2007 Atlas of Cast Metal-Matrix Composites Structures

Jerzy Sobczak
Andrzej Wojciechowski
Natalia Sobczak
Krystyna Pietrzak
Rajiv Asthana
Dariusz Rudnik
WFO
Commision 8.1
Cast Composites
ATLAS
OF CAST
METAL-MATRIX
COMPOSITES
STRUCTURES
Motor
Transport
Institute
2007
Foundry
Research
Institute
Jerzy Sobczak
Natalia Sobczak
Rajiv Asthana
Andrzej Wojciechowski
Krystyna Pietrzak
Dariusz Rudnik
ATLAS
OF CAST
METAL-MATRIX
COMPOSITE
STRUCTURES
Part I
Qualitative analysis
Motor Transport Institute - Warsaw
Foundry Research Institute - Cracow

2007
Translation assistance provided by Tomasz Drecki
With the sponsorship of:

- World Foundrymen Organization
- Ministry of Science and Higher Education of Poland
- Motor Transport Institute
- Foundry Research Institute
ISBN 978-83-60965-00-9
Copyright 2007 by
All rights reserved
No part of this book may be reproduced, stored in a retrieval

system, or transmitted, in any form or by means, electronic,
mechanical, photocopying, recording, or otherwise, without
the prior written permission of the publisher
Published by
First edition
PRINTED IN POLAND
Contents
Page
Summary
Foreword
From the Authors
I. Particulate dispersion-reinforced composites

I.1. Aluminum composites containing fly ash (ALFA composites)
I.2. Aluminum composites containing graphite
I.3. Aluminum composites containing silicon carbide
I.4. Aluminum composites containing aluminum oxide
I.5. Aluminum composites containing graphite and silicon carbide (hybrid)
I.6. Copper composites containing graphite
I.7. Lead composites containing fly ash
I.8. Lead composites containing graphite
11
11
31
47
61
64
70
80
81
II. Short fiber-reinforced composites

II.1. Aluminum oxide-reinforced aluminum composites
II.2. Carbon felt-reinforced aluminum composites
II.3. Carbon felt-reinforced zinc composites
II.4. Carbon felt-reinforced lead composites
83
83
85
92
95
III. Long fiber-reinforced composites

III.1. Carbon fiber-reinforced aluminum composites
III.2. Carbon fiber-reinforced copper composites
III.3. Sapphire fiber-reinforced nickel composites
96
96
99
101
IV. Gas reinforced composites (gasars)
106
V. Nano-composites
109
VI. Typical structural defects in metal-matrix composites

VI.1. Particulate dispersion-reinforced composites
VI.1.1. Macro-scale nonuniform arrangement of the reinforcing phase
VI.1.2. Micro-scale nonuniform arrangement of the reinforcing phase
VI.1.3. Porosity - gas bubbles and shrinkage
VI.1.4. Excessive reactivity between the metal matrix and reinforcement
VI.1.5. Contaminations and non-metallic inclusions
VI.2. Porous ceramic preforms reinforced composites made of short, long fibers
or particulates
VI.2.1. Structural discontinuities as a result of insufficient preform
infiltration
VI.2.2. Structural heterogeneity and discontinuities resulting from the
improper preform preparation
VI.2.3. Excessive reactivity between composite components
VI.2.4. Non-metallic inclusions
VI.3. Hybrid composites
VI.4. High volume fraction particulate-reinforced composites
VI.5. Long fiber-reinforced composites
114
114
114
115
119
121
125
Acknowledgements
143
126
126
129
131
134
135
137
140
Summary
The ATLAS displays microstructures of metal-matrix composite materials based on

aluminum, copper, zinc, lead, nickel (nickel-aluminide) as well as magnesium metal matrices,
manufactured by the authors. The composites were reinforced with different types of
particles (fly ash, graphite, silicon carbide and aluminum oxide), short fibers (aluminum oxide
and carbon felt) and long fibers (carbon and sapphire). Microstructures of gasars (a new
group of composites with gas as reinforcing phase) are also presented together with
microstructures of aluminum matrix nanocomposites. The analysis of structural
characteristics of each kind of material is supplemented by a description of the composite
type, method of manufacture as well as experimentally proven and potential service
properties. Typical structural defects of the cast metal-matrix composites are covered in
detail.
Foreword
Over the last fifty years, metal-matrix composites have seen wide-ranging
applications beyond the aerospace sector for which they were originally intended.
Consumer industry, electronic packaging industry, and most importantly,
transportation industry have been the most prominent sectors to adopt metal-matrix
composites in niche applications such as the brake disc and parts of the suspension,
power train and the engine including pistons and cylinder blocks' sleeves. The
remarkable design flexibility that these composites, and their higher-temperature
counterparts, ceramic-matrix composites, exhibit enables the composites practitioner
to design and adapt the material to suit the needs of the user industry.
In the ATLAS, the authors have put together an impressive collection of metalmatrix composite microstructures synthesized by them in Poland and USA using the
solidification and casting techniques. The microstructures of cast composites based
on low-melting, medium-melting, and high-melting point metal matrices ranging from
lead, zinc, magnesium, aluminum and copper to nickel-based intermetallics, are
presented. The diversity of these composites is captured in hundreds of scientifically
valuable and aesthetically beautiful photomicrographs, each of which is accompanied
with a description of the prominent structural features, including structural defects, if
any, processing conditions as well as proven and potential properties of the
manufactured composites. The photomicrographs display the composites containing
a wide variety of reinforcement including silicon carbide, aluminum oxide, graphite
and fly ash. In addition, the ATLAS presents the microstructure and processing of
new and emerging metal-based nanocomposites and gasar materials that are sure to
gain wider acceptance in industry in years to come.
I am unaware of any previous effort of this magnitude and scope at
systematizing and assembling the unique structural attributes of cast composites in
a single resource. The principal authors are leaders in the metal-matrix area and
deserve to be congratulated for an excellent contribution to the technical literature
that will undoubtedly be of immense value and use to the researcher and practitioner
alike.
July 30, 2007
Mrityunjay Singh, Ph.D.

Chief Scientist
Ohio Aerospace Institute
NASA Glenn Research Center
Cleveland, OH, USA
From the Authors
Following successful practical applications in the aerospace and aviation

industry, increasing use of metal-matrix composites in car design (particularly as
brake discs material, parts of the suspension, power train and parts of the engines)
makes the slogan get the composites down to earth ever more up to date and real.
It has generally been accepted that this new group of construction materials still
refers to the niche materials in civil engineering (mainly electronics and land
transport). The question is: will metal-matrix composites still remain the niche
materials? They will probably stay as such at least for the next decade, though this is
not an opinion shared by all the experts. One of the reasons is the fact that
metal-matrix composites are, because of their nature, a kind of creative materials that
can potentially be designed and adapted to the customers individual needs.
Composites are also more expensive than metals and monolithic alloys; hence the
prospect of their wider use demands offering something extra with respect to
properties and serviceability. As a consequence, introduction of these materials in
practice will always have a precisely defined reason. Probably, it is just those unique
characteristics that carve out niches for composite materials. Some of those niches
could, however, be quite big and significant. For example, vital parts of the
combustion engines, such as pistons and cylinder blocks sleeves are quite a big
niche, just like electronic systems enclosures. Together, those niches make
a substantial assortment of engineering applications, and their amount and size is
ever growing. Moreover, each new application brings new engineering experiences,
which significantly reduce barriers for the next applications, even if each time they
are exceedingly specific and unique.
The main obstacle in common use of composite materials may prove to be
accessibility of not only information about the level of their properties together with
the methods of forming a particular products out of them, but also comprehensive
knowledge regarding specific structural features, particularly, with respect to the
interpretation.
The structure of the material may be regarded as a subjectively variable area
of interpretation, from high level of abstraction, bringing in high imprecision of
system interconnections of the mutually linked parts, to relatively simple quality and
quantity evaluation of selected structural components. From the point of view of the
methodology of testing materials, characterization of structure, although an extremely
important means to obtain the desired state of the material, is not an end in itself. It is
how the structure manifests itself as a concrete, desired set of properties, mainly
physical, chemical and mechanical properties, that ultimately determines the aim !
In comparison with monolithic materials (metals and alloy), the structure of
heterogenic materials, particularly composite materials, gets enriched and
complicated by the presence of the second component - the reinforcing phase and its
interaction with the matrix itself. The degree of complexity in evaluating such
heterogeneous structures increases, which may bring about a loss of required
degree of adequacy in relating the chemical composition of the matrix, the presence
of the reinforcement and its type, the technological parameters of the composite
synthesis process, and the composites structure and properties. Hence the
importance of credible and ample supply of information from the area of tested
10
materials structures in connection with initial attributes of their creation as well as

detailed definition of the condition of their forming.
We present you with the first part of the atlas of metal-matrix composite
structures covering those composites that are primarily based on nonferrous metal
matrices, and which, in the vast majority of cases, were created and tested during the
last decade, by the authors, both in Poland (at the Foundry Research Institute in
Cracow and the Motor Transport Institute in Warsaw), as well as in the USA,
particularly at the Composites Centre of the University of Wisconsin - Milwaukee and
at the NASA Glenn Research Center in Cleveland, Ohio.
From the onset, this part of the planned trilogy is devoted to the quality
structure description, mainly at the micro-scale, generated under the optical
microscope, in connection with manufacturing parameters of various kinds of cast
composites. The second part of the atlas will refer to quantitative structural analysis,
while the third and the last part, will cover the structural attributes of metal-matrix
composites as revealed by the scanning electron microscope.
The microstructure characterization was conducted mainly under the optical
OLYMPUS PMG3 microscope using polarized light technique and phase contrast as
well as using stereoscopic OLYMPUS SZ40 microscope and appropriately selected
method of preparing samples allowing for the specifics of the ground (polished)
surface to be analyzed. A few structural tests were also carried out on electron
scanning STEREOSCAN 420 microscope. The structure of each kind of composite,
apart from structural characteristics, is also accompanied by abbreviated description
of the type of its constituents, manufacturing methods, and expected service
properties, usually verified in the course of self-conducted tests.
The authors would like to express modest hope that this publication will
somewhat contribute to increasing the knowledge about structure of the family of
advanced materials such as metal-matrix composites, their chemical contents,
qualitative properties, and the manufacturing techniques developed on the basis of
know-how used. The know-how is often either protected and undisclosed in the
current open literature or it may be unknown and rarely used in creating advanced
innovative materials due to the difficulties experienced at the experimental level.
We would like to express our gratitude to professor Pradeep Kumar Rohatgi,
Director of the Composites Center at the University of Wisconsin-Milwaukee, for his
extensive help, particularly at the beginning of our activities in the field of
metal-matrix composites as well as numerous ever inspiring discussions. Our thanks
also go to professor Ludmila Boyko from the State Metallurgical Academy of Ukraine
in Dnepropetrovsk, for directing our attention towards highly porous metallic media
with controlled contents and gas bubble morphology, known as gasars.
11
Particulate dispersion-reinforced composites
I.
I.1.
Aluminum composites containing fly ash (ALFA composites)
52K/x fly ash composite (x = 5, 10 and 15 vol. %)

Matrix: 52K aluminum alloy (USA) - 9.18 Si, 2.55 Zn, 2.50 Cu, 1.01 Fe, 0.23 Mn, 0.13 Mg, 0.08 Ni,
0.07 Cr, 0.07 Pb, 0.05 Ti (wt. %).
Reinforcing phase: fly ash from PSI Energy electrical power plant (USA) contains mainly
cenospheres (microspheres) and about 10 % microgranules of the following chemical composition
(converted into oxides, wt. %):
Oxide
Microspheres
Microgranules
SiO2
58.0
38.5
Al2O3
32.2
17.1
Fe2O3
5.05
25.1
K2O
3.5
2.5
MgO
1.6
1.0
TiO2
1.2
1.5
CaO
0.8
4.0
Na2O
0.7
0.5
SO3
0.3
1.9
P2O3
0.1
0.5
An example appearance of the external cenospheres collected from another electrical power plant
(Dayton Power and Light Co., USA), used in the subsequent tests, is shown in Fig. I.1.1.
Manufacturing method: mechanical stirring method (vortex) with gravity casting into grey iron die.
Following melting, the composite slurry was subjected to squeeze casting under a pressure of
220 MPa for 45s (die temperature - bottom cavity/top squeeze plunger: 190-230/170-200C). The
casting temperature of the composite suspension was maintained within 670-690C range. Squeeze
cast cylinder of 80 mm diameter and 25-30 mm height was subjected to the following heat treatment
according: solutionizing at 540C/12 h, cooling in water at 70C; artificial aging at 160C/24 h.
Properties: lower (microgranules reinforcement) and very low (cenospheres reinforcement) density,
increased and satisfactory mechanical properties, significant resistance to grinding (wear off) and
thermal shock, decreased thermal expansion and thermal conductivity, good machinability,
advantageous economic and ecological manufacturing parameters (mainly due to waste material
character of the reinforcing phase).
Structural characteristics (Figs. I.1.2 - I.1.7): dominating effect of the external pressure during
solidification is noticeable in the fly ash-reinforced aluminum composites, characterized by low content
of cenospheres and microgranules relatively uniformly dispersed in the metal matrix. Microstructural
investigation proved that the hydrostatic pressure, applied to the solidifying composites prevents the
growth of eutectic phase crystals in the favored directions after the eutectic temperature has been
achieved. External pressure also leads to the increase of the -phase amount in the structure and
solidification of the cooled eutectic in the direct vicinity of the dendritic solidification front. As a result of
the pressure application, liquid aluminum alloy fills up the microspheres, solidifying inside them in
a much pulverized structure. Modifying influence of the external pressure is also observed on the
structure of the whole composite matrix.
12
Fig. I.1.1.
As-received fly ash reinforcing phase used for manufacturing ALFA composites. This is fly ash from the Dayton
Power and Light Co electrical power plant, (USA), in the shape of glassy-like cenospheres with the following
chemical composition (converted into oxides, wt. %): 61.0 SiO2, 25.8 Al2O3, 5.0 Fe2O3, 3.6 K2O, 1.6 MgO,
1.0 TiO2, 0.8 CaO, 0.7 Na2O, 0.3 SO3, 0.1 P2O3. Cenospheres, representing mainly amorphous material, are of
varying size as well as non-uniform color due to diversified chemical composition (e.g. ginger brown color revels
high content of the iron oxides)
13
Fig. I.1.2.
Fig. I.1.3.
Structure of 52K/5 vol. % fly ash aluminum alloy composite, obtained by vortex method. Following melting, the
composite was subjected to squeeze casting and heat treatment (precipitation hardening). Non-etched sample.
Polarized light
composite was subjected to squeeze casting and heat treatment (precipitation hardening). Sample etched with
Keller reagent. Polarized light
14
Fig. I.1.4.
Polarized light
15
c
Fig. I.1.5.
c
Fig. I.1.6.
Polarized light
16
Fig. I.1.7.
17

AK12/9 wt. % fly ash composite
Matrix: AK12 aluminum alloy (AlSi12CuNiMg) 12.20 Si, 1.15 Cu, 0.95 Ni, 0.90 Mg, 0.60 Fe,
0.20 Zn, 0.19 Mn, 0.09 Ti (wt. %).
Reinforcing phase: fly ash from Dayton Power and Light Co. electrical power plant (USA) contains
mainly microgranules of the following chemical composition: 55.9 SiO2, 30.2 Al2O3, 5.4 Fe2O3,
1.3 CaO, 2.7 K2O, 1.0 MgO, 1.6 TiO2, 0.2 Na2O, 0.3 SO3, 0.4 P2O3.
Manufacturing method: introduction of initially enriched reinforcing phase by mechanical stirring
(vortex) under argon and squeeze casting under the pressure of 170 MPa for 45 s, (die temperature
bottom/top - 180/220C). The slurry was poured into the die at the temperature of 750C and squeeze
cast in order to produce combustion engine pistons of 90 mm diameter.
Structural characteristics (Fig. I.1.8): good acceptability of the reinforcing phase by the metal matrix
is noticeable due to intensive chemical character of the interaction between the composite
constituents. This statement reflects the presence within the structure of the large primary silicon
crystals, formed as a result of the reaction between the oxides (mainly SiO2 and FexOy) with liquid
aluminum according to the oxy-redox reaction 3MeO+2Al=Al2O3+3Me. Also significant amount of
cracked fly ash microgranules is an indirect proof of intensive interactions taking place in a given
composite.
18
Fig. I.1.8.
Structure of squeeze cast AK12/9 wt. % fly ash composite. As-cast. Non-etched sample. Polarized light (a, b, d,
f) and phase contrast (c, e, g)
19

