Thm Sohd Fdms, 96 (1982) 93-101

93

METALLURGICAL AND PROTECTIVE COATINGS

ABRASIVE W E A R O F I O N - P L A T E D T I T A N I U M N I T R I D E C O A T I N G S
O N P L A S M A - N I T R I D E D STEEL S U R F A C E S *
E. H. SIRVIO AND M. SULONEN
Laboratory of Metal Formmg and Heat Treatment, Helsmkt Umverstty of Technology, Vuorzmlehentte
2 A, 02120 Espoo 12 (Finland)

H. SUNDQUIST
Metals Laboratory, Technical Research Centre of Fmland, Revontulentle 7, 02100 Espoo 10 (Fmland)
(Received March 9, 1982, accepted Aprd 5, 1982)

The abrasive wear of ion-plated titanium nitnde coatings on hardened tool

steel and on hardened and plasma-nitrided tool steel was studied. Wear tests were
made with a dry s a n d - r u b b e r wheel set-up, and the initial surface roughness of the
specimen was one of the test parameters.
A wear mechanism for hard coatings on softer substrates under abrasive wear
conditions was suggested. The wear initiates on the tops of the asperities where the
base material is exposed first. Wear proceeds with the formatmn of craters at these
sites and the growth of these craters by fractures on the ridges formed by the coating
material.
The wear rate of coated steel increases with increasing initial surface roughness.
A considerable increase takes place when the scale of the surface roughness is of the
same order of magnitude as the coating thickness. This increase can be shifted to a
higher surface roughness if a subsurface hardening process, in this case plasma
mtrlding, is used.

1. INTRODUCTION
H a r d titanium nitride coatings have recently been used successfully as wearresistant coatings for metal cuttmg and forming tools. The development of plasmaenhanced deposition processes has made It possible to deposit titanium nitride onto
tool steels using low deposition temperatures 1'2. In metal cutting m a n y work
materials contain particles of phases which have a much higher hardness than that of
the workplece as a whole. M a n y of these secondary particles are harder than the
matrix m high speed tools and retain their hardness to higher temperatures. Such
matermls in the work material may cause abrasion, especially on steel tools, under
conditions of seizure as well as under sliding conditions, and m most published
papers on cutting tool wear the majority of flank wear, in particular, is attributed to
abrasion 3.

* Paper presented at the Internatmnal Conference on Metallurgical Coatings and Process Technology,
San Diego, CA, U S A,, Aprd 5-8, 1982
0040-6090/82/0000-0000/$02.75

O ElsevierSequola/Pnnted In The Netherlands

94

E, H SIRVIO, M SULONEN, H. SUNDQUIST

TltanIum-nltrlde-coated high speed steel twist drills have shown improved

wear resistance especially when hard abrasive steel is used as a workpiece 4' 5. Also,
when ductile iron containing a large amount of hard particles and a highly workhardened matrix is machined, titanium nltrlde coatings have prolonged the life of
high speed steel wedge cutters, spur cutters, hobs and thread cutters 6.
Because of the abrasive wear resistance of titanium nitride it has also been used
as a hard coating for watch cases In this apphcatlon a very thin coating is used
which requires a hardened subsurface, e.g. a hard chromium-plated base material ~.
2

