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Evaluation of wear resistance of thin hard

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 Wear 251 (2001) 861–867

Evaluation of wear resistance of thin hard coatings by a

new solid particle impact test
Y. Iwai a,∗ , T. Honda a , H. Yamada a , T. Matsubara b , M. Larsson c , S. Hogmark d
a Department of Mechanical Engineering, Fukui University, 3-9-1 Bunkyo, Fukui 910-8507, Japan
b Macoho Co. Ltd., Ishido-cho, Nagaoka 940-2032, Niigata, Japan
c Balzers Sandvik Coating AB, Box 42056, SE-126 12 Stockholm, Sweden
d The Angstrom Laboratory, Uppsala University, SE-751 21 Uppsala, Sweden

Abstract
For the evaluation of tribological properties of thin hard coatings, several experimental techniques are normally used, such as scratch
testing and testing against abrasive, erosive, and sliding wear, and fretting. In this paper, we propose slurry jet, a new type of solid particle
impact test, in order to quickly evaluate wear properties of thin, single layered or multilayered physical vapor deposited (PVD) coatings. By
slurry jet 1 ␮m alumina particles were impacted at high velocity perpendicular to thin PVD coatings of TiN, TiN/NbN, TiN/TaN, TiN/CrN,
TiN/TiAlN deposited on a high speed steel (HSS) substrate material.
The coatings proved to have much higher erosion resistance than the substrate material and, consequently, the wear rate increased
significantly to the higher level of the HSS material when the coatings were penetrated. The maximum peak-to-valley roughness (Ry ) of
the eroded coatings was of the order of 0.1–0.5 ␮m, suggesting that the size of the detached particles was of the same order. The ranking
of erosion resistance and correlation to the mechanical properties, such as hardness and critical normal load obtained by scratch testing are
discussed.
We conclude that the proposed evaluation test is fast and easy to accomplish. It generates reproducible results and is very sensitive to the
quality of the coating. Thus, it can preferentially be used as a screening test when evaluating coatings and coated materials. In particular,
the interface strength of multilayered coatings with very thin lamella can be assessed.
For the coatings included in this study, the TiN/TiAlN proved to have the highest erosion resistance, whereas the TiN/CrN was the worst.
© 2001 Elsevier Science B.V. All rights reserved.
Keywords: Slurry jet impact test; PVD coating; Evaluation; Wear resistance

1. Introduction Tests aimed at the intrinsic coating properties or at distin-

Today, homogeneous and multilayered coatings are in-
creasingly being used to improve the tribological properties
of a wide variety of mechanical components such as tools
for metal cutting and forming, and machine elements such
as rolling or sliding bearings, seals, piston/cylinder systems,
and valves [1,2].
As to the evaluation of tribological properties of thin hard
coatings, several experimental techniques are being used,
such as scratch testing; abrasive and erosive testing, sliding
and fretting wear testing. A continuing development of ver-
satile and reliable techniques for evaluation of coated com-
ponents is important for the development and tribological
assessment of new coating composites and their applications.
∗ Corresponding author. Tel.: +81-776-27-8544; fax: +81-776-27-8748.
E-mail address: iwai@mech.fukui-u.ac.jp (Y. Iwai).
guishing between the properties of the coating and substrate
material, respectively, should allow the wear rate of the coat-
ing to be determined independently of that of the substrate.
Hutchings [3] has reviewed the application of solid parti-
cle erosion testing to coated samples. Erosion testing has
proven to be a suitable tool for studies of crack initiation and
propagation in thin hard coatings [4]. Conventional particle
erosion tests such as gas-blast [5], centrifugal [6] and slurry
erosion tests [7,8] have been used to study the erosion dura-
bility of coatings when impacted by relatively large solid
particles of a diameter many times larger than the coating
thickness. However, failure of thin hard coatings often oc-
curs unevenly [6] and after a short test duration [7] due to
this high ratio of particle diameter to coating thickness. It is
also difficult with these techniques to focus the impingement
of tiny solid particles on a small area of the target. If parti-
cle erosion is to be used as a means to test intrinsic coating
properties, a test method which involves the impact of very