AG10/5 wt. % fly ash composite
Matrix: AG10 aluminum alloy (AlMg10) - 9.50 Mg, 0.10 Mn, 0.20 Fe (wt. %).
Reinforcing phase: fly ash from Skawina electrical power plant (Poland) of the following composition:
38.5 SiO2, 17.1 Al2O3, 25.1 Fe2O3, 4.0 CaO, 2.5 K2O, 1.0 MgO, 1.5 TiO2, 0.5 Na2O, 1.9 SO3, 0.5 P2O3
(5 wt. %).
Manufacturing method: mechanical stirring method (vortex) using the device for refining and
modifying Al alloys (URM-1 type, designed by Foundry Research Institute) and gravity casting into
permanent mould (made from grey iron). Following melting, the composite was subjected to squeeze
casting under a pressure of 230 MPa for 45 s (die temperature bottom/top: 190-230/170-200C).
The casting temperature of the composite slurry was maintained within 670-690C range. Cylindrical
castings (70 mm diameter and 90 mm height) were subjected to the following heat treatment:
solutionizing at 430C/16 h, cooling in water at 70C; natural aging for 96 h.
Properties: lower density, satisfactory mechanical properties, significant resistance to grinding (wear
off) and thermal shock, decreased thermal expansion and thermal conductivity, good machinability
properties, advantageous economic and ecological manufacturing parameters (mainly due to waste
material character of the reinforcing phase).
Structural characteristics (Fig. I.1.9): The characteristic feature of the composites manufactured
using fly ash from Skawina electrical power plant is the less uniform arrangement of the reinforcing
phase in the metal-matrix when compared with composites obtained using fly ash from the PSI Energy
electrical power plant (USA) (Figs. I.1.2 - I.1.7). It is, however, a deceptive effect because it is linked
with the reinforcing phase properties in the as-received state and not with an effect of agglomeration
during the composite manufacture. In the case of coal burning in the Skawina electrical power plant,
resultant fly ash contains a large amount of primary agglomerates, consisting of a few to a few dozens
of different size particles, permanently bridged with one another. The squeeze pressure facilitates
filling with the liquid metal the cavities between the particulates and even micro-cracks and open
porosity within individual particles. While visible in the photomicrographs, the structural discontinuities
are within large agglomerates and form enclosed porosity.
20
g
Fig. I.1.9.
Structure of AG10/5 vol. % fly ash composite: (a, b) gravity cast and (c-g) squeeze cast. Non-etched sample.
Polarized light (a, b, d-g) and phase contrast (c)
21

Al/25 wt. % fly ash composite
Matrix: pure aluminum (99.5 wt. % Al).
Reinforcing phase: fly ash from the Dayton Power and Light Co electrical power plants (USA) mainly
containing microgranules of the chemical composition (wt. %.): 55.9 SiO2, 30.2 Al2O3, 5.4 Fe2O3,
1.3 CaO, 2.7 K2O, 1.0 MgO, 1.6 TiO2, 0.2 Na2O, 0.3 SO3, 0.4 P2O3.
Manufacturing method: mechanical alloying method involving mixing of matrix powder with fly ash
particles in a rotating and vibrating mill, under argon atmosphere, and then compacting the mixture
under pressure.
Properties: lower density, increased mechanical properties (particularly ultimate tensile strength),
significant resistance to grinding (wear off) and thermal shock, fundamentally decreased thermal
expansion and thermal conductivity, good machinability, advantageous economic and ecological
manufacturing parameters (mainly due to the waste material character of the reinforcing phase).
Structural characteristics (Figs. I.1.10 - I.1.11): The characteristic features of the initial constituent in
the form of composite powder are (Fig. I.1.10):
1) presence of a substantial amount of the reinforcing phase,
2) a high degree of reinforcing phase break-up, stemming from the milling effect of the fly ash
particulates, while a significant part of microspheres of diameter below 10 m does not get
destroyed,
3) a high degree of homogeneity in the arrangement of the reinforcing phase within metal matrix,
4) relatively low presence of structural discontinuities in the regions of large composite particles,
which are essentially agglomerates of composite particulates (from several dozens to several
hundred times smaller).
The characteristic features of the composite obtained from composite powders using powder
compaction under pressure are (Figs. I.1.11 - I.1.12):
1) complete lack of structural discontinuities,
2) complete disappearance of microspheres as well as larger fractions of microspheres due to
their interaction with metal matrix,
3) more than ten times smaller size of the reinforcing phase precipitates in comparison with the
primary composite powder,
4) very minute reinforcing phase precipitates are created mainly by aluminum oxide particulates
produced due to oxy-redox reaction between aluminum and fly ash constituents
(2Al+3MeO=Al2O3+3Me), mainly silicon oxide and iron oxide since the reactivity of titanium
oxide is negligible, while calcium oxide and magnesium oxide do not react with the metal
matrix,
5) banding of the fine aluminum oxide precipitates, resulting from Al/metal oxide interactions.
22
23
Fig. I.1.10.
Structure of Al/25 wt. % fly ash composite (initial composite powders) obtained by mechanical alloying.
Non-etched sample. Polarized light (a-f, g, h, j, l) and phase contrast (i, k, m)
24
Fig. I.1.11.
Structure of Al/25 wt. % fly ash composite obtained by mechanical alloying followed by compaction of composite
powders by know-how technology. Transverse section. Non-etched sample. Polarized light (b, c, e, g) and phase
contrast (d, f, h). Figure (a) shows macrostructure of investigated section
25
Fig. I.1.12.
Structure of Al/25 wt. % fly ash composite obtained by mechanical alloying followed by compaction of composite
powders by know-how technology. Longitudinal section. Non-etched sample. Polarized light (b, c, e, g) and
phase contrast (d, f, h). Figure (a) shows macrostructure of investigated section
26
20 m
a
10 m
b
Fig. I.1.13.
Structure of Al/30 vol. % fly ash composite obtained by mechanical alloying followed by compaction of composite
powders under a pressure of 3000 MPa. Non-etched sample
27
AK12/60 vol. % fly ash composite

Matrix: AK12 aluminum alloy (AlSi12CuNiMg) 12.2 Si, 1.15 Cu, 0.95 Ni, 0.90 Mg, 0.60 Fe, 0.20 Zn,
0.19 Mn, 0.09 Ti (wt. %).
Reinforcing phase: fly ash from Dayton Power and Light Co. electrical power station (USA)
cenospheres of chemical content (wt. %): 59.8 SiO2, 32.2 Al2O3, 5.1 Fe2O3, 0.4 CaO, 1.4 K2O,
0.8 MgO, 0.8 TiO2, 0.2 Na2O, 0.2 SO3, 0.3 P2O3.
Manufacturing method: squeeze infiltration of the porous preform (porosity 40 vol. %) of
cenospheres under a pressure of 170 MPa for 45 s (die temperature top/bottom - 180/220C). The
matrix alloy was poured in the die at a temperature 760C. A cylinder of 70 mm diameter and 30 mm
height (in as-cast state, without heat treatment) was squeeze cast.
Properties: significantly lower density (in the extreme case bordering on 1 g/cm3), decreased thermal
expansion, electrical expansion and thermal conductivity, increased energy and sound absorption
characteristics, good machinability, advantageous economic and ecological manufacturing
parameters.
Structural characteristics (Fig. I.1.13): in spite of the high content of the reinforcing phase, the
preform is relatively well infiltrated by liquid matrix. The arrangement of the ash particulates in the
matrix corresponds to their initial distribution in porous preform, and the rigid packing of particulates
does not change in spite of a high pressure being exerted on the whole set. Parts of damaged
particulates are completely filled up due to liquid metal infiltration through micro-cracks in the walls of
microspheres. The apparent lack of metal penetration between the particulates, visible at high
magnifications, is a consequence not so much of the imperfections in the technological process of
squeeze infiltration method to manufacture the composites as it is of the process of preparing the
preform itself (a binding compound was used to manufacture the preform). On one hand, binding
compound causes bridges to appear, rigidly connecting the microspheres. But on the other hand,
relatively good wetting of the preform particulates by the binder contributes to complete filling up and
closure of the areas between some microspheres, making it impossible for the liquid metal to infiltrate
such areas. In microspheres that get coated with bonding compound, structural discontinuities
present in the micro sphere walls appear to get sealed, which increases the amount of microspheres
that remain unfilled with the metal-matrix.
28
Fig. I.1.13.
Structure of Al/60 vol. % fly ash composite, obtained by squeeze infiltration of the porous preforms made of
cenospheres. Non-etched sample. Phase contrast (c, e, g, i)
29
A356/5.0 wt. % fly ash composite

Matrix: A356 aluminum alloy (AlSi7Mg) 7.2 Si, 0.40 Mg, 0.60 Fe, 0.30 Mn (wt. % ).
Reinforcing phase: aluminum composite powders containing 25 wt. % of fly ash from Skawina power
station (Poland) and of the following content: 81.66 SiO2, 6.69 Al2O3, 4.37 Fe2O3, 4.29 CaO,
1.58 MgO, 0.40 K2O, 0.21 Na2O, 0.29 SO3, (wt. %), manufactured by mechanical alloying method,
using mixing in the rotating-vibrating mill under argon atmosphere.
Manufacturing method: mechanical stirring (vortex) of reinforcement with liquid metal of 720C
temperature for 24 h and gravity casting into the metal mould (cast iron).
Properties: lower density, increased and satisfactory mechanical properties, significant resistance to
grinding (wear off) and thermal shocks, decreased thermal expansion and thermal conductivity, good
machinability, advantageous economic and ecological manufacturing parameters (mainly due to waste
material character of reinforcing phase).
Structural characteristics (Fig. I.1.14): during manufacturing of the initial reinforcing phase by
mechanical alloying method, using aluminum powder and fly ash particulates, a pulverisation of main
part of the ash particulates takes place together accompanied by their homogenous arrangement in
the metal matrix. At the same time, mutual interaction between metal and ceramics takes place,
leading to one of a kind final activation of reinforcing phase, aimed at facilitating its introduction into
the metal bath (with the subsequent distribution of it within the entire volume). This way it is possible to
obtain not only a high degree of metal-ceramic slurry homogeneity, but also its satisfactory stability.
This is confirmed by relatively homogenous arrangement of fly ash particulates dispersed in the A356
alloy matrix, even in case of gravity casting. Reinforcement phase particulates, in their majority, are
located in the areas between dendrites of the aluminum solid solution, where also eutectic (Al+Si),
gets collected. In the given case, as in majority of ceramic reinforcing phases (SiC, Al2O3, graphite), fly
ash particulates compose inactive nucleants for the stable aluminum solution and its growth causes
reinforcement particulates to be pushed out into the inter-dendral areas. On the other hand, the same
particulates form active nucleants for the eutectic silicon precipitations.
30
Fig. I.1.14.
Structure of A356/15 wt. % fly ash composite, manufactured by vortex method using initial preparation of the
reinforcing phase by mechanical alloying method. Conventional light (a, b, d, f, h) and phase contrast (c, e, g, i)
31
I.2.
Aluminum composites containing graphite
Al/GrNi composite (5 vol. % nickel-coated graphite)

Reinforcing phase: nickel-coated platelet graphite particulates (about 20 wt. % Ni) of 150 m
average dimension.
Manufacturing method: mechanical stirring method (vortex), gravity cast into grey iron die and
squeeze cast under the pressure of 110 MPa for 30 s (die temperature - bottom/top 190-230/170-200C). The casting temperature of the composite slurry was maintained at 720C.
A die-cast cylinder casting (80 mm diameter and 40 mm height) was annealed at 300C for 4 h.
Structural characteristics (Fig. I.2.1): nickel-coated graphite platelets are well wetted by liquid
aluminum. This is a result of nickel coating dissolving in aluminum, and this process is accompanied
by reactive metal penetration inside the individual platelets via micro-cracks, which in turn causes the
platelet itself to divide into several smaller pieces.
10 m
Fig. I.2.1.
Structure of squeeze cast Al/5 vol. % GrNi composite. Non-etched sample. Polarized light
32
AK11/xGrNi composite (x = 2.5, 5.0 vol. % nickel-coated graphite)

Matrix: AK11 aluminum alloy 12.10 Si, 0.11 Mn, 0.42 Fe (wt. %).
Reinforcing phase: nickel-coated graphite particulates (NOVAMET, 50 wt. % Ni) of 75-120 m
average dimensions.
Manufacturing method: mechanical stirring method (vortex), gravity cast into grey iron die or
squeeze cast under a pressure of 110 MPa for 30 s (die temperature - bottom/top 190-230/170-200C). The casting temperature of the composite suspension was maintained at 720C.
A die-cast cylinder (80 mm diameter and 40 mm height) was annealed at 300C for 4 h.
Properties: slightly increased density, satisfactory mechanical properties, improved tribological
characteristics (decreased wear and friction coefficient in experiments with steel counter sample),
especially after squeeze casting; a reduction in the thermal expansion coefficient is expected.
Structural characteristics (Figs. I.2.2 - I.2.5): nickel-coated graphite particulates are well wetted by
the liquid metal matrix which is why there are no structural discontinuities at the interface between
matrix and graphite particulates as well as no particulate agglomerates form during composite
manufacture.
The susceptibility to wetting in the AK11/xGrNi system is linked with the high degree of chemical
interaction due to intensive dissolution of nickel coating in the liquid matrix during composite
manufacture.
Excessive dissolution of the nickel coating, however, causes an undesired effect because of a change
in the chemical composition of the metal matrix, its superfluous enrichment with nickel, and the
formation of the brittle Al3Ni intermetallic phase precipitates as well as primary Si precipitates.
An increase in the volumetric fraction of nickel-coated graphite being introduced in the matrix causes
an increase in the amount of these precipitates.
The significant fact is that in the case of gravity cast composites, apart from Al(Ni)+Al3Nieut eutectic,
Al3Niprim primary precipitates also form. These precipitates have a shape of elongated platelets of
differing dimensions.
Irrespective of the composite manufacturing method, primary silicon precipitates have a tendency to
grow on dispersed graphite particulates.
Graphite
Siprimary
Sieut
Al3Ni
Graphite
a
20 m
33
Si prim.
Al3Ni
Graphite
20 m
b
10 m
c
Fig. I.2.2.
Structure of AK11/2.5 vol. % GrNi composite: gravity cast (a), squeeze cast (b, c). Sample etched with Kellers
reagent. Polarized light
20 m
a
34
20 m
b
Fig. I.2.3.
Structure of AK11/5 vol. % GrNi composite: gravity cast (a), squeeze cast (b). Sample etched with Kellers
reagent. Conventional light (a) and polarized light (b)
35
AK20/5.7 vol. % nickel-coated graphite composite

Matrix: AK20 aluminum alloy - 22.34 Si, 1.50 Cu, 1.10 Ni, 0.60 Mg, 0.25 Mn, 0.45 Fe (wt. %).
Reinforcing phase: nickel-coated graphite particulates (NOVAMET, 50 wt. % Ni) of 75-120 m
average dimensions.
Manufacturing method: mechanical stirring method (vortex), squeeze cast under a pressure of
110 MPa for 30 s (die temperature - bottom/top - 190-230/170-200C). The casting temperature of the
composite slurry was maintained at 720C.
Cylindrical castings (70 mm diameter and 90 mm high, were subjected to heat treatment according to
the following parameters: solutioning at 510C/3.5 h, cooling at hot water, aging at 240C/6.5 h.
Properties: satisfactory mechanical properties, significantly improved tribological characteristics
(decreased wear and friction coefficient in experiments with steel counter sample). A reduction in the
thermal expansion coefficient is essential expected.
Structural characteristics (Figs. I.2.4 - I.2.6): there are no structural discontinuities at the interface
between the matrix and graphite particulates as well as no particulate agglomerates form during
composite manufacture because nickel-coated graphite particulates are well wetted by the liquid metal
matrix.
These benefits are linked with the high degree of chemical interaction due to intensive dissolution of
nickel coating in the liquid aluminum alloy during composite manufacture.
Dissolution of the nickel coating results in changes of its thickness and structure accompanied with the
formation of discontinuities, especially in its matrix-side layer.
Despite the fact that nickel dissolution causes a change in the chemical composition of the metal
matrix, application of squeeze casting suppresses its superfluous enrichment with nickel, resulting in
the undesired formation of high volume fraction of brittle Al3Ni intermetallic phase precipitates, as it
takes place in the case of gravity cast composites of the same system.
Irrespective of the composite manufacturing method, primary silicon precipitates have a tendency to
nucleate at the surface of dispersed graphite particulates.
36
Fig. I.2.4.
Structure of squeeze cast AK20/5.7 vol. % GrNi composite. Top of the casting. Non-etched sample. Polarized
light (a, b, d, f, h) and phase contrast (c, e, g, i)
37
38
Fig. I.2.5.
Structure of squeeze cast AK20/5.7 vol. % GrNi composite. Middle of the casting. Non-etched sample. Polarized
39
Fig. I.2.6.
Structure of squeeze cast AK20/5.7 vol. % GrNi composite. Bottom of the casting. Non-etched sample. Polarized
40
A356/5.7 vol. % nickel-coated graphite composite

