlcrostructures, 393
TEM, 212 stereologlcal methods, 235
for surface preparanon, 139
transmlssmn electron microscopy
Fe-Zn couples, 212
Jeffnes plammetnc method, 254 HSLA-100, 199
Joint Committee on Powder Dlffracnon twin band identification, 243
Standards, 184 ultrathln sections, 155
X-ray absorpt]on, 177
L X-ray fluorescence, 177
X-ray methods, 184
Laboratory evaluation and safety, E4 X-ray spectrometry, 177
subcommittee, 6 Metallographlc terminology and
Lapping plates, abrasives on, 313 nomenclature of Phase Diagrams,
Laser-welded mckel-alummum bronze, E4 subcommittee on, 6
microstructure, 327 Metallography
Light microscopes, 88 history, 3, 83
Light mxcroscopy quantitative (see Quantitative
HSLA-100, 199 metallography)
laser-welded nickel-aluminum bronze, Metal matnx composites, Nb-2Y, TEM,
327 189
quant~tanve and stereolog~cal methods, Metal oxide slags, 429
235 Mlcroanalysls
Local orientation measurement, 88 early development, 224
with electron beams, 167
M Mlcrographs, stereo, 88
Mlcromdentanon Hardness Tesnng, E4
Macrophotography, laser-welded mckel- subcommxttee, 6
aluminum bronze, 327 Microprobes, electron, 88
Manufacturing, of electron beam Microscopes
instruments, 167 analytical transmission, 177
Martens~te, formanon and morphology, hght, 88
167 resolution, 88
Matenals analysis scanning electron, 88, 177
automotive components, 109 scanning tunnel, 88
ultrathin section techmques, 155 translmlSsion electron, 88
Mechamcal alloys, hzgh magmficatmn transmission electron, 88
metallography, 344 Microscopy, ultrathm sectioning
Mercury quench method, 167 technique, 155
Metallographic techniques Mlcrostructure
for AL 9021,344 advanced materials, 313
automonve, 109 AL 902 l, 344
M~crostructure--contmued Phase transformations

analysis, history, 313 martenslte, 167
automotive materials, 109 Wldmanstatten structures, 167
cast titanium in silica-containing Phosphate-bonded molds, 429
investment mold, 429 Photography, E4 subcommittee, 6
Cu-Nb powders, 363 Polishing
electron microscopy, history, 224 advanced matenals, 313
electrorheologlcal fluids, 372 of speomens, 139
Fe-Zn couples, 212 ultrathln sectioning technique, 155
fracture surface fractal dimenmon, 295 Powder Diffraction File, 184
galvanized steels, 414 Powder metallurgy, Cu-Nb alloy, 363
gram size measurement, 254 Product specifications, quantitative and
HSLA-100, 199 stereologlcal methods, 235
laser-welded mckel-alummum bronze, Profilometry, fractal dimension
327 measurement, 295
mlcroanalysis, early development, 224 Publications, Committee E4, 33
microscopes and imaging devices, 88
Nb-2Y, 189 Q
necklace, 189
scanning electron beam instruments, Quantitative analysis, techniques
167 development, 167
sohdlfied, metallographlc techniques, Quantitative fractography, 295
393 Quantitative image analysis, corrosion-
twin band identification, 243 resistant coatings, 254
ultrathin section techmques, 155 Quantitative metallography
X-ray methods, 184 grain size measurement, 266
Mlcrosuperplastlcity, AL 9021,344 in standards and specifications, 235
Mixed-phase specimens, surface subcommittee, 6
preparaUon, 139 Quartz, reaction with titanium, 429
Montectlc systems, development,
transparent model alloy system, R
393
Radiators, automotive, 109
N Rapid solidification, Cu-Nb powders, 363
Recommended Practice for Dllatometrlc
Necklace mlcrostructure, 189 Analysis, E4 subcommittee, 6
Nickel-aluminum bronze, laser-welded, Recrystahzatlon, Nb-2Y composites, 189
microstructure, 327 Resolution, of microscopes, 88
Nlobmm-yttna composites, TEM, 189 Rubber, in automotive matenals, 109
Nomenclature, ASTM Committee E4
role, 6, 83 S
O Sample selection and preparation, E4

subcommittee on, 6
Optical microscopy Scanning, in microscopy, 88
electrorheological fluids, structure, 372 Scanning electron microscopes, 88, 177
HSLA- 100, 199 Scanning electron microscopy
Oxide dispersion strengthening, Nb-2Y cast titanium in slhca-contamlng
composites, 189 investment mold, 429
Oxygen evolution, AL 9021,344 Cu-Nb powders, 363
HSLA-100, 199
P laser-welded nickel-aluminum bronze,
327
Phase identification in metal alloys, E4 mechanically alloyed aluminum, 344
subcommittee, 6 Scanning tunnel microscopes, 88
INDEXES 453
Selected area diffraction Transmission electron microscopes, 88,