ABRASIVE WEAR OF THIN HARD COATINGS

Abrasion is a wear process in which detachment of wear particles from the

surface may occur by ploughing, microchipping or fracturing 7. During ploughing a
high hydrostatic stress component is imposed on the wear surface in front of an
abrasive particle enabling plastic deformation even in typically brittle materials.
Plastic deformation also extends into the subsurface because of the cumulative effect
of strain hardening and wear. In a surface coated with a thin hard layer subsurface
plastic deformation may readily take place and brittle fracture of the coating may
occur.
When hard thin coatings are considered as protection against abrasive wear,
the initial surface roughness of the specimen is important. In two-body as well as in
three-body abrasion the wear begins at the tips of the asperities where the load is
high The running-in of the surface proceeds at a high rate until an equilibrium state
is reached, and the surface roughness becomes typical for the abrasion parameters
used, i.e. load, size and shape of the abrasive particles, materials involved etc. The
wear rate is then lower than that initially and remains constant.
If the dimensions of the initial surface roughness are of the same order of
magnitude as the coating thickness, the coating wears offat the tips of the asperities
revealing the base material. The wear rate of the softer base material IS higher, and a
crater surrounded by sharp edges of the coating material is formed. Consequently
these ridges form sharp new tips with a high load concentration and are abraded or
fractured off; thus, the size of the wear crater continues to grow quickly.
If the initial surface roughness is considerably less than the coating thickness,
the wear of the tips does not reveal the base material during the running-in period.
Consequently, the wear rate of the surface will be characteristic of the coating
material used, and for hard coatings this will be marginal compared with the wear
rate of the base material.
During ploughing abrasion, the plastic deformation of the base material may
cause cracks in the coating and crater-type wear may take place. A third possibility
for this rapid wear is the existence of imperfections in the thin hard coating or poor
adhesion of the coating to the substrate.
Hardening treatments penetrating to greater depths than the coating may be
used as a pretreatment before coating to prevent plastic deformation of the
subsurface. Plasma nltrlding is suggested as a suitable pretreatment as it can be done
m the same equipment as the deposition
In this work an investigation on the abrasive wear of titanium mtrlde coatmgs
on tool steel specimens was made using a dry sand-rubber wheel test 8. The mm was

ABRASIVE WEAR OF ION-PLATED

Ti

NITRIDE COATINGS

95

to study the effect of the initial surface roughness on the abrasive wear of thin
coatings. Also a series of spectmens were prepared to study the effect of subsurface
hardening, by using plasma nitridlng as a pretreatment.
The reported hardnesses of the quartz sand used in the sand-wheel tests varies
between 800 and 1200 HV, and the hardness of ion-plated titanium nitride coatings
between 2000 and 3000 HV. Hence the ratio of the hardness of the wear surface to
that of the abrasive varies from 1.7 to 3.5, and a very low wear rate is to be expected
as long as the base material is not exposed.

3.

EXPERIMENTAL PROCEDURE

3.1 Preparation of the coatmgs

A reactive ion plating process with a discharge supported by a negative filament
was used to produce titanium nitride coatings 1. Titanium was evaporated with an
electron beam gun at an evaporation rate of 0.8 g min ~. The chamber pressure
during coatmg was maintained at 5 mTorr. The atmosphere consisted of argon and
nitrogen gases. The cathode voltage was biased a few hundred volts negative, and
the ion current was 250 mA. The total area of the specimens coated was 120 cm 2,
gtving an average current density of about 2 mA cm 2. The temperature of the
specimen during the coating was continuously monitored and remained below
280 C. Figure 1 shows a scannmg electron micrograph of the resultant coating on
an edge of a fractured specimen. Plasma nltriding was made in the same chamber
using the low pressure plasma nltrlding prQcess 9. The pressure used was 40 mTorr,
the atmosphere consisting of nitrogen and hydrogen gases. The specimens were
biased 4 kV negative, giving a current of 90 mA and thus a current density of
0.75 m A c m 2. Under these conditions the temperature of the specimens was
maintamed at 450 C, and the nltridlng process was conducted for 4 h. The resulting
diffusion zone was about 50 ~tm thick, as can be seen in Fig. 2 which is an optical
micrograph of the surface.

F~g 1 Scanning electron mJcrograph of an Ion-plated t~tanlum intrude coating on hardened tool steel
(speclrnen 1 3)

96

E . H . SIRVIO, M. SULONEN, H. SUNDQUIST

Fig. 2 Optical mlcrograph of a plasma-nltrlded and tltanlum-nltrlde-coated tool steel surface (Nltal
etched, specimen 3 5)

The test specimens were made of AISI D3 tool steel in a hardened and tempered
(450 C) condition. Three different surface roughnesses were machined for each
case. The R a values of the surface roughnesses used varied from 0.06 to 11.6 gm The
properties of the specimens and the wear test results are given in Table I.
3.2. Wear tests

Figure 3 is a schematic Illustration of the test equipment used The abrasive

(quartz sand) is introduced between the test specimen and a rotating wheel which
has a chlorobutyl rubber rim with a hardness of Durometer A-60. The test specimen
as pressed against the rotating wheel with a force of 130 N while a flow of sand (about
TABLE I
PROPERTIES OF T H E TEST SPECIMENS A N D W E A R TEST RESULTS