Metal matrix: A356 aluminum alloy (AlSi7Mg) - 7.11Si, 0.30Mg, 0.48Fe, 0.31Mn (wt.%).
Reinforcing phase: nickel-coated graphite particulates (NOVAMET, 50 wt. % Ni) of average
dimension 75-150 m.
Manufacturing method: centrifugal casting. Nickel-coated graphite particulates (50Gr/50Ni) of
average dimension 75-150 m were heated to a temperature of 200C for 2 h, before being introduced
into the metal, following a newly developed procedure. Graphite mould temperature - 200C,
temperature of liquid metal 740C (directly before the introduction of nickel-coated graphite), time of
stirring composite slurry - 2 min, temperature of pouring - 740C, rotational speed (graphite inlay
placed tightly in a cast iron tube) - 1200 rpm, casting dimensions: diameter - 55 mm, length 100 mm.
Properties: slightly increased density, acceptable mechanical properties, improved tribological
characteristics (decreased wear and friction coefficient in experiments with steel counter sample),
especially on internal layers of the centrifugal castings; a decrease in the thermal expansion
coefficient could be expected.
Structural characteristics (Fig. I.2.7): The centrifugal force causes loss of structural homogeneity of
the gravity cast A356/5.7 GrNi composite (Fig. I.2.7) and generates four zones (Figs. I.2.8 and I.2.9).
Zone I (a, c, e) forms an external layer on the casting, does not contain graphite particulates and is
characterized by dispersive structure with relatively uniform distribution of a large quantity of Al3Ni
phase, which forms as a result of the dissolution of nickel coating (from the graphite surface) in the
liquid metal matrix.
Zone II (g, i, k) bordering zone I also does not contain graphite particulates but, contrary to zone I, the
Al3Ni phase precipitates in zone II have a shape of elongated plates with an arrangement clearly
determined by the direction of solidification. Isolated graphite particulates appear in this zone and
eutectic participates are much larger than in all other zones.
Zone III (m) is a transition zone, between internal layer of the casting surface (zone IV) and zone II.
In zone IV (o, r, t) there is accumulation of particulates of graphite which are driven out of other zones
by the centrifugal force.
In order to explain the specifics of structure of centrifugally cast A356/GrNi composite castings, some
aspects linked with crystallization of the metal matrix as a ternary Al-Si-Ni alloy should be taken into
account. This is because dissolution of nickel coating, initially spread over graphite, takes place during
creation of metal suspension as well as in the course of its spinning and crystallization.
Zone I, initially takes shape as a result of solidification of the suspension layer in contact with the
mould, which is at a significantly lower temperature. Then, during spinning with simultaneous cooling
of the suspension, its de-lamination takes place because centrifugal force segregates the heavier
Al3Ni phase precipitates outside (i.e., farthest from the centre of rotation), and lighter graphite
particulates on the inside periphery of the casting (i.e., nearest the centre of rotation). Internal
concentrations of graphite particulates create a unique three-dimensional network (beginning of zone
IV) inside of which grow the primary blocky Al3Ni phase precipitates during further decrease of the
temperature. The movement of those precipitates, in comparison with other areas of the centrifugal
casting, is severely restricted. As a result, these precipitates lodge themselves between relatively large
graphite particulates. Further rotation and cooling of the suspension is accompanied by flowing out of
the liquid metal into zones II and III, in which the pseudo-binary eutectic Al-Al3Ni crystallizes first at
a temperature of 577C with a preferred orientation. In the last stages of solidification at a temperature
of 547C, the crystallization of ternary eutectics Al-Al3Ni-Si finally occurs.
Fig. I.2.7.
100 m
Structure of A356/5.7 vol. % Ni-coated

graphite (50:50) composite made by vortex
method and gravity cast into a grey iron die.
As-cast. Etched with Keller reagent
41

a-b
c-d
e-f
I
Fig. I.2.8.
g-h
i-j
k-l
II
m-n
o-p
III
r-s
t-u
IV
Structure of centrifugally cast A356/5.7 vol. % Ni-coated graphite (50:50) composite. The sequence of structure
evolution is shown, beginning with the external layer, through the middle zone, the transition zone, and ending
with the internal (near centre) zone. Remarks on the picture refer to Figs. I.2.9 and I.2.10
42
43
Fig. I.2.9.
Structure of centrifugally cast A356/5.7 vol. % Ni-coated graphite (50:50) composite. The sequence of structure
evolution is shown, beginning with the external layer I (a - h), through the middle zone II (i - l), the transition zone
III (m, n), and ending with the internal zone IV (o - u). Non-etched sample. Conventional light (on the left) and
phase contrast (on the right). 100x
44
45
46
Fig. I.2.10.
Structure of centrifugally cast A356/5.7 vol.% Ni-coated graphite (50:50) composite. The sequence of structure
evolution is shown, beginning with the external layer I (a - h), through the middle zone II (i - l), the transition zone
III (m, n), and ending with the internal zone IV (o - u). Non-etched sample. Conventional light (on the left) and
phase contrast (on the right). 500x
47
I.3.
Aluminum composites containing silicon carbide
2014/20 vol. % SiC composite

Matrix: 2014 aluminum alloy (AlCu4SiMg) 4.40Cu, 0.80Si, 0.8Mn, 0.60Mg, 0.30 Fe (wt. %).
Reinforcing phase: single crystal silicon carbide platelets (hexagonal, -SiC) (from Third Millennium
Technologies, Inc., USA); of average platelet sizes 20-70 m diameter x 0.50-5 m thickness;
as-received (i.e., uncoated).
Manufacturing method: mechanical agitation using ultrasonic vibrations and gravity - die-casting.
Pre-heated SiC platelets were spread over the melt poured in a graphite mould at 800C, and the
surface of the melt was touched with a titanium horn connected to an ultrasound generator.
Structural characteristics: Only the finest variety of SiC platelets (20-70 m x 0.50-5 m) was
dispersed in the melt using ultrasound as it was thought to present the greatest challenge to
immersion and dispersion. Fig. I.3.1 shows a uniform distribution of the SiC in the matrix; no excessive
agglomeration of SiC platelets was observed. The matrix structure showed finer dendrites as
compared to a stir-cast composite to which Mg had been added for improved wettability. There was
virtually no gas porosity evident at optical magnifications.
50 m
Fig. I.3.1.
Structure of 2014l/xSiC graphite composite obtained by mechanical stirring coupled with ultrasonic vibration and
then gravity cast to mould. Non-etched sample. Conventional light
48
Al/20 vol. % SiC composite

Reinforcing phase: nickel-coated silicon carbide particulates of 20-80 m (SiCNi) diameter
Manufacturing method: mechanical stirring method (vortex), squeeze casting.
Structural characteristics (Fig. I.3.2): homogeneous arrangement of nickel-coated reinforcement
phase particulates in the aluminum matrix, resulting from good susceptibility of nickel-coated areas to
be wetted by liquid aluminum. This is linked to a process of dissolution of nickel coating in metal bath.
20 m
20 m
Fig. I.3.2.
Structure of Al/20 vol. % Ni-coated SiC squeeze cast composite. Non-etched sample. Polarized light
49
F3S.15S (A359/15 vol. % SiC), F3S.20S (A359/20 vol. % SiC) as well as F3S.30S (A359/30 vol. %
SiC) composite (F3S.xxS composites family)
Matrix: A359 (AlSi9Mg) aluminum alloy 8.50-9.50 Si, 0.45-0.65 Mg, 0.20 Fe, 0.20 Cu, 0.20 Ti
(wt. %).
Reinforcing phase: silicon carbide particulates of average diameter 20 m.
Manufacturing method: mechanical stirring method (vortex) similar to the method patented by
DURALCAN Co., involving remelting and gravity casting into grey iron die and/or squeeze casting
under the pressure of 230 MPa for 45 s (die temperature bottom/top 190-230C/170-200C). The
casting temperature of the composite slurry was maintained at 670-690C. A cylinder (80 mm
diameter and 40 mm height) was squeeze cast. A precipitation hardening heat treatment was applied:
solutionizing at 538C/8 h, cooling in water to 70C, followed by aging at 154C/5 h.
Properties: increased mechanical properties, especially after squeeze casting (including fatigue
properties), considerable improvement of tribological characteristics (significant reduction of wear, to
the highest cast iron grades), a reduction in the coefficient of thermal expansion, an increase in the
thermal conductivity.
Structural characteristics (Figs. I.3.3 - I.3.8): SiC particulates are wetted by the liquid Al matrix and
bond well with the matrix upon solidification. No structural discontinuities are observed at the interface
between SiC particulates and metal matrix in either as-cast composite or fractured composite
(Fig. I.3.3).
The macro-scale structure of the F3S.20S gravity cast composite containing 20 vol. % SiC is
characterized by a homogeneous distribution of the reinforcing phase particulates. However, at the
micro-scale, SiC particulate agglomerates are observed in, the inter-dendritic regions, and within the
surrounding (Al-Si)eut eutectic. This agglomeration is due to the particle pushing phenomenon created
by growing (Si) phase, and taking place during composite solidification (Fig. I.3.4).
The squeeze cast composite shows much higher degree of structure homogeneity resulting from the
formation of Al(Si) solid solution. Another characteristic feature of such composites is the significant
refinement of the primary (blocky) silicon crystals and modification of the eutectic silicon (Sieut)
precipitates.
Irrespective of the composite manufacturing method, there is a tendency for both Sieut phase and ironrich phases to grow on the surface of the SiC particulates, which in turn leads to creation of bridges
between reinforcing phase particulates. This is particularly clearly revealed under polarized light
(Figs. I.3.4 e, I.3.5 e), when parts of SiC particulates become transparent, with an appropriate setting
of the polarizer.
Heat treatment of such composites causes an increase in the volume fraction of the Al(Si) phase
precipitates as well as spheroidization of eutectic silicon precipitates. The effect of heat treatment on
composite structure is shown in Fig. I.3.6.
Observations of composite microstructure under polarized light (Fig. I.3.7) at optical magnifications
demonstrate that the undesirable aluminum carbide (Al4C3) phase does not form. The second phase
precipitates growing on SiC particulates (clearly visible under different polarizer settings, because SiC
particle becomes transparent) represent eutectic silicon.
An increase in SiC content to 30 vol. % is an additional factor which increases the homogeneity of the
reinforcing phase distribution in the metal matrix (Fig. I.3.8).
50
SiC
SiC
Fig. I.3.3.
SEM view of the fracture surface of squeeze cast F3S.15S (A359/15 vol. % SiC) composite. As-cast
51
Si eut
e
Fig. I.3.4.
The structure of gravity cast F3S.20S composite (A359/20 vol. % SiC). As-cast. Non-etched sample.
Conventional light (a, c, e) and phase contrast (b, d)
52
e
Fig. I.3.5.
The structure of squeeze cast F3S.20S composite (A359/20 vol. % SiC). As-cast. Non-etched sample.
Conventional light (a, c, e) and phase contrast (b, d)
53
Fig. I.3.6.
The influence of heat treatment on the structure of squeeze cast F3S.15S composite (A359/15 vol. % SiC):
(a-c) as-cast, (d-f) after heat treatment. Non-etched sample. Polarized light
54
c
Fig. I.3.7.
Fig. I.3.8.
The structure of squeeze cast F3S.15S composite (A359/15 vol. % SiC) after heat treatment, shown under
polarized light (various images of the same place taken under different settings of microscope polarizer),
illustrating growth of eutectic silicon precipitates on the SiC particulates. Non-etched sample
The structure of F3S.30S composite (A359/30 vol. % SiC). Non-etched sample. Phase contrast
55

Technologies, Inc., USA); of three average platelet sizes - 250-500 m diameter and 25-50 m
thickness; 50-250 m diameter and 5-25 m thickness; and 20-70 m diameter and 0.50-5 m
thickness; both as-received and copper-coated SiC platelets were utilized.
Manufacturing method: counter-gravitational infiltration of packed binder-less silicon carbide platelets
(packing density ~52%) by the molten 2014 aluminum alloy under nitrogen gas pressure; SiC platelets
were packed in quartz tubes via multistage compaction of loose powders; infiltration was done in
a stainless steel pressure vessel with a melting furnace, consisting of two semi-cylindrical heating
elements, housed inside the pressure vessel; quartz tubes containing packed SiC were attached using
leak-tight fittings to the lid of the pressure vessel which, upon closure, led to partial immersion of the tube
in the molten alloy held in a graphite crucible inside the pressure vessel; an argon blanket was maintained
over the SiC inside the quartz tube to reduce the oxidation of the liquid front; preheating time of SiC beds:
3-5 min; melt temperature: 800C; nitrogen gas pressure: variable, 525-850 kPa; infiltration time: 3-5 min;
slow cooling at the conclusion of infiltration in ambient air.
Both as received and copper-coated SiC platelets were infiltrated. Cu-coating was done to promote
the wettability and facilitate the infiltration. Copper coating was deposited on SiC using an electroless
plating technique. For this, SiC platelets were stirred for 3 h in a solution of 10 g/l of SnCl2 and 40 ml/l of
concentrated HCl. The platelets were then stirred for 15 min in a solution 0.5 g/liter PdCl2 and 1 ml/l
concentrated HCl. After stirring, the solution was decanted, and platelets washed twice with distilled water.
Finally, the platelets were stirred for 15 min in the plating bath of following composition: 10 g/liter
CuSO4.5H2O, 10 g/liter NaOH, 50 g/l sodium potassium tartrate, and 10 ml/l formaldehyde. The coating
deposition was confirmed with the SEM examination.
Properties: considerable improvement of tribological characteristics expected, significant reduction in
thermal expansion coefficient and increase in the thermal conductivity, increased hardness and
strength, and decreased ductility.
Structural characteristics: A high volume fraction and a uniform distribution of SiC platelets are
achieved in the SiC/2014Al composites via infiltration of fine and coarse SiC (Fig. I.3.9); however,
some metal-starved cavities persist in the cast microstructure because of the difficulty of filling small
gaps between closely-spaced or nearly-touching platelets. Color-etching of polished samples reveals
the presence of micro-segregation in the alloy matrix between coarse (250-500 m x 25-50 m) SiC
platelets (Fig. I.3.10); micro-segregation is nearly completely erased when inter-particle spacing
becomes very small as in the case of fine (20-70 m x 0.50-5) SiC platelets (Fig. I.3.11). The growth of
primary Al dendrites is physically constrained by the SiC platelets as shown in Fig. I.3.12, and the
inter-dendritic eutectic deposits on the SiC. A number of secondary phases in the alloy matrix of the
infiltrated composite bars (Fig. I.3.13) are revealed by color etching, which include Al15(CuFeMn)3Si2,
CuAl2, Al20Cu2Mn3, Mg2Si and CuAl2Mg.
20 m
a
Fig. I.3.9.
20 m
Structure of 2014/xSiC composites transverse to the infiltration direction, pressure: 710 kPa, melt temperature:
800C, infiltration time: 3 min; as-received SiC platelet size: 20-70 m diameter and 0.50 - 5.0 m thickness (a);
250-500 m diameter and 25-50 m thickness (b)
56
200 m
Fig. I.3.10.
Structure of 2014/xSiC composite transverse to the infiltration direction showing SiC distribution and microsegregation; pressure: 525 kPa, melt temperature: 800C, infiltration time: 5 min, SiC size: 250-500 m diameter
and 25-50 m thickness, as-received SiC. The sample was color etched with a solution of 4 g KMnO4 and 2 g
NaOH in 1 l distilled water
10 m
Fig. I.3.11.
Structure of 2014/xSiC composite showing suppression of coring in the solidified matrix due to diffusional
constraints imposed by small inter-particle spacing in compacts made from fine SiC platelets; pressure: 750 kPa,
melt temperature: 800C, infiltration time: 5 min, SiC size: 20-70 m diameter and 0.50 - 5.0 m thickness, asreceived SiC. The sample was color etched with a solution of 4 g KMnO4 and 2 g NaOH in 1 l distilled water
57
10 m
a
Fig. I.3.12.
10 m
Structure of 2014/xSiC composite showing two regions. Section transverse to the infiltration direction showing
physically constrained growth of Al dendrites, the inter-dendritic eutectic, and micro-segregation in cored
dendrites growing within the network of packed SiC platelets; pressure: 825 kPa, melt temperature: 800C,
infiltration time: 5 min, SiC size: 50-250 m diameter and 5-25 m thickness, Cu-coated SiC; the sample was
color etched with a solution of 4 g KMnO4 and 2 g NaOH in 1 l distilled water
10 m
a
Fig. I.3.13.
10 m
Structure of two regions of a color-etched 2014/SiC composite transverse to the infiltration direction showing
secondary phase precipitation in the inter-particle regions. The composite was produced by gas pressure
infiltration using nitrogen gas at a pressure of 525 kPa (melt temperature: 800C, infiltration time: 5 min). The
sample was color etched with a solution of 4 g KMnO4 and 2 g NaOH in 1 l distilled water. The phases that form
during normal solidification of 2014 Al alloy include: Al15(CuFeMn)3Si2, CuAl2, Al20Cu2Mn3, Mg2Si and CuAl2Mg
58
AK12/60 vol. % SiC composite

Matrix: AK12 aluminum alloy (AlSi12CuNiMg) 12.20 Si, 1.15 Cu, 0.95 Ni, 0.90 Mg, 0.60 Fe, 0.20 Zn,
0.19 Mn, 0.09 Ti (wt. %).
Reinforcing phase: silicon carbide particulates in the shape of a preform of 40 vol. % porosity.
Manufacturing method: squeeze infiltration method under a pressure of 230 MPa for 45 s (die
temperature - bottom: 200-220C, pressure core: 190-200C). The pouring temperature of AK12 alloy:
720C.
thermal expansion coefficient and increase in the thermal conductivity.
Structural characteristics (Fig. I.3.14 - I.3.15): further increase of reinforcing phase content up to
60 vol. % is possible because the preform of 40 vol. % porosity is fully infiltrated with liquid matrix
under pressure. Structural analysis of such composites shows incomplete local filling of the areas
between particulates with metal that are particularly clearly revealed under polarized light (Fig. I.3.9).
However, this is only an apparent effect that results from the use of binder to fabricate the rigid porous
preform. This is because liquid binder wets and links individual reinforcing phase particulates via
bridges, which resemble structural discontinuities in appearance. Such a composite, with the
reinforcing phase content over 50 vol. %, should in fact be called a ceramic-matrix composite material.
c
Fig. I.3.14.
Structure of squeeze cast AK12/60 vol. % SiC composite (silicon carbide preform, infiltrated with AlSi12CuNiMg
alloy under pressure. Non-etched sample. Phase contrast
59
c
Fig. I.3.15.
Structure of squeeze cast AK12/60 vol. % SiC composite (silicon carbide preform infiltrated with AlSi12CuNiMg
alloy under pressure). Non-etched sample. Polarized light
60
Al/70 vol. % SiC composite