Fe-Zn couples, 212 177
Selected area diffraction Transmission electron microscopy
history, 184 early development, 224
Shear ridges, AL 9021, 344 Fe-Zn couples, 212
Silica, vitreous, lnterfaclal, 429 HSLA-100, 199
Silica-containing investment molds, for laser-welded nickel-aluminum bronze,
commercially pure htanlum, 429 327
Size, grain, 254 nioblum-yttna composites, 189
Slit-island analysis, fractal d~menslon Transmissions, automotive, 109
measurement, 295 Transparent materials, for solidification
Sohdlficat~on, transparent materials for, phenomena, 393
393 Triple-point count method, 254
Specml Committee on Grain Twin bands, identification with AI, 243
Characteristics, 6
Specifications, product (see Product U
specifications)
Specimens Undercutting, of specimens, 139
early studies of Wldmanstatten and
martenslte, 167 V
surface preparation, 139
X-ray methods, 184 Valvetraln, automotive, 109
Sprayed coatings, mlcrostructure analysis, Vitreous silica, interracial, 429
313
Standards (see ASTM standards) W
Statistical analyses
electrorheolog~cal fired structure, 372 Weld zone, in laser-welded nickel-
grain size measurement, 254 aluminum bronze, 327
Steels Wldmanstatten structures, formation and
in automotive materials, 109 morphology, 167
galvamzed, fadure analysis, 414 Windshields, automotive, 109
low-carbon, TEM, 199 Wood, in automotive matenals, 109
Stereological methods, in standards and
speoficatlons, 235 X
Stereo mIcrographs, 88
Surface rehef, Wldmanstatten structures X-ray absorption, 177
and martenslte, 167 X-Ray Crystal Analysis, E4
Surfaces, fracture, fractal dimension, 295 subcommittee, 6
X-ray diffraction, methods history, 184
T X-ray fluorescence, 177
X-ray mlcroanalyzers, 167
Telescopes, cloud-piercing, 88 X-ray spectrometry, development, 177
Thermal analysis, E4 subcommittee on, 6
Thermal spray coatings, quantitative Z
image analysis, 254
Titanium, cast, reaction with slhca- ZAF method, 167
containing investment mold, 429 Zeta phase, Fe-Zn couples, 212
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The History of ASTM Committee E4 on Metallography--

Some Incidental History of Metallography and ASTM Committee E 4 - -

Research Under the Microscope--WILLIAM G. FRICKE,JR 88

METALLOGRAPHIC PREPARATION TECHNIQUES

Automotive Materials and Their Characterization: 1916 to 1 9 9 1 -

New Diamond Grinding Disks for Specimen Surface l>reparation--

Advancements in Ultrathin Section Techniques for the Characterization of Brittle

The Early Metallographic Studies of Chih-Hung Chon on the Formation and

X - R A Y AND ELECTRON METALLOGRAPHY

Those Magnificent Men on Their Scanning Machines--KURT F. J HEINRICH 177

Seventy-Five Years of Activity in X-Ray Methods by ASTM Committee E4.06--

Microstrnetural Studies of an Oxide-Dispersion-Stabilized Niobium Composite

Transmission Electron Microscopy of the lnterdiffusion Regions of Iron-Zinc

Some Reflections on the Early Development of Electron Microscopy and

Quantitative Metallography in Test Method Standards and Product

Artificial Intelligence for Twin Identification--JOHN J. FRIEL

The Use of Quantitative Image Analysis for the Characterization of Corrosion-

Examination of Some Grain Size Measurement Problems--

Measurement and Interpretation of Fracture Surface Fractal Dimension--

In Search of Mierostructure--JAMES A NELSON 313

The Microstructure of Laser-Welded Aluminum BronzeS--DAVID E BELL,

Metallography of Mechanically Alloyed Aluminum--WILLIAM J. D SHAW 344

Microstructural Investigations of Rapidly Solidified Copper-Niobium (Cu-Nb)

Metallography Applied to the Structure of Electrorheoiogical (ER) Fluids--

Interpreting Solidification Phenomena and Microstructural Evolution in Metals

Some Failure Analysis Case Histories in Galvanized Steel Products--

Characterization of Reaction Between Cast Titanium and Silica-Containing

Author Index 447

Subject Index 449

George F. Vander Voort Samuel M. Purdy

Francis J. Warmuth Albert Szirmae

The History of ASTM Committee E4 on

ABSTRACT. Organized on 10 October 1916 to estabhshed standard magnifications for micro-

KEY WORDS: metallography, history, standards, testing

ASTM E4 on Metallography, organized on 10 October 1916, grew out of Committee E 1 on

Supervisor, Materials Characterization, Carpenter Technology Corporation, Reading, PA 19612

ance of standards is an obvious yardstick. E4 has published forty-two standards Of these,

.............. j ......... ~ ...............................................................................................................................................................

wntten by Dr John J Friel o f P n n c e t o n Gamma-Tech, current Sub 11 chairman Frank Vel-

OIficers Committee E4 on Metallography

First Vice Chairmen

2nd Vice Chairmen

Sub I on Sample Selection and Preparation and Photography

Sub 2 on Metallographic Terminology and Nomenclature of Phase Diagrams

Sub III on Thermal Analysis/Sub 3 on Nomenclature

Sub 5 on Microindentation Hardness Testing

Sub 6 on X-Ray Methods

Sub VII on Methods of Thermal Analysis

Sub 8 on Grain Size

Sub X on Decarburization/Sub X on Research

Sub 11 on X-Ray and Electron Metallography

Sub 14 on Quantitative Metailography

Sub XV on Emission Microscopy

Sub 16 on Phase Identification in Metal Alloys

Sub 17 on Laboratory Evaluation and Safety

Committee FA Award Winners

Fellows Prior to the Award of Merit

Honorary ASTM Members

Past ASTM Officers

Joseph R. Vilella Award