Specimen
number

Treatment

Bulk
hardness
(HRC 150)

Surface
roughness
Ra (~tm)

Wear
(mg)

Relative
wear

11
12
13
21
22
23
31
32
33
34
35
36

Coated

54
57
58
53
55
54
57
57
56
54
58
58

95
11
0 06
95
!.3
0 06
11 6
35
14
14
007
0 07

31
8
6
121
97
107
62
37
34
32
24
31

0 23
0 06
0 04
0 90
0 72
0 79
0 46
0 27
0 25
0 24
0 18
0 23

Reference
samples

Uncoated

135

Plasma
nltnded
Coated and
nltrlded

56 58

0 1-12

ABRASIVE WEAR OF ION-PLATED Ti NITRIDE COATINGS

97

HOPPER
QUA R]Z SAND

WEIONTS
RUBBER LINED WHEEL

Fig 3 Schematic view of the set-up used for the dry sand-rubber wheel wear test
300 g m m - 1) a b r a d e s the test surface. The specimens were weighed before a n d after
the test, a n d the loss m mass was recorded.
T h e tests were m a d e a c c o r d i n g to an A S T M s t a n d a r d 8 with s o m e modific a t i o n s The d~fferences from s t a n d a r d p r o c e d u r e s were as follows (the values of the
c o r r e s p o n d i n g s t a n d a r d test p a r a m e t e r s are in brackets). The d i a m e t e r of the r u b b e r
wheel was 185 m m (228.6 ram) a n d the n u m b e r of r e v o l u t i o n s used in each test was
420 (100). This gives a sliding distance of 244 m (71 8 m).
T h e force on the specimen was the same as that specified in the s t a n d a r d , i.e.
130 N. T h e size of the q u a r t z s a n d particles used varied, m a i n l y (80%) between sieve
sizes 50 a n d 150 c o r r e s p o n d i n g to d i a m e t e r s from 300 to 100 I~m
4 RESULTS

4.1. Wear o f titamum mtrlde coatings

F i g u r e 4 shows a p h o t o g r a p h of the tested specimens. The p h o t o g r a p h was
t a k e n with an mclined hght source a n d the wear t r a c k is clearly seen. The bright
areas in the wear t r a c k are the areas where the c o a t m g has been w o r n through. As

la)

(b)

~c)

Fig 4 W e a r tracks on the tested htanium-mtrlde-coated specimens (a) 1 1, (b) 1 2 and (c) 1 3

98

E H SIRVIO, M. SULONEN, H, SUNDQUIST

Fig 5 Scanning electron mlcrograph of the wear surface of specimen 11 Coating Is still present at the
sites of the valleys of the m~nal surface

can be seen, coating 1.3 has hardly been worn through, and coating 1.2 has worn
through on the tops of the highest aspentles. Coating 1.1 has been worn through on
the tops of the asperities in a large area of the wear track. In spite of th~s all the valleys
of the m~tlal surface retain the coating, as can also be seen m Fig. 5 which is of the
same surface.
The new surface profile obtained as a result of abrasive wear is a mirror ~mage of
the original, as the initial valleys have changed to hps of new asperities with hard
coating on the top. On the s~te of an ininal t~p there ~s now a valley.
The wear of the test specimens and their relanve wear compared with that of
untreated specimens is presented in Table I. The wear of coated samples was
between 4% and 23% of that of the untreated specimens
The total wear increased considerably when the surface roughness R, was
increased from 1 to 10 lam. This is expected according to the wear mechanism of
hard coatings proposed earher When the surface roughness ~s 10 gin, the thickness
of the coating (6 gm) is exceeded and the wear rate is h~gh where the base material is
revealed. In this specimen most of the wear (31 rag) is wear of tool steel beneath the
initial asperities When the surface roughness is less than the film thickness, wear ~s
more moderate, and it seems that even with these low roughnesses a coating on a
smoother surface gives better wear protection.