Reinforcing phase: preform made of SiC particulates bonded using liquid glass binder. Preform
porosity about 30 vol. %.
Manufacturing method: gas pressure infiltration in an autoclave under a pressure of 7 MPa at 800C
for 30 min.
Structural characteristics (Fig. I.3.16): complete preform infiltration with liquid matrix. Examination
under the optical microscope magnifications does not disclose the existence of aluminum carbide
precipitates, despite relatively high temperature as well as extended reaction time. This is related with
the use of colloidal silicon dioxide as a binder (thin layer of SiO2 protects the SiC particulates from
their direct contact with liquid aluminum).
15 m
Fig. I.3.16.
Structure of Al/70% vol. % SiC composite, manufactured by gas pressure infiltration in the autoclave.
Non-etched sample. Polarized light
I.4.
61
Aluminum composites containing aluminum oxide
A356/20 vol. % aluminum oxide composite (COMRALTM)

Matrix: A356 aluminum alloy (AlSi7Mg) - 7.2 Si, 0.40 Mg, 0.60 Fe, 0.30 Mn (wt. %).
Reinforcing phase: microgranules (incorrectly known in the literature as microspheres) of MICRAL20 type, based on aluminum oxide (Al2O3 + mullite).
Manufacturing method: mechanical stirring method (vortex). Following melting, the composite was
subjected to squeeze casting under a pressure of 230 MPa for 45 s (die temperature - bottom/top:
190-230/170-200C). The casting temperature of the composite suspension was maintained at
670-690C. A cylindrical casting (70 mm diameter and 90 mm height) was produced but it was not
heat treated.
Properties: increased mechanical properties, considerable friction and wear resistance, and thermal
shock resistance, decreased thermal expansion and conductivity, good machinability.
Structural characteristics (Fig. 1.4.1-1.4.3): at the macro scale in the gravity cast composites,
microgranules of aluminum oxide are homogeneously distributed. But at a micro-scale, there is a clear
tendency for the reinforcing phase to gather in the interdendritic areas, as a result of the particle
pushing phenomenon.
The castings manufactured using squeeze casting method display significantly smaller segregation
and more homogenous arrangement of microgranules in the metal matrix. This is linked with an
essential influence of pressure on crystallization, and, consequently, with the refinement of metal
matrix structure (including, both Al solid solution as well as Al-Si eutectic).
10 m
Fig. 1.4.1.
SEM image of the reinforcing MICRAL-20 microgranules based on aluminum oxide with fine spinel particulates
on their surface
62
63
h
Fig. I.4.2.
i
TM
Structure of A356/20 vol. %. aluminum oxide (COMRAL ) composite, gravity cast into a metal die. Non-etched
sample. Conventional light (a, b, d, f) and phase contrast (c, e, g, i)
20 m
a
20 m
b
Fig. I.4.3.
TM
Structure of squeeze cast A356/20 vol. % aluminum oxide (COMRAL ) composite. Non-etched sample.
Polarized light
64
I.5.
Aluminum composites containing graphite and silicon carbide (hybrid)
A356/15 vol. % SiC/5 vol. % graphite composite

Matrix: A356 aluminum alloy (AlSi7Mg) - 7.2 Si, 0.40 Mg, 0.60 Fe, 0.30 Mn (wt. % ).
Reinforcing phase: silicon carbide particulates of average 20 m diameter and graphite particulates
of about 100 m diameter.
Manufacturing method: mechanical stirring method (vortex) based on displacement neutral
buoyancy principle.
Properties: unique set of tribological properties, improved machinability (in comparison with silicon
carbide-reinforced aluminum composites, e.g. DURALCAN composites).
Structural characteristics (Fig. I.5.1) the gravity cast hybrid composites are characterized by very
uniform arrangement of both reinforcing phases in the metal matrix. A high degree of metal-ceramic
slurry stability, resulting from the displacement neutral buoyancy properties, has great significance in
creating such structure during the slurry formation and its subsequent casting.
b
Fig. I.5.1.
Structure of hybrid composite produced from A356 alloy reinforced with 15 vol. % SiC and 5 vol % graphite,
gravity cast into die. Non-etched sample. Phase contrast (a) and conventional light (b)
65

A356/15 vol. % SiC/5 vol. % graphite composite
Matrix: A356 aluminum alloy 7.2 Si, 0.40 Mg, 0.60 Fe, 0.30 Mn (wt. %).
Reinforcing phase: silicon carbide particulates of average 20 m diameter and graphite particulates
of about 100 m diameter.
Manufacturing method: mechanical stirring method (vortex) and centrifugal casting in graphite mould
of 100 mm internal diameter, rotational speed of 1000 rpm.
Properties: unique set of tribological properties, varying radially outward from the cylindrical cast axis,
self-lubricating properties of the internal layer (graphite-enriched) and high resistance to wear of the
external layer (silicon carbide-enriched).
Structural characteristics (Fig. 1.5.2 - 1.5.3): Segregation of particulates of both reinforcing phases
and shaping of the laminar structure indicate the important influence of the centrifugal force on the
spatial distribution of the reinforcing phases according to their densities. SiC particulates being heavier
than the metal-matrix are driven outward towards the external layer of the centrifugal cast. In contrast,
lighter graphite particles tend to migrate towards internal layer, while the transition layer is devoid of
the reinforcing phase. Besides SiC particulates, individual graphite particles of very large dimensions
are observed in the external zone. In the internal zone, there are gas bubbles besides graphite. In
comparison to the reinforced areas, the thickening of dendrites in the metal matrix is visible within this
layer, which is devoid of SiC and graphite particulates. This suggests that the reinforcing particles
restrict the growth of dendrites.
a-b
Fig. I.5.2.
c-d
e-f
g-h
i-j
k-l
m-n
o-p
Structure of centrifugally cast A356/15vol.%SiC/5vol.% graphite composite. The sequence of the layers structure
is shown: graphite-rich internal layer (a-b, c-d, e-f), transition layer (g-h), and SiC-rich middle - external layers (i-j,
k-l, m-n, o-p)
66
67
Fig. I.5.3.
Structure of centrifugally cast A356/15vol.%SiC/5vol.%Gr composite. Internal layer (a-f), transition layer (g-h),
and middle - external layer (i-p). Non-etched sample. Conventional light (on the left) and phase contrast (on the
right). 100x
68
69
Fig. I.5.4.
Structure of centrifugally cast A356/15vol.%SiC/5vol.%Gr composite. Internal layer (a-f), transition layer (g-h),
and middle - external layer (i-p). Non-etched sample. Conventional light (on the left) and phase contrast (on the
right). 500x
70
I.6.
Copper composites containing graphite
C90300/7.5 vol. % graphite composite

Matrix: C90300 copper alloy (CuSn8Zn4) - 8 % Sn, 4 % Zn (wt. %).
Reinforcing phase: graphite particulates of average 5 m diameter.
Manufacturing method: mechanical stirring method (vortex), gravity cast into graphite mould or grey
iron die. The composite slurry casting temperature was maintained at about 1050C. Cylindrical
castings were made (40 mm diameter and 120 mm height).
Properties: lower density, improved tribological characteristics (decreased wear and friction
coefficients in tests with steel counter sample); a decrease in the thermal expansion coefficient can be
expected.
Structural characteristics (Figs. I.6.1 and I.6.2): despite a large difference in the densities of graphite
and copper alloy, a homogeneous arrangement of the reinforcing phase in the metal matrix has been
obtained both along the length and cross-section of the gravity castings. This occurred because a
special operation of de-agglomerating graphite particulates was implemented prior to their introduction
into the metal bath. Composite material gravity cast into grey iron die (Fig. I.6.2) has more uniform
distribution of graphite particles, compared to that gravity cast into graphite mould (Fig. I.6.1).
II
200 m
III
Fig. I.6.1.
Structure of the C90300/7.5 vol. % graphite composite, gravity cast into a graphite mould: I top of the casting,
II middle of the casting, III bottom of the casting. Non-etched sample
Fig. I.6.2.
71
Structure of C90300/7.5 vol. % graphite composite, obtained by vortex method and gravity cast in a grey iron
die. Non-etched sample. Conventional light
72
C90300/7.5 vol. % graphite composite

Matrix: C90300 copper alloy (CuSn8Zn) - 8 % Sn, 4 % Zn, (wt. %).
Reinforcing phase: graphite particulates of average 5 m dimensions
Manufacturing method: mechanical mixing method (vortex) with centrifugal casting in graphite.
Properties: lower density, improvement of the tribological characteristics (decreased wear and friction
coefficient in tests with steel counter sample), particularly of the centrifugal castings internal layer.
Thermal expansion coefficient decrease can be expected.
Structural characteristics: photographs shown on Figs. I.6.3 - I.6.5 depict structural details of
individual areas visible on the cross-section of the C90300/7.5 vol. % graphite composite casting,
under conventional light and using phase contrast. Centrifugally cast composites have layered
structure, formed as a result of centrifugal force and density differences between graphite and copper
alloy. With clear division into three zones. I coarse grained external layer, practically not containing
graphite phase, but with structural discontinuities in a shape of porosity. II - transition layer of relatively
homogenous fine graphite particulates arrangement and pulverised metal matrix structure as a result
of the introduction of technological additive (titanium acc. to know how method) into the metal matrix
(up to the 1 wt. % level) in order to improve wettability of graphite particulates by liquid copper alloy.
Both graphite particulates alone as well as very fine (below 1 m) precipitations occurring as a result
of an interaction between graphite and titanium dissolved in the alloy, form heterogeneous
crystallisation nuclei. They cause clear brake up of the matrix grain in this zone of the composite
casting. III internal layer, graphite enriched and containing graphite bubbles and agglomerates.
a-b
c-d
e-f
I
Fig. I.6.3.
g-h
i-j
II
k-l
m-n
III
Structure of centrifugally cast C90300/7.5 vol. % graphite composite. The sequence of the layers structure
evolution is shown: I external layer (graphite free), II transition layer, III internal layer (graphite enriched).
Non-etched sample. Conventional light. Markings on the picture refer to Fig. I.6.4 and I.6.5
Structural pictures shown indicate various reasons for the porosity to occur depending on centrifugal
casting spot being analyzed. In the external graphite free layer, the sporadic gas shrinkage porosity
occurs (with a domination of shrinkage porosity) typical for the matrix alloy. In the internal layer
however, enriched with graphite, the occurrence of large gas bubbles is linked with gassing up of the
liquid metal-ceramic suspension (typical for the vortex method) and formation of large graphite
particulates agglomerates, combined with bas bubbles, being pushed out towards the centre of the
cylindrical casting under the centrifugal force.
73
74
Fig. I.6.4.
evolution is shown beginning with external layer I (a - h), through the middle one II (i - j), ending with III (k-n).
Non-etched sample. Conventional light (on the left) and phase contrast (on the right). 100x
75
76
Fig. I.6.5.
evolution is shown beginning with external layer I (a - h), through the middle one II (i - j), ending with III (k-n).
Non-etched sample. Conventional light (on the left) and phase contrast (on the right). 500x
77
Cu-Ni/Gr composite
Matrix: pure copper (initial), Cu-Ni alloy.
Reinforcing phase: nickel-coated graphite (50 : 50).
Manufacturing method: gravity-assisted infiltration of loose nickel-coated graphite deposit (50 : 50)
conducted in a graphite mould.
Properties: improved tribological characteristics, especially at increased temperatures.
Structural characteristics (Fig. I.6.5): very homogeneous arrangement of graphite particulates in the
metal matrix. Good infiltration of the inter-particle cavities between the graphite particulates because
of the dissolution of nickel coating in pure copper. Nickel segregation in the metal matrix takes place.
Fig. I.6.5.
Structure of Cu-Ni/Gr composite obtained by gravity-assisted infiltration of loose nickel-coated graphite deposit
(50 wt. % Ni). Non-etched sample. Conventional light
78
CuFe10Sn7Zn3/2.0 vol. % graphite composite

Matrix: CuFe10Sn7Zn3 copper alloy
Reinforcing phase: flaky graphite.
Manufacturing method: mechanical stirring method (vortex) and centrifugal casting in a graphite
mould of 100 mm internal diameter, rotational speed: 1000 rpm.
Properties: improved tribological characteristics expected (decreased wear and friction coefficients,
particularly of the centrifugally cast internal layer). A decrease in the coefficient of thermal expansion
can be expected.
Structural characteristics: (Fig. I.6.6): during stirring of the composite slurry together with ground
cast iron pieces containing flaky graphite, the dissolution of the iron in the liquid metal matrix takes
place, resulting in in-situ matrix reinforcement with graphite particulates. During centrifugal casting,
segregation of the metal suspension takes place because of the reinforcing phase segregation under
centrifugal force. This is because "freed" graphite particulates gather in the internal layer of the
centrifugal casing, while external layer becomes enriched with iron phase and contains pieces of
partially melted cast iron.
Cu
Cast iron
Cast iron
Cu
79
Fig. I.6.6.
Structure of centrifugally cast CuFe10Sn7Zn3/2.0 vol. % graphite composite: (a-d) external layer, (e-h) transition
layer, (i-l) internal layer. Non-etched sample. Polarized light
80
I.7.
Lead composites containing fly ash
Pb/60 vol. % fly ash composite

Matrix: lead containing 98.7 wt. % Pb.
Reinforcing phase: fly ash from Dayton Power and Light Co. power stations (USA), cenospheres of
chemical content (wt. %): 59.8 SiO2, 32.2 Al2O3, 5.1 Fe2O3, 0.4 CaO, 1.4 K2O, 0.8 MgO, 0.8 TiO2,
0.2 Na2O, 0.2 SO3, 0.3 P2O3.
Manufacturing method: squeeze infiltration of the porous preform (porosity 40 vol. %) made of
cenospheres, under a pressure of 10 MPa in 90 s (die temperature - bottom/top: 80/40C). Lead was
poured at 320C. Squeeze cast cylinder of 50 mm diameter and 120 mm height was made.
Properties: significantly lower density (approximately 5 g/cm3), decreased thermal expansion,
increased energy and sound absorption characteristics, good machinability, and advantageous
economic and ecological manufacturing parameters.
Structural characteristics (Fig. I.7.1): in spite of a lack of wettability between liquid lead and fly ash,
the application of external pressure makes it possible to produce a composite material of high
reinforcing phase content, and devoid of structural discontinuities (e.g., porosity) between particulates.
Some of the fly-ash particles, predominantly containing cracks or open porosity, are filled with liquid
matrix during infiltration.
20 m
Fig. I.7.1.
Structure of Pb/60 vol. % fly ash composite obtained by squeeze infiltration. Non-etched sample. Polarized light
1.8.
81
Lead composites containing graphite
Pb/60 vol. % graphite composite

Matrix: lead containing 98.7 wt. % Pb.
Reinforcing phase: nickel-coated graphite particulates (NOVAMET, 50 wt. % Ni) of average
dimension 75-150 m.
Manufacturing method: squeeze infiltration of the porous preform (porosity 40 vol. %) of nickelcoated graphite under a pressure of 60 MPa for 180 s (die temperature - top/bottom: 90/110C). The
matrix metal was poured in the die at a temperature of 320C. Squeeze cast cylinder of 50 mm
diameter and 120 mm height was made.
Properties: essentially lowered density, increased energy and sound absorption characteristics, good
machining properties, decreased thermal expansion.
Structural characteristics (Fig. I.8.1): uniform distribution of reinforcing phase in Pb matrix and good
filling of high volume fraction porous reinforcing preform with liquid matrix are obtained because of two
effects, i.e. covering of graphite particles with metallic Ni layer and application of high pressure.
82
Fig. I.8.1.
Structure of Pb/60 vol. % GrNi composite obtained by squeeze infiltration. Non-etched sample. Conventional light
(a, b, d, f) and phase contrast (c, e, g)
Short fiber-reinforced composites
II.
II.1.
Aluminum oxide-reinforced aluminum composites
83
AK12/78 vol. % aluminum oxide composite

Matrix: AK12 aluminum alloy (AlSi12CuNiMg) 12.2 Si, 1.15 Cu, 0.95 Ni, 0.90 Mg, 0.60 Fe, 0.20 Zn
0.19 Mn, 0.09 Ti (wt. % ).
Reinforcing phase: Short fiber preform based on aluminum oxide of initial porosity 782 %, made by
MORGAN Ltd. (chemical composition of the fiber made of Al2O3 according to the manufacturer:
96 wt. % Al2O3, 4 % SiO2). Individual fibers bonded with colloidal silica in the amount of 5 wt. %,
randomly spatially distributed and oriented. The preforms were of 95 mm external diameter and
30 mm height.
Manufacturing method: squeeze infiltration of the preform (initially preheated up to 700C at
a maximum rate of 300C/h) with a liquid aluminum alloy at 730C, final pressure of 230 MPa, and
infiltration time of 45 s; die temperature - bottom/ top: 220/190C. Initial pressure ratio was 5-10 MPa
during first 10 s of infiltration.
Properties: improved mechanical properties at room and at elevated temperature, high resistance to
thermal shock, decreased thermal expansion, electrical conductivity, and thermal conductivity, and
increased resistance to wear.
Structural characteristics (Fig. II.1.2): porous ceramic preform is characterized by a uniform
arrangement of fibers in its entire volume (Fig. II.1.1). The application of external pressure for the
infiltration (Fig. II.1.2) ensures complete filling of the preform cavities with the liquid metal and aids in
establishing permanent and intimate contact between the reinforcing phase and the metal-matrix. At
the same time, the external pressure does not cause distortion of the preform, which is evidenced by
a homogenous spacing of the fibers in the matrix and a lack of directional orientation.
The characteristic features of the microstructure of such composites are: 1) uniform infiltration of the
preform by the liquid metal, 2) lack of structural discontinuities, and 3) growth of silicon phase
precipitates (both eutectic silicon and primary silicon) on the surface of the aluminum oxide fibers; this
is a very beneficial phenomenon because it enhances the interfacial bonding between matrix and
reinforcing phase, thus favouring improved mechanical properties of the composite material.
Fig. II.1.1.
SEM image of the preform made of short fibers based on Al2O3
84
c
Fig. II.1.2.
Structure of AK12/78 vol. % Al2O3 composite produced by squeeze infiltration of porous preform (made from
short alumina fibers with SiO2 binder) with AlSi12CuNiMg alloy. Non-etched sample. Conventional light (a, b)
and phase contrast (b)
II.2.
85
Carbon felt-reinforced aluminum alloys
Al/carbon felt composite

Reinforcing phase: carbon felt preform of estimated initial porosity 70 vol. %, manufactured from
fibrous organic raw material by POLGRAPH Company, Nowy Scz (Poland). The preform consists of
individual carbon fibers of 10-13 m thickness with a random spatial distribution and in-plane
orientation. The felt preforms alone were of 80 mm diameter and 40-50 mm height.
Manufacturing method: squeeze infiltration of the thermally-activated carbon preform by liquid
aluminum at 780C, under a pressure of 230 MPa applied for 30 s; die temperature - bottom/top:
130-180/120-160C.
Properties: lower density, increased hardness, lower strength and plasticity, decreased thermal
expansion, decreased thermal and electrical conductivity, good machinability, and advantageous
Structural characteristics: carbon felt in its initial state (Fig. II.2.1) forms entangled continuous fibers
arranged in one direction and characterized by an inhomogeneous diameter and varying
cross-section. Within the carbon felt-reinforced aluminum-matrix composite structure (Fig. II.2.2), the
majority of the fibers retain their primary orientation, while the cavities between the fibers become
completely filled with liquid matrix. Structural discontinuities, in the form of pores between
agglomerates of many fibers occur rather sporadically (Fig. II.2.2 c). However detailed microscopic
examination under polarized light leads to the conclusion that such pores are actually primary defects,
which exist in the original felt prior to infiltration. These defects originate during the process of preform
manufacture when some fibers may form permanent bond with some or even umpteen fibers in such
a way that closed porosity forms inside this agglomerate. This closed porosity remains inaccessible to
the liquid metal during infiltration even under large pressures.
Aluminum carbide (Al4C3) precipitates were not found in the composite under optical microscopy
magnifications.
A characteristic feature of the carbon felt-reinforced composites is the presence of porosity inside
individual fibers. This is primary porosity of the fibers, spread over their entire length, because fibers
themselves are carbon tubes of different shapes and wall thicknesses (not necessarily coaxial).
Fig. II.2.1.
SEM image showing carbon felt structure
86
87
Fig. II.2.2.
Structure of squeeze infiltrated Al/carbon felt composite. Non-etched sample. Conventional light (a, b, d, f, h) and
phase contrast (c, e, g, i)
88
AlTi4/carbon felt composite

Matrix: AlTi4 aluminum alloy (3.8 wt. % Ti).
fibrous organic material by POLGRAPH company, Nowy Scz (Poland). The preform consists of
individual carbon fibers of the 10-13 m thickness with a random spatial distribution and in-plane
Manufacturing method: squeeze infiltration of the thermally-activated carbon preform by liquid
aluminum alloy at 1000C, under a pressure of 230 MPa, for 30 s; die temperature - bottom/top:
130-180/120-160C.
expansion, decreased electrical and thermal conductivity, good machinability, and advantageous
Structural characteristics (Fig. II.2.3): the character of carbon fiber arrangement in the AlTi4 metal
matrix is similar to that in pure aluminum. The distinguishing feature is the presence of the Al3Ti phase
precipitates in the metal matrix alone, especially on the preform edges (Fig. II.2.3 a). Their rounded
shape indicates that they are primary precipitates, which have not quite been dissolved in the matrix
during its melting. Within the preform, the Al3Ti phase appears in the form of fine needles, often
growing on the surface of the carbon phase, including the surfaces of the carbon flakes (Fig. II.2.3 b)
as well as the carbon fibers (Fig. II.2.3 c).
Figures II.2.3 b-d show structural defects, in the form of cracks, that occur occasionally in the carbon
phase of the composite. An examination of the regions under polarized light revealed that the origin of
these defects is linked with the carbon felt manufacturing process. In particular, these discontinuous
form as a result of wetting of the whole group of fibers by a large amount of binder in such a way as to
fuse the fibers inside large flakes of binder while maintaining the same uniform and directionally
oriented arrangement as in remaining part of the felt. Also, because during the felt manufacturing
process the binder gets carbonized, the homogeneity of the carbon phase areas is maintained. The
fractured areas (cracks) appearing in such flakes are not filled with metal, which proves that they are
formed after the infiltration process is complete, probably during cooling of the composite as a result of
considerable solidification shrinkage, which is characteristic for the matrix alloy. The phenomenon of
cracking of large flakes of the carbon phase does not occur in the case of other matrix alloys (e.g.,
AK12 alloy or pure Al).
d
Fig. II.2.3.
Structure of squeeze infiltrated AlTi4/carbon felt composite. Non-etched sample. Polarized light
89
90
AK12 / carbon felt composite

Matrix: AK12 aluminum alloy (AlSi12CuNiMg) - 12.2 Si, 1.15 Cu, 0.95 Ni, 0.90 Mg, 0.60 Fe, 0.20 Zn
0.19 Mn, 0.09 Ti (wt. % ).
Manufacturing method: squeeze infiltration of the thermally-activated carbon preform by the liquid
aluminum alloy at 760C, under a pressure of 230 MPa for 30 s; die temperature - bottom/top:
130-180/120-160C.
Structural characteristics (Fig. II.2.4): The characteristic feature of carbon felt-reinforced AK12
alloy-matrix composite is a complete lack of structural discontinuous inside the carbon preform and
even very large flakes of the carbon phase do not show any minute cracks (Fig. II.2.4 a-f).
91
h
Fig. II.2.4.
Structure of squeeze infiltrated AK12/carbon felt composite. Non-etched sample. Polarized light (a-f) and
conventional light (g-h)
92
II.3.
Carbon felt-reinforced zinc composites
Zn/carbon felt composite

Matrix: pure zinc (99.6 wt. % Zn).
Manufacturing method: squeeze infiltration of the thermally-activated carbon preform by liquid zinc at
550C, under a pressure of 230 MPa for 30 s; die temperature - bottom/top: 130-180/120-160C.
Structural characteristics (Fig. II.3.1): under conventional light, the composite structure
(Fig. II.3.1 a-e) shows defects in the form of structural discontinuities (due to the lack of metal
infiltration into the enclosed space between aggregates of permanently bonded fibers) (Fig. II.3.1 b-d).
In contrast to the Al matrix, in the case of Zn matrix, the minute cracks were found in large carbon
phase flakes, and some of these cracks were filled with metal (Fig. II.3.1 e). The use of polarized light
allows observation of the zinc matrix structure, i.e. its directional solidification and twinning
(Fig. II.3.1 f-o). Within the area around a single grain of the matrix phase, the directional arrangement
of twins is the same as the direction of fracture in the carbon phase flake in this grain (Fig. II.3.1 o).
93
94
n
Fig. II.3.1.
Structure of squeeze infiltrated Zn/carbon felt composite. Non-etched sample. Conventional light (a-e) and
polarized light (f-n)
II.4.
95
Carbon felt-reinforced lead composites
Pb / carbon felt composite

Matrix: pure lead (99.6 wt. % Pb).
Manufacturing method: squeeze infiltration of the thermally-activated carbon preform by liquid lead
at 480C, under a pressure of 230 MPa for 30 s; die temperature: bottom - 130-180C, plunger
120-160C
Properties: substantially lower density, increased hardness and strength, lower plasticity, decreased
thermal expansion, decreased electrical (insignificantly) and thermal conductivity, good machinability,
and advantageous economic and ecological manufacturing parameters.
Structural characteristics: selected technological process ensures good infiltration of the fibrous
preform with liquid lead together with the establishment of intimate contact between the reinforcement
and the matrix as well as their good interfacial bonding.
Fig. II.4.1.
SEM images of fracture of Pb/carbon felt composite
96
Long fiber-reinforced composites
III.
III.1.
Carbon fiber-reinforced aluminum composites
AlTi4/carbon fiber composite

Matrix: AlTi4 aluminum alloy (3.8 wt. % Ti).
Reinforcing phase: long (continuous) carbon fiber of PAN type, shaped into porous preform.
Individual carbon fibers of about 8 m diameter, spatially distributed and oriented in one selected
direction in the preform.
Manufacturing method: squeeze infiltration of the thermally-activated carbon fiber preform by the
liquid alloy at 1000C, under a pressure of 230 MPa for 30 s; die temperature - bottom - 180C,
plunger: 170C.
Properties: substantially lower density (down to 2.15 g/cm3), increased stiffness and strength, and
significantly lower thermal expansion (especially in the direction of fiber orientation).
Structural characteristics: (Fig. III.1.1): in spite of the presence of a large volume fraction of the
reinforcing phase in the preform, the use of squeeze infiltration causes complete filling of the carbon
fiber preform by liquid metal matrix. This is the reason for the complete absence of structural
discontinuities, such as porosity, which would form due to impossibility to locally wet the reinforcing
phase (Fig. III.1.1). An additional factor, positively influencing the homogenous arrangement of the
fibers in the metal matrix, is the use of titanium as an alloy additive to aluminum matrix. Titanium
increases chemical interaction in the fiber/matrix system. It also contributes to improving
physiochemical compatibility of the composite components by slowing down the formation of
undesirable aluminum carbide (Al4C3) while at the same time ensuring an improvement in wettability of
carbon fibers by the liquid matrix.
97
Fig. III.1.1.
Structure of squeeze infiltrated AlTi4/carbon fiber composite. Non-etched sample. Conventional light (a, b, d, f)
and phase contrast (c, e, g)
98
Al/carbon fiber composite (nickel-coated)

Matrix: pure aluminum (99,99 wt. % Al).
Reinforcing phase: long (continuous) carbon fiber from CYANAMID (USA) nickel coated (50 wt. %
Ni), formed into a preform. The preform consists of individual nickel-coated carbon fibers of about
10-18 m thickness spatially distributed and oriented in one selected direction.
Manufacturing method: squeeze infiltration of the thermally-activated carbon fiber preform by liquid
aluminum at 1000C, under a pressure of 230 MPa for 30 s; die temperature bottom/top: 180/170C.
Properties: increased rigidity and strength, lower thermal expansion (especially in the direction of
fiber orientation)
Structural characteristics (Fig. III.1.2): the Al-matrix composite, reinforced with nickel-coated carbon
fibers (Cf(Ni)), is characterized by relatively homogenous arrangement of fibers in the metal matrix on
a macro-scale (Fig. III.1.2 a). However, on a micro-scale, in spite of a very good wettability of nickel
coated carbon fibers by the liquid Al, there are agglomerates of fibers in the composite (Fig. III.1.2 b)
as well as structural discontinuities in the form of porosities inside these agglomerates. Structural
analysis under higher magnifications (about 500x) shows that these are primary flaws occurring in the
preform in the initial state before infiltration and preform solutioning with liquid metal. These primary
flaws originate in the process of nickel coating, which is usually carried out on a bundle of a few
hundred fibers. Additionally, occasional bonding of a few to a few dozens of fibers into one
conglomerate may take place, which then gets coated with one common nickel layer. This creates
enclosed porosity between fibers, which is impossible to be filled by liquid metal even under high
pressure. Interestingly, in areas where heterogeneous arrangement of fibers can be observed, there is
also heterogeneous thickness of the nickel coating, with the coating thickness even exceeding the
fiber diameter itself.
Under higher magnifications, eutectic Al-Al3Ni is revealed in grain boundaries, which results from the
dissolution of the nickel coating in the liquid Al.
b
Fig. III.1.2.
Structure of squeeze infiltrated Al/nickel coated carbon fiber composite. Non-etched sample. Conventional light
III.2.
99
Carbon fiber-reinforced copper composites
Cu/carbon fiber composite

Matrix: pure copper (99.7 wt. % Cu).
Reinforcing phase: long (continuous) carbon fiber of PAN type, shaped into a preform. Individual
carbon fibers of about 8 m diameter, spatially distributed and oriented in one selected direction in the
preform. The initial preform thickness was 5 mm, with relatively loosely arranged, but directionally
oriented fibers.
Manufacturing method: infiltration of the thermally-activated carbon fiber preform by liquid copper at
1200C under a pressure of 230 MPa for 60 s; die temperature - bottom/top: 300/270C.
Properties: substantially lower density, increased rigidity and strength, significantly lower thermal
expansion (especially in the direction of fiber orientation)
Structural characteristics (Fig III.2.1): due to a relatively loose character of fiber arrangement in the
preform and initially, during pressure application, the metal infiltration is accompanied by thickening of
the preform in such a way as to obtain local reinforcement of the cast surface, up to 0.5 mm.
The areas between the fibers are completely filled with liquid matrix; however, in areas where the
fibers were not sufficiently stiffened, the loss in the homogeneity of fiber arrangement may
occasionally occur in the metal matrix because of their displacement during infiltration with liquid metal
and bunching together into agglomerates of several fibers (Fig. II.2.1 a, b). For comparison, in areas
where the fibers are immobilised, their arrangement in the metal matrix is homogenous (Fig. III.2.1 c).
Under large magnifications, micro-cracks are revealed inside individual fibers (visible in figures
III.2.1 b, c). Their location and shape suggest that they are formed during preparation of the sample
itself for the structural examination, most probably, during cutting of the composite casting.
100
Fig. III.2.1.
Structure of squeeze infiltrated Cu/carbon fiber composite. Non-etched sample. Conventional light (a, b, d) and
phase contrast (c, e)
101
III.3.
Sapphire fiber-reinforced nickel composites
NiAl/saphire fiber composite