4.2 Wear of plasma-mtrlded surfaces

The surface hardness of plasma-nitnded hardened tool steel surface is about
1000 HV, i.e. about the same as that of the abrasive sand. Thus the treatment does
not give full protection against abrasive wear. Nevertheless, the increase in hardness
lowers the wear rate at the beginning of the test, as the wear of metals is inversely
proportional to their hardness. This had only a slight effect on the wear results in this
study, as the thickness of the diffusion layer was only 50 ;am and was penetrated
during the test. The wear of all the plasma-nltrided specimens was between 70% and
90% of that of the untreated specimens, and the wear scar was smooth without any
differences due to the initial surface roughness

ABRASIVE WEAR OF ION-PLATED

Tt

NITRIDE COATINGS

99

4.3

Wear of titanium nitrtde coattngs on plasma-mtrtded steel

Table I shows that in this study the wear of steel specimens coated with
titanium nitride and plasma nitrlded was higher than that of specimens only coated
with titanium nitnde. This behaviour was found to be due to the differences in the
structures of the coatings on hardened and on plasma-nitrided steel. Figure 6 shows
scanning electron micrographs of Vickers indentations made on coatings for the
two cases. It can be seen that the coating on the plasma-nitrided surface has a larger
grain size than the coatmg on the untreated surface. It is also more brittle as it is
cracking at the edges of the Vickers indentation. The larger grain size can be
explamed as due to the higher temperature (450 C) at the beginning of the coating
process originating from the preliminary plasma nitrtding process.

(a)

(b)

Fag 6 Scanning electron mlcrographs of Vlckers lndentataons m the surface of specimens (a) 1 3 and
(b) 3 5

~ x l - - " "

05

LU

~00S
Q::

001

01

_ _ _ _ ~ L ~

05
1
5
SURFACE ROUGHNESS, Ra, lam

10

Fag 7 Relattve wear of the tested specimens as a function of the initial surface roughness x, plasma
mtrlded, C), tltamum mtrlde coated, 0, both treatments The wear is compared with that of untreated
AISI D3 steel m a hardened condmon

100

E.H. SIRVIO, M SULONEN, H SUNDQUIST

When all the results of this study are plotted in a graph (Fig 7) it can be seen
that the increase in wear of the tltanlum-nltrlde-coated samples takes place at lower
surface roughnesses than when the base material has been plasma nltrlded.
Consequently, it is suggested that, if the specimens were cooled after the plasma
nltndlng process and before coating, the wear resistance of the coating could be
further improved, particularly if the surface roughness were of the same order of
magnitude as the coating thickness.
5

CONCLUDING REMARKS

The abrasive wear of hard thin coatings is clearly dependent on the Initial
surface roughness if the coating is substantially harder than the abrasive grit The
wear of titanium nltrlde coatings on surfaces with a roughness of the same order of
magnitude as the coating thickness can be improved by subsurface hardening of the
base material, if the coating structure and adhesion are the same
Abrasive wear of hard coatings on softer substrates takes place according to the
suggested wear mechanism. Wear starts with the formation of a crater of exposed
base material. The growth in the area of the crater proceeds by fractures of the
coating at the ridges, and the growth in its depth by conventional abrasive wear
This is seen m Fig. 8, where a scratch by an abrasive particle extends to the ridge of
the crater causing fractures at impact However, no wear groove has formed on the
coating under the track of this abraswe particle beyond the crater edge, and no
ploughing or mlcrocuttlng abraswe wear has taken place

Fig 8 Track of abrading asperity on exposed base material The particle has impinged on the edge of the
wear crater, ~e the coating, causmg fractures and deformalton

ACKNOWLEDGMENTS

The authors wish to acknowledge the contnbuUon of D. G Teer and

A Matthews, who developed the ion plating process used here. Thank are also due
to A Korhonen for invaluable discussions

ABRASIVE WEAR OF ION-PLATED

Ti

NITRIDE COATINGS

101

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M a t t h e w s a n d D G Teer, ThmSohdFtlms, 72(1980) 541-549
K Sun, R R Nlrnmagaddaand R F Bunshah, ThznSohdFtlms, 64(1979)191-203
M Trent, Treatise Mater Sct Technol, 13 (1979) 443-489
Buhl, H K P u l k e r a n d E Moll, ThmSohdFdm~,80(1981)265-270
R Nlmmagadda, H J Doerrand R R Bunshah, Thm SohdFtlms, 84 (1981) 303-306
Sundqmst, E H. Slrvlo and M Kurkmen, Proc Conf on lon-asststed Surface Treatments-

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Techmques and Apphcattons, Warwtck, September 1982

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