Matrix (at. %): nickel-base intermetallic NiAl (49.9-50.3Ni, 49.7-50.1Al), NiAl(Yb) (62.1-62.6Ni,
36.8-37.3Al, 0.36-0.11 Yb), NiAl(Cr) (60.2Ni-28.2Al-11.4Cr), and NiAl(W) (67.4Ni-31.4Al-1.5W).
Reinforcing phase: long (continuous) single crystal sapphire fibers (SaphikonTM) with average
diameter 178 m.
Manufacturing methods: two methods of composite manufacture were utilized:
1. NASAs patented Powder-cloth (PC) technique in which a cloth or sheet of atomized matrix
powders is created by mixing them with Teflon binders and a solvent to a dough-like consistency;
fiber mats of specified thickness are produced by filament winding and by application of a PMMA
coating; matrix cloth and fiber mats are then stacked in layers and vacuum hot pressed during
which binders are removed; the orientation of individual plies and stacking sequence provide
flexibility in designing the composite properties.
2. Floating-zone directional solidification (DS), which is a container-less solidification technique to
produce the composites. The DS was done on either powder-cloth feedstock with ~25 vol. % fibers,
or on vacuum induction melted and chill cast (in Cu-mould) composites (the chill cast composites
had low, <0.5%, fiber volume fraction and were fabricated by laying sapphire fibers in a Cu-mould
with fiber ends rigidly supported within holes drilled in steel end caps). The DS was done under
3 psi (gauge) pressure of ultrahigh purity argon gas in a 25 kW radio frequency (RF, 400 kHz)
vacuum induction furnace using a water-cooled copper current concentrator; a current adjusting
type three-mode proportional controller was used to set the temperature and control the power
input to the coil; DS was carried out by traversing a 8 mm long molten zone along the length of the
feedstock at a constant speed (~6.0 cm/h).
Properties: substantially lower density, increased rigidity and strength at room-temperature and
elevated temperatures, significantly lower thermal expansion (especially in the direction of fiber
orientation), increased hardness, decreased ductility, and improved wear resistance are expected.
With W and Cr alloying of NiAl and incorporation of sapphire in the composite, dual-phase toughening
potential together with high-temperature strength is expected in the composite.
200 m
25 m
a
Fig. III.3.1.
Structure of NiAl/saphire fibers composite made by powder-cloth (PC) method. The arrows in (b) denote the
residual micro-porosity from incomplete densification of the NiAl matrix powders during composite fabrication
Structural characteristics: in the powder-cloth (PC) composite, polycrystalline NiAl matrix contains
rows of sapphire fibers distributed in the matrix (Fig. III.3.1 a), and there is some residual porosity
(marked by arrows in Fig. III.3.1 b). After hot pressing there is no evidence of interfacial reaction. The
directional solidification (DS) of polycrystalline PC feedstock reduced the number of NiAl grain
boundaries coincident on the fiber surface (Fig. III.3.2), which led to an increase in the
room-temperature fiber/matrix interfacial shear strength. This is because the NiAl grain boundaries
coincident on the fiber surface act as crack initiation sites during loading of the fiber. In a manner
102
similar to the PC composites, there was no evidence of interfacial reaction layers in the DS
composites; however, porosity in the matrix persisted after the DS. The surface appearance of
sapphire fibers extracted the sapphire-NiAl matrix composites synthesized by different fabrication
techniques is shown Fig. III.3.3; there is no evidence of extensive surface degradation or damage. The
original fiber distribution of the PC feedstock was slightly altered after DS (Fig. III.3.2), but the overall
uniformity of fiber distribution was not appreciably affected. The matrix structure of the DS composites
(Fig. III.3.2) exhibited coarser grains, as compared to the NiAl matrix in the PC composites
(Fig. III.3.1).
Unlike Yb in NiAl, chromium alloying of NiAl only moderately attacks the sapphire; Cr preferentially
precipitates on to the sapphire fiber, as revealed by the SEM examination (Fig. III.3.4) of fibers
separated from the NiAl(Cr) matrix by etching. In addition, Cr bonds to the sapphire fiber (Fig. III.3.5).
There is, however, no evidence of reaction product layer formation. The DS structure of the
NiAl(Cr)/sapphire composite displays NiAl cells with fine Cr precipitates distributed within the cells and
the eutectic in the intercellular colonies (Fig. III.3.6). Depending upon whether the fiber resides
predominantly in the intercellular colonies or within the NiAl grains, preferential segregation of either
eutectic Cr or primary Cr precipitates, respectively occurs at the fiber/matrix interface (Fig. III.3.7).
In contrast to both Yb and Cr alloying of NiAl, with 1.5 at. % W in NiAl, the fiber/matrix interface is
completely devoid of any reaction products and secondary precipitates (Fig. III.3.8.). The addition of
W and Cr to NiAl and incorporation of sapphire in the composite creates fiber-reinforced composites
with dual-phase toughening potential together with attainment of high-temperature strength.
200 m
25 m
a
Fig. III.3.2.
Structure of NiAl/saphire fibers composite after directional solidification (DS) from PC feedstock. The arrows in
(a) indicate the porosity in the matrix. The DS was done in the floating-zone mode. DS reduced the number of
NiAl grain boundaries coincident on the fiber surface, which led to an increase in the fiber/matrix interfacial shear
strength. No interfacial reaction layers at optical magnifications. Non-etched sample
100 m
a
Fig. III.3.3.
SEM views of the surface of fibers extracted from NiAl/sapphire fibers composites processed under the following
conditions: (a) powder-cloth (PC) composites that were subsequently directionally solidified using the
floating-zone directional solidification (DS) technique, (b) vacuum induction melted and chill cast (in copper
mould) composites after DS in the floating-zone mode. The fibers were extracted from the composite by
dissolving the matrix in a boiling solution of 75% acetic acid, 23% nitric acid, and 2% HCl acid. Average fiber
diameter 178 m. The matrix contained equi-atomic fractions of Ni and Al
103
1 m
7 m
a
Fig. III.3.4.
SEM view of a sapphire fiber extracted from a sapphire-reinforced NiAl(Cr) composite at (a) low- and (b) high
magnifications. The composite was fabricated using the floating-zone directional solidification (DS) of vacuum
induction melted and chill cast composite (fiber volume fraction ~0.5 wt. %, average sapphire fiber diameter
178 m). The fiber surface shows good bonding between the chromium precipitates and the oxide fiber. The
fibers were extracted from the composite by dissolving the matrix in a boiling solution of 75% acetic acid, 23%
nitric acid, and 2% HCl acid
30 m
Sapphire/NiAl(Cr)
interface region
Eutectic chromium
Sapphire fiber
Cr precipitates
Eutectic chromium
2 m
c
Fig. III.3.5.
SEM views of the fiber/matrix interface in a directionally solidified NiAl(Cr)/sapphire fibers composite: (a)
chromium-rich layer around a sapphire fiber embedded in the composite matrix, (b) a higher magnification view
of a region of Fig. (a), and (c) the sapphire/NiAl(Cr) interface region showing intimate bonding between eutectic
Cr particles and the sapphire fiber. Also noticeable is the cellular NiAl matrix structure and the fine secondary Cr
precipitates that form from supersaturated NiAl matrix during cooling at the conclusion of solidification. The
composite was produced by vacuum induction melting and chill casting in a copper mould followed by directional
solidification (DS) in the floating-zone mode. The fiber volume fraction in the composite: ~0.5 wt. % with
average fiber diameter of 178 m
104
a
Fig. III.3.6.
SEM photomicrographs of a directionally solidified NiAl(Cr)/sapphire fibers composite in a fiber-free region

showing the cellular NiAl structure with intercellular NiAl-Cr eutectic (a), and a higher magnification view of
a eutectic region (b). The DS was carried out in a floating-zone mode. The SEM views in (a) and (b) are
transverse to the growth direction. The composition of the matrix alloy after DS (in at. %) is: 60.2Ni-28.2Al11.4Cr and ~300 ppm oxygen
Secondary Cr
precipitates and
wear tracks
Eutectic Cr
Fiber
Fiber
2 m
a
Fig. III.3.7.
SEM views of de-bonded interfaces in DS NiAl(Cr)/sapphire fiber composite after the fiber push-out test. The DS
was done on vacuum induction melted and chill cast feedstock (fiber volume fraction < 0.5%). Front-face of
a composite wafer showing secondary Cr precipitates within the NiAl cells and microplastic grooving of the NiAl
matrix during sliding of the fiber (a), and preferential segregation of eutectic Cr at the fiber/matrix interface in the
region of the displaced fiber (b). The composition of the DS matrix (in at. %) is 60.2Ni-28.2Al-11.4Cr and
~300 ppm oxygen
a
Fig. III.3.8.
4 m
Fiber
Fiber/matrix interface in NiAl(W)/sapphire composite produced by vacuum induction melting and chill casting in
a copper mould followed by directional solidification (DS) in the floating-zone mode. Reaction-free fiber/matrix
interface on a polished surface (a) and within the region of a pushed fiber in a fiber push-out test (b). The fiber
volume fraction in the composite: ~0.5 wt. %, average fiber diameter is 178 m, and the composition of the
matrix (in at. %) is 67.4Ni-31.4Al-1.5W and ~300 ppm oxygen
105

Nickel-base superalloy (Hastealloy)/sapphire fiber composite
Matrix: Nickel-base superalloy of composition (in wt. %): 47.5Ni-21.5Cr-17.8Fe-8.3Mo-1.7Co-0.3Mn0.4Si-0.2Al-0.1Cu-0.4Nb-0.06Ti-0.08C-0.020.

Reinforcing phase: single crystal sapphire fibers (SaphikonTM), average fiber diameter: 130 m.
Manufacturing method: pressure infiltration casting in a pressure vessel that contained a pair of
induction coils, powered with a RF generator, to independently heat preform and metal; preforms of
uni-directionally aligned sapphire fibers in recrystallized alumina moulds; top-pour infiltration
configuration; melt temperature: 1400-1500C; infiltration time: 3-5 min; pressurizing gas:
ultrahigh-purity argon; samples cooled at the conclusion of infiltration with argon gas inside the pressure
chamber.
Properties: increased hardness and strength at room-temperature and elevated-temperatures, strong
interfacial bond, decreased ductility, improved wear resistance, and decreased thermal expansion are
expected.
Structural characteristics: good penetration of inter-fiber channels occurred (Fig. III.3.8); some
fiber-to-fiber contact was unavoidable because of high fiber volume fractions. Short infiltration times and
large fiber contents limited the extent of fiber attack by the reactive solutes (e.g., Cr) of the matrix.
Structural observation of extracted fibers, however, showed evidence of chemical interaction.
500 m
200 m
10 m
50 m
c
Fig. III.3.8.
Structure of Hastealloy/sapphire fibers composite produced by pressure infiltration showing fibers distribution in
the cross-section of the infiltrated composite bar (a) and (b), and higher magnification views of the fiber
arrangement, and capillary channels between fibers (c) and (d). Fiber diameter 130 m
106
Gas reinforced composites (gasars)
IV. Gas "reinforced" composites (gasars)

Copper and nickel gasars
Matrix: pure copper, pure nickel
Reinforcing phase: gas in the form of bubbles of diversified morphology, dimensions and contents in
the metal matrix.
Manufacturing method: directional crystallization under pressure from liquid metal saturated with gas
mixture (hydrogen and argon or nitrogen) according to the know-how of a protected manufacturing
technique, known as gasar process or lotus-like structures process.
Properties: substantially lower density, increased mechanical properties, especially tensile strength
and plasticity (generally in case of the bubbles of diameter below 1-10 m range and their contents in
the structure up to 30 vol. %) in the direction of bubble growth, increased damping of mechanical
energy and sound, possibility to obtain continuous bubbles, i.e. by creating open porosity (permeable
structures).
300 m
70 m
300 m
c
Fig. IV.1.
SEM images of the fractured copper gasars under various magnifications
20 m
107
300 m
300 m
300 m
300 m
70 m
70 m
108
20 m
20 m
g
Fig. IV.2.
SEM images illustrating the structural changes in the nickel gasar, depending on the technological parameters of
the manufacturing process. Transverse cross-section (a, c, e, g) and lengthwise section (b, d, f, h)
Structural specifics: gasars can be classified as a separate, specific group of metal composite
materials manufactured using liquid-phase techniques. Gas being released from liquid metal (during
directional solidification, under variable ambient pressure) is regarded as a reinforcing phase.
For the purpose of practical applications, the most desirable bubble morphology is the one that closely
resembles cylindrical, parallel and evenly arranged capillaries, allowing full permeability of gasars in
a direction parallel to crystallization front to be achieved.
Final structure
Solid phase
Gas phase
Liquid
Gas
Cooling direction
1<2<3
Fig. VI.3.
Proposed scheme of gasar growth kinetics based upon structural examination, during different time of directional
solidification () at a constant velocity. The fracture surface of a copper gasars is shown as a final structure
under original magnification of 35x (SEM)
Solid phase
Gas phase
Metallic liquid
Gas
Non-metallic inclusions
Cooling direction
Fig. IV.4.
SEM micrographs and corresponding evaluation schemes of the nickel gasar structure formation beginning from
quasiboiling process (blister-like structure) (a) through the increase of crystallization velocity Vs (b, c, d) and
development of required dendritic structure (e)
109
Nano-composites
V.
Nano-composites
AlSi7Mg/ carbon nano-fibers composite

Matrix: AK7 aluminum alloy (AlSi7Mg) - 7.24 Si, 0.35 Mg, 0.46 Fe, 0.20 Mn.
Reinforcing phase: pipe-like carbon nano-fibers (Fig. V.1), thermally treated and known by the trade
name - Pyrograf - III (PR-19-LHT); these nano-fibers have high graphite content and unique
combination of properties, especially high thermal conductivity, the highest out of all known reinforcing
phases (Table V.1).
Fig. V.1.
Structure of the Pyrograf - III nano-fiber after catalytic elongation and thickening (CVD - chemical vapour
deposition). Thickness of the nano-pipe wall in the initial stage is about 20 nm ( 20%)
Table V.1.
Selected physical, mechanical and thermal properties of the Pyrograf - III nano-fibers in relation to heat treatment
Properties
3
Thickness, g/cm
Tensile strength, GPa
Young module, GPa
Thermal expansion coefficient, m/mK
Electrical resistance, cm
Thermal conductivity, W/mK
Nano-fibers as-received
1.8
2.7
400
1000
20
Nano-fibers after heat treatment

2.1
7.0
600
-1.0
55
1950
Properties: lower density, significantly increased stiffness and strength, significantly lower thermal
expansion, drastically increased thermal conductivity.
Manufacturing method I: squeeze infiltration of the loose carbon fibers deposit by liquid alloy at
740C, under a pressure of 120 MPa for 30 s; die temperature - bottom/top: 180/220C.
Structural characteristics (Fig. V.2): optical microscopy examination of nano-composites at the
micro-scale has only illustrational value due to the very fine dimensions of individual nano-fibers,
which are impossible to be. In the next stage of structural examinations, it is necessary to use high
resolution electron microscopy (HREM). Nevertheless, even observations under an optical microscope
show that arrangement of the reinforcing phase is non-uniform. There are areas of varying degree of
nano-fibers density, which may not be properly described even as nano-fiber colonies.
110
Nano-composites
Fig. V.2.
Structures of AK7/carbon nano-fibers composite obtained by squeeze infiltration of loose-bed nano-fibers

deposits. Transition layer: alloy-composite as well as structural areas illustrating arrangement of reinforcing
phase under various magnifications. Non-etched sample. Conventional light (a, b, d, f), phase contrast (c, e, g)
111
Nano-composites
Manufacturing method II: squeeze infiltration of the thermally-activated carbon nano-fiber preform
bonded with hydrated sodium silicate (about 75 vol. % porosity) with liquid alloy at 740C under
a pressure of 120 MPa for 30 s; die temperature - bottom/top: 180/220C.
Structural characteristic (Fig. V.3): observations under the optical microscope, especially with
500-1000x magnifications, show colonies of nano-fibers located in the preform walls, and being
divided by a significant amount of unburned (unremoved) bonding compound. In this case,
a heterogeneous arrangement of fibers in the infiltrated preform results from the specifics of the
preform preparation technology itself.
112
Fig. V.3.
Nano-composites
Structure of AK7 alloy reinforced with carbon nano-fiber preform by squeeze infiltration. Non-etched sample.
Conventional light (a, b, d, f) and phase contrast (c, e, g)
113
Nano-composites
Al/50 wt. % carbon nano-fibers composites
Matrix: pure aluminum.
Reinforcing phase: pipe-like carbon nano-fibers (Fig. V.1), thermally treated and known by the trade
name - Pyrograf - III (PR-19-LHT); these nano-fibers have high graphite content and unique
combination of properties, especially high thermal conductivity, the highest out of all known reinforcing
phases.
Manufacturing method: powder metallurgy (know-how)
Structural characteristics (Fig. V.4): microscopic observations show relatively uniform arrangement
of the nano-fiber colonies in comparison to liquid-phase methods. A characteristic feature of the
microstructure is the arrangement of the fiber colonies along the direction of deformation.
d
Fig. V.4.
Structure of Al/50 wt. % carbon nano-fibers composite obtained by powder metallurgy. Cross section (a, b) and
longitudinal section (c, d) related to the deformation direction. Non-etched sample. Conventional light
114
VI.
Typical structural defects in metal-matrix composites
VI.1. Particulate dispersion-reinforced composites

VI.1.1. Macro-scale nonuniform arrangement of the reinforcing phase (macro segregation) in
gravity cast composites, linked with the stability loss of initially homogenous metal-ceramic
slurry obtained, due to a significant density difference between reinforcing phase (dzb) and
metal matrix (dMe), resulting in either sedimentation phenomenon of the reinforcing phase
dzb > dMe or floating phenomenon of the reinforcing phase at dzb < dMe (Fig. VI.1.1).
b
Fig. VI.1.1.
Macrostructures of the lengthwise cross-sections of gravity cast composite ingots illustrating segregation of
reinforcing phase as a result of: a) sedimentation of the silicon carbide particulates in the A356/20 vol. % SiC
composite, for which dSiC>dA356; b) graphite floatation in the AK12/5.7 wt. % nickel coated graphite (50 wt. % Ni)
composite, for which dGr<dAK12
115
VI.1.2. Micro-scale nonuniform arrangement of the reinforcing phase (micro segregation) in

gravity cast composites, as a result of particulates agglomeration phenomenon (gathering
together of the particulates, contacting each other, into agglomerates, containing from few to
several dozens of particulates) (Fig. VI.1.2.1).
Three types of agglomeration are distinguished in metal matrix composites:
1) Primary agglomeration occurrs in the reinforcing phase before it gets introduced into the liquid
metal matrix and characterized by varying stability.
Particulates in unstable agglomerates, called soft agglomerates, are held by relatively week Van der
Waals forces or electrostatic ones, and whose de-agglomerating can be achieved by additional sifting,
mixing themselves or mixing with other powder, directly prior to the introduction of reinforcement into
the metal matrix.
In stable agglomerates, called hard agglomerates, the particulates are linked with each other by
permanent bridges, which do not get completely destroyed even during intensive mixing in molten
metal bath and in the same undestroyed state they are then permanently imbedded in solidifying
composite casting. In this case, the phenomenon of inheriting primary heterogeneity of the reinforcing
phase takes place, which can be effectively prevented by additional powder milling operation coupled
with its de-agglomeration using other powder material.
2)
Secondary agglomeration occurs during liquid-state processing, i.e. at some stages in the
formation of the metal-ceramic slurry or solidification of the composite casting. It is directly linked
with the particulate-liquid matrix or particulate-solid matrix interactions, which determine the
character of a particulate arrangement in the liquid metal bath or in the solidified composite
casting. Even initial de-agglomeration of the reinforcing phase prior to its introduction to the bath,
does not ensure homogenous arrangement of the reinforcing phase in the final product.
The following phenomena contribute to secondary agglomeration formation:
Interaction between reinforcing phase particulates and gas bubbles in the metal bath or as
a result of gas adsorption from the bath surface, which contributes to creation of clusters
containing few or a dozen of particulates linked with common blister (Figs. VI.1.2.2 a, b) or gas
layer (Fig. VI.1.2.2 c).
Local non-wetting of the reinforcing phase by liquid matrix, which contributes to a particle-particle
interaction in metal-ceramic slurry and facilitates gathering of the particulates in agglomerates in
such a way, that they touch each other but some voids remain between these particles because
they are non-wettable by the liquid matrix (Fig. VI.1.2.3).
Pushing out of the reinforcing phase particulates in front of the solidifying metal matrix (pushing
phenomenon), causing their forced undesirable redistribution. Significant fact is, that after
creating very homogenous metal-ceramic slurry using intensive mechanical stirring method, the
gravity castings of such composites have relatively homogenous distribution of the reinforcing
phase in the metal matrix on the macro-scale. However, the observation of the structure in the
micro-scale shows considerable segregation of the reinforcing phase particulates. This is linked
with the phenomenon taking place in the composite casting already during its solidification, thus
not really being a proof of the lack of homogeneity of the suspension formed. In case of
aluminum alloys matrix composites, the solidification begins from the formation of primary
precipitates of the solid phase solution. Further growth of its dendrites causes pushing
reinforcement phase particulates out, which are gathered, following solidification process, as
agglomerates in the eutectic between -phase dendrites (Fig. VI.1.2.4). The use of
technological operations decreasing grain size of primary phase precipitates, effectively
enhances homogeneity of the reinforcement phase distribution in the aluminum matrix of the
gravity cast composites (e.g. refining, use of the external pressure, fast cooling).
3) Ternary agglomeration occurs at some stages in creation of metal-ceramic slurry or during

formation of composite casting, due to the action of some external factors (e.g. centrifugal or
electromagnetic force), forcing a violent particulates movement in a particular direction, their
congestion and formation of agglomerates containing large amount of particulates.
The difference between secondary and ternary agglomerates based upon structural examinations
is difficult, because visually they look very much alike. In this case decisive significance has the
comparison of the same composite material structure, cast in two methods - gravitationally and
with the presence of external factor (i.e. two composite samples are manufactured in one
experiment using two different methods, but out of the same composite slurry). Such example of
the copper alloy matrix composite containing graphite particulates, is shown on Figs. I.6.2 and
I.6.3.
116

Following gravity casting, the composite has very homogenous structure, which results from
uniform arrangement of graphite phase in the matrix (Fig. I.6.2). This is a testimony to not only
a very high degree of homogeneity of the composite slurry obtained, but also of its sufficient
stability, allowing to permanently form such a structure during further solidification of matrix in the
gravity casting. The same homogenous and sufficiently stable in gravity conditions slurry becomes
unstable under the centrifugal force, which manifests itself by the formation of ternary
agglomerates occurring only in the external layer of the centrifugal casting (Fig. I.6.3).
d
Fig. VI.1.2.1.
Structure of squeeze cast AG10/5.0 wt. % fly ash composite, illustrating occurrence of primary agglomeration;
(a, b) depict stable (hard) agglomerates, while (c, d) depict the agglomerate of the particles, which partially
becomes destructed, because fly ash particles are separated with a metal-matrix layer, maintaining their initial
position though, in relation to each other (structure heredity phenomenon). Non-etched sample. Phase contrast
(a, c, d) and conventional light (b)
117
c
Fig. VI.1.2.2.
Structure of gravity cast AK12/3.7 wt. % fly ash composite (Dayton Power and Light Co., USA), illustrating
secondary agglomeration due to particle-gas bubble interaction. Non-etched sample. Conventional light
Fig. VI.1.2.3.
SEM image of gravity cast F3S.15S composite fracture (A359/15 vol.% SiC), depicting secondary agglomeration
of a few SiC particles due to local non-wetting of reinforcing phase by the liquid matrix evidenced by the absence
of continuous contact between SiC particles and metal matrix)
118
Fig. VI.1.2.4.
Structure of gravity cast F3S.15S composite (A359/15 vol. % SiC). Arrows show secondary agglomeration effect
due to particle pushing phenomenon in such a way that the reinforcing particles are being gathered in low
melting temperature matrix component (in this case, the Al-Si eutectic). Non-etched sample. Polarized light
119

VI.1.3. Porosity - gas bubbles and shrinkage
This type of structural macro discontinuity is characteristic to gravity casting. The main reason for the
gas bubbles to occur is excessive gassing of the composite slurry during melting of metal-matrix or
during intensive mechanical stirring of metal bath itself while introducing reinforcing phase. The
presence of ceramic particles in the bath contributes to increasing stability of gas bubbles formed,
because particulates gather on the bubble surface, creating rigid skeleton like three-dimensional
construction (Fig. VI.1.3.1). The occurrence of shrinkage porosity is liked with the tendency of the
metal matrix to shrink during solidification and further cooling of the casing. It is possible to
differentiate between these two types of porosity by the shape of the defect itself, because the gas
bubbles naturally have the spherical shape, while shrinkage porosity has irregular shape, often of very
developed area (Fig. VI.1.3.2).
b
Fig. VI.1.3.1.
Structure of gravity cast F3S.15S composite (A359/15 vol. % SiC), depicting the gas bubbles and shrinkage
porosity. None-etched sample. Polarized light
120
Fig. VI.1.3.2.
Structure of A356/20 vol. % alumina composite (COMRAL) cast into the metal mould, depicting
micro-shrinkage (marked with arrows). Non-etched sample. Polarized light
Fig. VI.1.3.3.
Structure of AK12/fly ash (microspheres) composite obtained by squeeze infiltration, depicting gas-shrinkage
porosity (marked with arrow). Non-etched sample. Phase contrast
121
VI.1.4. Excessive reactivity between the metal matrix and reinforcement

Reactivity in the metal-matrix reinforcement phase system ensures the formation of a good bonding
between matrix and reinforcement, but excessive reactivity can lead to undesirable effects including
structural defects.
1) Occurrence of the structural discontinuities as a result of cracking of the reinforcement

material
Example 1
High reactivity in Al fly ash system (Figs. VI.1.4.1, VI.1.4.2) may lead to intensive oxy-redox reaction
of the FexOy, SiO2 and mullite (main ingredients of the fly ash) with Al, which lead to the formation of
aluminum oxide, Si and Fe, and which are accompanied by cracking of fly ash particles.
Example 2
Cracking of the graphite phase in the aluminum matrix after heating of the Al-graphite slurry to the
temperature of about 950C, occurring due to excessive reactivity, stemming from the creation of the
aluminum carbide (Fig. VI.1.4.3). Similar phenomenon, in the case of the composites reinforced with
carbon fibers or graphite, leads to weakening fibers and falling level of composite mechanical
properties, and even their complete loss.
2) Increase of the composite structural heterogeneity

High reactivity in the Al - fly ash system (Figs. VI.1.4.1, VI.1.4.2) leads to rapid increase of the amount
and size of the primary Si precipitates, which have a tendency to grow on the fly ash particles, thus
contributing to the increase of the structural heterogeneity of such composite.
In the case of reinforcement in the shape of microsphere (Fig. VI.1.4.2) their cracking contributes to
filling cavity inside the microsphere with liquid metal (particularly in the case of casting under external
pressure). Inside the sphere, the content of Si and Fe is significantly higher than in the outside areas,
which also contributes to increasing structural homogeneity of the composite.
3) Formation of undesirable compounds

Example 1
Excessive reactivity in Al/C system leads to the formation of undesirable aluminum carbide (Al4C3),
which, actively reacting with water vapor, contributes to the creation of a gas product (methane), thus
weakening bonding between the matrix and the reinforcement phase and contributing to the formation
of micro-cracks in the ready product (Fig. VI.1.4.4).
Example 2
Similar to Al/C system, excessive reactivity in Al/SiC system may cause the formation of undesirable
Al4C3 compound (Fig. VI.1.4.5).
Example 3
Unproper conditions of manufacturing cast composites reinforced with metal-coated ceramic phase
lead to the excessive dissolving of the coating in the metal matrix, cause weakening of the bonding
between matrix and reinforcement, contributing to undesirable changes of the end product properties.
Widely used technological coating of the ceramic phase (e.g. carbon fibers, graphite powder and
aluminum oxide) is nickel coating, whose dissolving in the aluminum matrix causes the formation of
the excessive amount of brittle Al3Ni compound precipitations (Fig. VI.1.4.6).
122
Si
Si
Si
Fig. VI.1.4.1.
Structure of AK12/3.7 wt. % fly ash composite (Dayton Power & Light Co., USA), depicting excessive reactivity of
the fly ash particulates in contact with liquid matrix, which leads to reduction of such type of oxides as SiO2 and
mullite by Al (main fly ash ingredients) and the formation of Si. In the saturated with silicon metal-matrix, large
primary precipitations of the Si crystals form, growing on the surface of the ash particulates (arrows indicate
cracks in the particulates). Non-etched sample. Conventional light
Fig. VI.1.4.2.
Structure of 52K/15 vol. % fly ash composite, depicting cracking of the microsphere and its filling with the liquid
matrix as well as the formation of large amounts of Si and iron-reach precipitates inside the microsphere as
a result of chemical reactions taking place between liquid matrix and oxides. Sample etched with Kevlar agent.
Polarized light
123
Al4C3
Fig. VI.1.4.3.
Structure of Al-graphite composite after heating to about 950C, depicting cracking of the large graphite particle,
due to excessive reactivity caused from aluminum carbide formation. Non-etched sample. Polarized light
Al
Al4C3
graphite
Fig. VI.1.4.4.
Structure of the Al/graphite interface after heating up to 950C for 30 min and weathering out in the open for
1 month. Al4C3 precipitates are visible at the metal graphite interface as well as deformation lines and cracks in
Al as a result of gas product formation (methane) due to reacting Al4C3 with water vapor from the atmosphere.
Non-etched sample. Polarized light
124
Fig. VI.1.4.5.
Structure of gravity cast F3S.20S composite structure (A359/20 vol. % SiC) after heating in the liquid state with
visible needle-like Al4C3 precipitates formed on the surface of SiC particles. Effective methods to prevent
occurrence of aluminum carbide in DURALCAN composites are: thorough temperature control of the liquid
suspension as well as increased silicon contents in the matrix (usually Si 7 wt. %). Non-etched sample.
Polarized light
125

VI.1.5. Contaminations and non-metallic impurities
Typical example of the contamination of the cast composites that may take place during improper
melting process is presence of continuous oxide films (Fig. VI.1.5).
c
Fig. VI.1.5.
Structures of gravity cast F3S.20S composite (A359/20 vol. % SiC), illustrating inhomogeneous distribution of
reinforcing phase due to the formation of the oxide films and their getting through from the areas inside the
composite casting. Non-etched sample. Polarized light
126
VI.2. Porous ceramic preform reinforced composites

VI.2.1. Structural discontinuities due to insufficient preform infiltration, caused, amongst the
others by low metal temperature, local non-wetting, insufficient infiltration pressure, capture of
gases inside the preform and lack of possibility to extract them (Figs. VI.2.1.1 - VI.2.1.3).
Fig. VI.2.1.1.
SEM images of the AK12/22 vol. % Al2O3 composite fracture, depicting the solidified infiltration front inside short
fiber preform (MORGAN Company) due to its unfinished infiltration with AK12 alloy (time of pressure being
exerted about 3 s)
Fig. VI.2.1.2.
127
SEM images of the AK12/20 vol. % Al2O3 composite fracture, depicting the solidified infiltration front inside short
fiber preform (DIDIER Company) due to its unfinished infiltration with AK12 alloy
128
Fig. VI.2.1.3.
Structure of AK12/fly ash composite (microspheres) obtained by squeeze infiltration of porous preform with AK12
alloy, illustrating its incomplete filling with liquid matrix due to insufficient wettability in the metal-ceramic system
(marked with arrow). Non-etched sample. Phase contrast
129
VI.2.2. Structural heterogeneity and discontinuities resulting from the improper preform
preparation
Both heterogeneous thickness of the nickel coating layer on the fibers as well as their heterogeneous
distribution contribute to the formation of significant Ni segregation in the matrix, where the areas
between the fibers are used up by eutectic (Al+Al3Ni), while other area by Ni solid solution in Al
(Fig. VI.2.2.1).
130
Fig. VI.2.2.1.
Structure of Al/nickel coated carbon fibers composite, depicting structural heterogeneities caused from
nonuniform distribution of reinforcing phase in Al matrix, nonuniform thickness of nickel coating and matrix
segregation due to the dissolution of Ni coating in liquid Al. Non-etched sample. Conventional light (a, b, d, f) and
phase contrast (c, e, g)
131

VI.2.3. Excessive reactivity between composite components
1) Cracking of the reinforcing phase (Fig. VI.2.3.1).
2) Weakening of the ceramic preform.

In the case of an intensive interaction between liquid matrix and binder component, used to
form a rigid construction of the ceramic preform, the mechanical weakening of the inter-fiber
bonding occurs in the preform. This is accompanied by changes of its dimensions and shape,
even crack appearance, thus contributing to undesirable changes of the end product
properties (Fig. VI.2.3.2).
3) Formation of undesirable compounds (Fig. VI.2.3.3).
4) Disadvantageous changes of the matrix chemical composition (Fig. VI.2.3.4).
Fig. VI.2.3.1.
Structure of Al matrix composite reinforced with porous preform made from short Al2O3 fibers and SiO2, depicting
cracking of the reinforcing phase as a result of its interaction with metal matrix. Non-etched sample. Phase
contrast (a-c) and conventional light (d)
132
200 m
SiO2 + Mg
SiO2 + 2Mg
Al(Mg) + Si
MgSiO2
2MgO + Si
[Al(Mg) + Si]eut
Mg
b
Fig. VI.2.3.2.
Structure of MgAl8Zn2 alloy locally reinforced with ceramic preform (MORGAN, UK), consisting of 95 wt. % short
fibers (96% Al2O3 and 4% SiO2) as well as 5 wt. % of SiO2-based binder, showing the dimensional and shape
changes of the preform, its deformation and cracking (a). Scheme (b) shows changes in the preform structure
caused from two effects, i.e. applied external pressure and weakening of interfiber connections in the preform
that takes place due to consumption of binder by chemical reactions liquid.
133
c
Fig. VI.2.3.3.
Structure of Al/carbon fiber composite obtained by gas pressure infiltration in the autoclave (p = 7 MPa,
T = 800C, = 30 min), depicting the formation of the aluminum carbide at the fiber/matrix interface. Non- etched
sample. Polarized light
a
Fig. VI.2.3.4.
Structure of the composite obtained with initially pure Al matrix and reinforced with nickel coated carbon fibers
using gas pressure infiltration in the autoclave (p = 7 MPa, T = 800C, = 30 min). As a result of intensive
interaction between nickel coating and Al, a complete dissolving of Ni in the metal matrix takes place, and thus
exposing the fibers. This causes further chemical reaction between Al and nickel and formation of large amount
of aluminum carbide (Al4C3). At the same time, a disadvantageous change of chemical composition of the matrix
itself, takes place, caused by rapid growth of Ni content as well as contributing to the formation of large amount
of brittle Al3Ni precipitates. Non-etched. Polarized light
134
VI.2.4. Non-metallic inclusions

Just like with particulate dispersion-reinforced composites, in case of continuous fibers reinforced
composites, there may be oxide films, especially appearing in the areas close to the castings surface
(Fig. VI.2.4.1).
c
Fig. VI.2.4.1.
Structure of AK11/carbon felt composite in the vicinity of the casting surface, depicting structural discontinuities
due to occurrence of oxide films. Non-etched sample. Conventional light
135
VI.3. Hybrid composites

In the case of hybrid composites, introduction of the second reinforcing phase may be aimed at
obtaining additional positive effect of increased structural homogeneity through preventing segregation
of the reinforcing phase, using the effect of the neutral buoyancy. To this effect, two phases are
selected in such a way, so that one of them had a density higher than the other, in comparison to
liquid matrix, thus ensuring significant limiting of the undesirable movement of the particulates in the
metal bath.
To make use of the neutral buoyancy effect it is required to strictly control the conditions of the
process, both of reinforcing phase preparation as well as manufacturing of the composite, while not
following these requirements contributes to increasing structural heterogeneity, in comparison to other
composites.
Example 1
In the Al/SiC/graphite type of composites, too thick nickel coating on the graphite particles causes
disadvantageous increase of their density, which contributes to speeding up of the sedimentation
process of both SiC and graphite reinforcing phases (Fig. VI.3.1).
Example 2
For excessive dissolution of the Ni in the liquid metal in case of the Al/SiC/graphite type composites
containing nickel coated graphite, the excessive increase of the matrix density itself takes place,
above that of the SiC phase. This causes increase of structural heterogeneity due to an undesirable
floating of particles, both SiC and graphite ones.
Fig. VI.3.1.
Structure of lower part of the gravity cast hybrid composite made from A356 matrix reinforced with 15 vol. % SiC
and 5 vol. % nickel coated graphite particles. Non-etched sample. Conventional light
136
SiC
Al3Ni
Al3Ni
SiC
Al3Ni
Graphite particle
Ni coating
Al3Ni
Fig. VI.3.2.
Al3Ni
Structure of hybrid composite produced from A356 alloy reinforced with 15 % silicon carbide and 5 % graphite,
gravity cast into the metal die. Sample etched with Kevlar agent. Conventional light
137
VI.4. High volume faction particulate-reinforced composites

Technologies, Inc., USA) of three average platelet sizes - 250-500 m diameter 25-50 m thickness;
50-250 m diameter 5-25 m thickness; and 20-70 m diameter 0.50-5 m thickness; both
as-received and Cu-coated SiC platelets were utilized.
Manufacturing method: counter-gravitational infiltration of packed binder-less silicon carbide platelets
(packing density ~52 %) by the molten 2014 aluminum alloy under nitrogen gas pressure; SiC platelets
were packed in quartz tubes via multistage compaction of loose powders; infiltration was done in
a stainless steel pressure vessel with a melting furnace, consisting of two semi-cylindrical heating
elements, housed inside the pressure vessel; quartz tubes containing packed SiC were attached using
leak-tight fittings to the lid of the pressure vessel which, upon closure, led to partial immersion of the tube
in the molten alloy held in a graphite crucible inside the pressure vessel; an argon blanket was maintained
over the SiC inside the quartz tube to reduce the oxidation of the liquid front; preheating time of SiC beds:
3-5 min; melt temperature: 800C; nitrogen gas pressure: variable, 525-850 kPa; infiltration time: 3-5 min;
slow cooling at the conclusion of infiltration in ambient air.
Both as received and copper-coated SiC platelets were infiltrated. Cu-coating was done to promote
the wettability and facilitate the infiltration. Copper coating was deposited on SiC using an electroless
plating technique. For this, SiC platelets were stirred for 3 h in a solution of 10 g/l of SnCl2 and 40 ml/l of
concentrated HCl. The platelets were then stirred for 15 min in a solution 0.5 g/l PdCl2 and 1 ml/l
concentrated HCl. After stirring, the solution was decanted, and platelets washed twice with distilled water.
Finally, the platelets were stirred for 15 min in the plating bath of following composition: 10 g/l
CuSO4.5H2O, 10 g/l NaOH, 50 g/l sodium potassium tartrate, and 10 ml/l formaldehyde. The coating
deposition was confirmed with the SEM examination.
thermal expansion coefficient and increase in the thermal conductivity, increased hardness and
strength, and decreased ductility.
Structural characteristics: A structural imperfection sometime observed in infiltrated composite bars
made from loosely-packed SiC beds is the disruption and channeling of the packed bed under melt
shear. This leads to the formation of clearly demarcated SiC-impoverished and SiC-enriched regions
(Fig. VI.4.1). Normal solidification microstructure (cored dendrites and interdendritic eutectic) of the
matrix alloy develops in the SiC-impoverished region of the disrupted compact (Fig. VI.4.2)
Another imperfection is the spatial variation of the composite microstructure with the infiltration height.
A greater amount of porosity and secondary phases precipitate near the top of the infiltrated bar and
less porosity and secondary phases form near the bottom (Fig. VI.4.3). In addition, a greater preferred
orientation (stratification) of the SiC platelets due to higher melt shear occurs at the bottom. Thus, both
the matrix solidification features (secondary phases, porosity) and SiC distribution vary with the
infiltration height, resulting in an undesirable spatial variation of the composite properties.
Finally, the chemical interactions between the reinforcement particulates and matrix after prolonged
contact at elevated temperatures gives rise to extensive degradation of the SiC platelets (Fig. VI.4.4)
due to the formation of a large amount of the brittle reaction product, aluminum carbide (Al4C3).
138
Typical structural defects in metal composites
200 m
Fig. VI.4.1.
Structure of 2014/xSiC composite showing channeling near the periphery of specimen transversed to the
infiltration direction. Sharply demarcated SiC-starved and SiC-enriched regions form because of channeling in
the packed SiC network under melt shear; pressure: 825 kPa, melt temperature: 800C, infiltration time: 3 min,
SiC size: 50-250 m diameter and 5-25 m thickness, as-received SiC. Non-etched sample. Conventional light
20 m
10 m
Fig. VI.4.2.
Structure of 2014/xSiC composite at two magnifications of cored dendritic structure in the channeled region (SiC
impoverished region) of sample of I.3.12; pressure of 825 kPa, melt temperature: 800C, infiltration time: 5 min,
SiC size: 50-250 m diameter and 5-25 m thickness, as-received SiC; the sample was color etched with
a solution of 4 g KMnO4 and 2 g NaOH in 1 l distilled water. Conventional light
139
10 m
a
Fig. VI.4.3.
10 m
Structure of 2014/xSiC composite showing the variation of microstructure and SiC distribution with height in
composite produced by infiltration counter to gravity. The microstructures are shown for samples cut lengthwise
across their diameters (i.e., views are parallel to the infiltration direction): (a) shows greater porosity and second
phase precipitation near the top of the infiltrated bar, and (b) shows less porosity and secondary phases at the
bottom (melt entrance) but also greater directional stratification of the platelets due to greater melt shear at the
bottom; pressure of 825 kPa, melt temperature: 800C, infiltration time: 5 min, SiC size: 250-500 m diameter
and 25-50 m thickness, Cu-coated SiC; the sample was color etched with a solution of 4 g KMnO4 and 2 g
NaOH in 1 l distilled water. Conventional light
10 m
Fig. VI.4.4.
Transverse section of 2014/xSiC infiltrated counter-to-gravity with a 30 min hold at 800C. The image, taken from
a section near the bottom of the infiltrated bar, shows extensive degradation of the Cu-coated SiC platelets due
to chemical reaction of SiC with molten Al upon prolonged contact; infiltration pressure: 525 kPa, melt
temperature: 800C, infiltration time: 30 min, SiC size: 50-250 m diameter and 5-25 m thickness, Cu-coated
SiC. Conventional light
140
VI.5. Long fiber-reinforced composites

NiAl/saphire fiber composite
Matrix: nickel-base intermetallic NiAl (49.9-50.3Ni, 49.7-50.1Al, at. %) and NiAl(Yb) (62.162.6Ni,
36.837.3Al, 0.360.11 Yb at. %).
Reinforcing phase: long (continuous) single crystal sapphire fibers (SaphikonTM) with average
diameter 178 m.
Manufacturing methods: two methods of composite manufacture were utilized:
1. NASAs patented Powder-cloth (PC) technique in which a cloth or sheet of atomized matrix
powders is created by mixing them with Teflon binders and a solvent to a dough-like consistency;
fiber mats of specified thickness are produced by filament winding and by application of a PMMA
coating; matrix cloth and fiber mats are then stacked in layers and vacuum hot pressed during
which binders are removed; the orientation of individual plies and stacking sequence provide
flexibility in designing the composite properties.
2. Floating-zone directional solidification (DS) which is a container-less solidification technique to
produce the composites. The DS was done on either powder-cloth feedstock with ~25 vol. % fiber,
or on vacuum induction melted and chill cast (in Cu-mould) composites (the chill cast composites
had low, <0.5%, fiber volume fraction and were fabricated by laying sapphire fibers in a Cu-mould
with fiber ends rigidly supported within holes drilled in steel end caps). The DS was done under
3 psi (gauge) pressure of ultrahigh purity argon gas in a 25 kW radio frequency (RF, 400 kHz)
vacuum induction furnace using a water-cooled copper current concentrator; a current adjusting
type three-mode proportional controller was used to set the temperature and control the power
input to the coil; DS was carried out by traversing a 8 mm long molten zone along the length of the
feedstock at a constant speed (~6.0 cm per hour).
Properties: substantially lower density, increased rigidity and strength at room-temperature and
elevated temperatures, significantly lower thermal expansion (especially in the direction of fiber
orientation), increased hardness, decreased ductility, and improved wear resistance are expected.
With W and Cr alloying of NiAl and incorporation of sapphire in the composite, dual-phase toughening
potential together with high-temperature strength is expected in the composite.
Structural characteristics: in the powder-cloth (PC) composite (Fig. VI.5.1), polycrystalline NiAl
matrix exhibits some residual porosity due to incomplete densification during hot pressing to fabricate
the composites. There is, however, no evidence of interfacial reaction. In the sapphire-reinforced
NiAl(Yb)-matrix composites made using the powder-cloth process (Fig. VI.5.2), besides matrix porosity
(marked by arrows in the figure), a considerable amount of interfacial reaction occurred between the
sapphire fiber and the ytterbium, which is a strong oxide former, and Yb2O3 is more stable than Al2O3
(the free energies of formation of Yb2O3 and Al2O3 at the DS are ~1727.5 kJ.mol-1 and
~1583.1 kJ.mol-1, respectively). The principal reaction products, independently identified using EDS
and x-ray diffraction, consist of Yb2O3 and Yb3Al5O12. The grain boundaries in the NiAl(Yb) matrix are
enriched in Ni3Al phase (arrows in Fig. VI.5.2 b). The directional solidification (DS) of the powder-cloth
sapphire-reinforced NiAl(Yb) composite feedstock led to an even more extensive fiber-matrix
interfacial reaction and formation of a thicker reaction zone as compared to the powder-cloth
composite (Fig. VI.5.3). This together with the presence of porosity and shrinkage cracks in DS
composites decreased the interfacial shear strength.
Fig. VI.5.4 shows the SEM images of the surface of fibers extracted from the PC and DS composite.
The fiber surface shows extensive chemical attack of the sapphire by the ytterbium in the NiAl(Yb)
matrix. The fibers were extracted from the composite by dissolving the matrix in a boiling solution of
75% acetic acid, 23% nitric acid, and 2% HCl acid. There was some loss of Yb from the matrix in the
fiber/matrix interface reactions; as a result, the Yb content (in at. %) decreased from 0.36 in the PC
composite to 0.19 in the DS composite.
The appearance of the sapphire fibers distributed in the matrix is shown for the various composites in
Fig. VI.5.5. The hot pressing step in the powder-cloth process leads to appreciable fiber breakage
during composite fabrication. This fiber damage is further accentuated when the PC composite is used
as a feedstock for floating-zone directional solidification (DS); this is because of the additional damage
caused due to the vigorous melt recirculation within the melt zone under a strong electromagnetic
141
field. In contrast, the composite made by vacuum induction melting and chill casting in copper mould
do not show any appreciable fiber breakage.
a
Fig. VI.5.1.
(a) Matrix region around a debonded sapphire fiber in a powder-cloth (PC) sapphire/NiAl composite showing
porosity due to incomplete densification during composite fabrication, and (b) shows wear tracks on NiAl grains
that formed due to sliding of debonded fibers during fiber push-out test. The matrix contains approximately
TM
equi-atomic fractions of Ni and Al. Reinforcement: single crystal sapphire fibers (Saphikon ), average fiber
diameter: 178 m
200 m
10 m
Fig. VI.5.2.
Structure of NiAl(Y)/saphire fibers composite produced by the powder-cloth (PC) technique. Arrows in (a)
denote the porosity in the matrix due to incomplete densification during hot pressing, and arrows in (b) denote
the Ni3Al phase that formed at matrix grain boundaries in the NiAl(Yb) matrix. A reaction layer at the fiber/matrix
interface in (b) is also visible. Non-etched sample
Fig. VI.5.3.
Low (a) and high (b) magnification views of a sapphire-reinforced NiAl(Yb) matrix composite after floating-zone
directional solidification. The DS was done on Powder-Cloth (PC) feedstock specimen. Extensive fiber/matrix
interfacial reaction and formation of shrinkage cracks is observed. Reinforcement: single crystal sapphire fiber
TM
(Saphikon ), fiber diameter: 178 m
142
a
Fig. VI.5.4.
SEM images of the surface of fibers extracted from the PC composite (a) and the DS composite (b). The fiber
surface shows extensive chemical attack of the sapphire by the ytterbium in the NiAl(Yb) matrix. The fibers were
extracted from the composite by dissolving the matrix in a boiling solution of 75% acetic acid, 23% nitric acid,
TM
and 2% HCl acid. Reinforcement: single crystal sapphire fibers (Saphikon ), average fiber diameter: 178 m.
The composition of the powder-cloth (PC) feedstock (in at. %) is 62.1Ni-36.8Al-0.36Yb. There was some loss of
Yb in the fiber/matrix interface reactions; as a result, there was less Yb in the DS material. The composition of
the DS composites (in at. %) is 62.5Ni-36.4Al-0.19Yb
e
Fig. VI.5.5.
Structure of various NiAl/sapphire fibers composites: (a) powder-cloth (PC) composite showing fiber breakage
during composite fabrication by hot pressing, (b) directionally solidified (DS) composite made from a PC
feedstock, (c) composite made by vacuum induction melting and chill casting in copper mould, (d) DS composite
showing fiber fragmentation due to matrix recirculation in the molten zone, and (d) fibers in a sapphire-NiAl(Yb)
composite
143
Acknowledgments
In the course of the preparation of this atlas, the results of experimental research were used, which in
turn were obtained during the following research projects:
1. Infiltration processing of silicon carbide platelet-reinforced aluminum alloy composites. Doctoral
Dissertation by R. Asthana, 1991, University of Wisconsin-Milwaukee, USA (Adviser:
P.K. Rohatgi)
2. Complex investigation of the interfacial phenomena of the liquid metals in contact with solid
bodies, Project No. MP/NIST 92-90, conducted in 1992-1996 by the Foundry Research Institute
and University of Wisconsin - Milwaukee, USA, and financed by Polish-American M. SklodowskaCurie Fond (Principal Investigators: N. Sobczak, P.K. Rohatgi)
3. Physical and chemical mutual interaction on the solid body liquid metal contact border, as a
factor shaping the structure and properties of heterogenic materials of aluminum alloys matrix.
Research project No. 773729203, conducted in 1992-1995 by the Foundry Research Institute and
financed by the Committee for Scientific Research, Poland (Project Manager: N. Sobczak)
4. Working out comprehensive technology to manufacture new generation castings reinforced with
ceramic or composite insertions using squeeze casting technology. Research project No.
7S20201804, conducted in 1993-1996 by the Foundry Research Institute, financed by the
Committee for Scientific Research, Poland (Principal Investigator: J. Sobczak)
5. Zone directional solidification of sapphire-reinforced NiAl-matrix composites, U.S. National
Academy of Sciences (through National Research Council), 1994-95, USA (Principal Investigator:
R. Asthana)
6. Effect of external pressure during solidification on the production of metal matrix composites and
use of such products in automotive industry, Project No. MP/NIST-95-231, conducted in 19951998 by the Foundry Research Institute and University of Wisconsin - Milwaukee, USA, financed
by Polish-American M. Sklodowska-Curie Fond (Principal Investigators: J. Sobczak, P.K. Rohatgi)
7. Settling behaviour of ceramic reinforcements in composite slurries, Faculty Research Initiative
Grant, University of Wisconsin-Stout, 1996, USA (Principal Investigator: R. Asthana)
8. Graded products with local composite reinforcement manufactured using centrifugal casting.
Research project No. 7T08B02211, conducted in 1997-1999 by the Foundry Research Institute
and financed by the Committee for Scientific Research, Poland (Principal Investigator:
J. Sobczak)
9. New generation of pistons for combustion engines as a result of optimising their properties by
formation of composite material structure. Ph.D. project No. 9T12C0131, conducted in 2000-2001
by the Motor Transport Institute and financed by the Committee for Scientific Research, Poland
(Principal Investigator: J. Sobczak, Ph.D. student: D. Rudnik)
10. Metallographic quantitative criteria of the selected service properties of composite materials made
brake discs. Ph.D. project No. 7T08B02718, conducted in 2000-2001 by the Motor Transport
Institute and financed by the Committee for Scientific Research, Poland (Principal Investigator:
J. Sobczak, Ph.D. student: A. Wojciechowski)
11. Working out the foundation of gasars technology new highly porous materials with
predetermined spatial lay out of porosity. Research project No. 7T08B01419, conducted in
2000-2003 by the Foundry Research Institute in cooperation with the Motor Transport Institute
J. Sobczak)
12. Physicochemical aspects of in-situ synthesis of Al-Al2O3 composites by liquid-phase processing.
Research project No. 7T08B00320, conducted in 2001-2004 by the Foundry Research Institute
N. Sobczak)
13. Starting up production of brake discs made of composite materials for the automotive industry
needs: Working out comprehensive technology of manufacturing brake discs out of Al/SiC
composites. Target project No. 10T120132000C/5220 conducted in 2001-2004 by the Motor
Transport Institute with the participation of the Foundry Research Institute, commissioned by the
Institute of Implementations and Polish Foundries Technologies Ltd. Project co-financed by the
Committee for Scientific Research, Poland
144
14. Optimisation of car component properties by formation of the new composite material structure.
Research project No. 9T12C01218 conducted in 1999-2002 by the Motor Transport Institute and
financed by the Committee for Scientific Research, Poland (Principal Investigator: K. Pietrzak)
15. Development of the synthesis of the light and economically justified construction materials
utilising waste products (fly ashes). Research project No. 3T08B06426, conducted in 2004-2007
by the Foundry Research Institute in co-operation with the Motor Transport Institute and financed
by the Ministry of Science and Information Technology, Poland (Principal Investigator:
J. Sobczak)
16. Effect of technological parameters on structure and properties of fly ash reinforced aluminum
matrix composites. Ph.D. project No. 3T08B05728, conducted in 2005-2007 by the Foundry
Research Institute and the Motor Transport Institute, and financed by the Committee for Scientific
Research, Poland (Principal Investigator: J. Sobczak, Ph.D. student: P. Darlak)
17. Innovative materials and processes for use in foundry industry. Commissioned research project
No. PBZ-KBN-114/TO8/2004, conducted in 2004-2008 by the Foundry Research Institute in cooperation with the Motor Transport Institute, and financed by the Ministry of Science and
Information Technology, Poland (Principal Investigator: J. Sobczak)
ISBN 978-83-60965-00-9

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2007 Atlas of Cast Metal-Matrix Composites Structures

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Jerzy Sobczak

Motor Transport Institute - Warsaw

Foundry Research Institute - Cracow

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From the Authors

I. Particulate dispersion-reinforced composites

II. Short fiber-reinforced composites

III. Long fiber-reinforced composites

IV. Gas reinforced composites (gasars)

VI. Typical structural defects in metal-matrix composites

The ATLAS displays microstructures of metal-matrix composite materials based on

July 30, 2007

Mrityunjay Singh, Ph.D.

From the Authors

Following successful practical applications in the aerospace and aviation

materials structures in connection with initial attributes of their creation as well as

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Aluminum composites containing fly ash (ALFA composites)

52K/x fly ash composite (x = 5, 10 and 15 vol. %)

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

AK12/60 vol. % fly ash composite

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

A356/5.0 wt. % fly ash composite

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Aluminum composites containing graphite

Al/GrNi composite (5 vol. % nickel-coated graphite)

Particulate dispersion-reinforced composites

AK11/xGrNi composite (x = 2.5, 5.0 vol. % nickel-coated graphite)

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

AK20/5.7 vol. % nickel-coated graphite composite

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

A356/5.7 vol. % nickel-coated graphite composite

Structure of A356/5.7 vol. % Ni-coated

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites

Particulate dispersion-reinforced composites