0043-1648/01/$ – see front matter © 2001 Elsevier Science B.V. All rights reserved.
PII: S 0 0 4 3 - 1 6 4 8 ( 0 1 ) 0 0 7 4 3 - 8
862 Y. Iwai et al. / Wear 251 (2001) 861–867
small particles is needed to minimize the maximum depth
to which the coating material is affected at each individual
impact.
In this paper, we propose a new type of slurry jet, i.e.
a solid particle impact test which utilizes a focused slurry
jet, in order to quickly evaluate wear properties of single
layered and multilayered physical vapor deposited (PVD)
coatings. The PVD coatings included in this study are TiN,
TiN/NbN, TiN/TaN, TiN/CrN, TiN/TiAlN deposited on flat
(20 mm ×40 mm ×2 mm) high speed steel (HSS) substrates.
The ranking of erosion resistance and its correlation to the
mechanical properties such as hardness and critical normal
load obtained by scratch testing are discussed. From these
results, we conclude that the proposed test can preferentially
be used as a screening test when evaluating coated materials.
2. Experimental
2.1. Test apparatus and procedure
Fig. 1 shows a schematic view of the test apparatus, which
was developed by Matsubara at Macoho Co. Ltd. It consists
of a specimen holder, a tank and a stirrer to mix solid par-
ticles in liquid, a nozzle to eject the test liquid, a regulator
to adjust compressed air pressure and a solenoid valve con-
nected with a timer to control on–off of liquid flow. The
flowing stream of water containing solid particles sucked
from the tank, is mixed with compressed air in the noz-
zle, and eventually a slurry jet is ejected at high velocity
in atmosphere. The cross-section of the nozzle is square by
3 mm × 3 mm, which generates a rectangular scar on a flat
specimen. The shape of a square was chosen because it has
Fig. 1. Schematic view of the slurry jet tester. The insert shows detail of
the nozzle.
the advantage over circle in the easy measurement of the
central region of the scar. The jet velocity is regulated by
the pressure of the compressed air, but could, unfortunately,
not be measured. For the pressure of 0.5 MPa used in this
experiment, the maximum velocity was estimated to over
100 m/s at the exit of the nozzle by the double-disc method
[9]. However, the error of this method may be severe for
small particles and particles of low density. The impinge-
ment angle of the jet relative to the test surface can be var-
ied from 15 to 90◦ by tilting the specimen holder. In this
test 90◦ impact was used. The test piece was mounted at
10 mm distance from the end of the nozzle. The test liquid
was tap water containing angular alumina particles with a
size distribution in the range of 0.5–2.5 ␮m, with an average
diameter of 1.0 ␮m, as erodent. The alumina particles have
a hardness ranged from 1800 to 2000 HV [10]. The erodent
was added into tap water of the volume of 2 l in 3 wt.%, i.e.
the concentration of the alumina particles was 3 wt.% in the
tank, and the slurry was kept at room temperature.
The wear loss of the coatings after the tests was too small
to be resolved by weighing. Instead, the geometry of the
eroded surface was measured with a stylus profilometer at
three positions along the center-line of the square scar. In
addition, the worn surfaces were studied by SEM and AFM
to reveal the wear mechanisms.
2.2. Test materials
2.2.1. Substrate material
As substrate material, a powder metallurgical (PM) HSS
with the chemical composition (wt.%) of 1.3C, 4.2Cr,
5.0Mo, 6.4W, 3.1V and 8.5Co, was used. It was heat treated
by austenitisation at 1180◦ C followed by tempering 3× 1 h
at 560◦ C, resulting in a primary carbides volume fraction
of 13% and a hardness of 9.2 GPa. All substrates were pol-
ished to mirror finish, corresponding to a center-line average
roughness (Ra ) value of approximately 5 nm. Uncoated HSS
was included in the erosion test as a reference material.
2.2.2. Coating materials
The coating materials and their properties are listed in Ta-
ble 1. The first four are experimental coatings, and the last
one is commercially available. The TiN coating is a mono-
layer, while the others have a multilayered structure, i.e. they
were obtained by alternately depositing two different com-
pounds.
The total thickness of the coatings was in the range of
2.5–4.4 ␮m, as estimated from fractured cross-sections in
the SEM. The individual layer thickness, see Table 1, was
estimated similarly.
All multilayered coatings with individual layers of
0.01/0.005 ␮m thickness were found to be harder than the
coarsely laminated TiN/TiAlN (21 GPa) and the homoge-
neous TiN (21 GPa), see Table 1. All the coatings show a
higher surface roughness than the uncoated substrate (Ra :
60–250 nm).
 Y. Iwai et al. / Wear 251 (2001) 861–867 863

Table 1
Coating materials and their propertiesa
Coating Deposition Coating Coating Individual layer Hardness HV0.050 Ra (nm) Critical normal
technique structure thickness (␮m) thickness (␮m) (GPa) load (N)
TiN REB Homogenous 2.8 ± 0.2 – 21 ±1 100 ± 30 50 ± 10
TiN/TaN REB/RMS Multilayered 3.2 ± 0.2 0.01/0.005 39 ±4 110 ± 50 53 ± 7
TiN/CrN REB/RMS Multilayered 3.7 ± 0.3 0.01/0.005 24 ±1 170 ± 80 36 ± 4
TiN/NbN REB/RMS Multilayered 2.8 ± 0.3 0.01/0.005 38 ±2 160 ± 40 40 ± 5
TiN/TiAlN RAE Multilayered 4.1 ± 0.3 0.1/0.1 21 ±1 220 ± 60 40 ± 20
a REB: reactive electron beam evaporation; RMS: reactive dc magnetron sputtering; RAE: reactive arc evaporation.

A crucial property of coated components is the adhesion
of the coating to the substrate. In the conventional scratch
test, a Rockwell diamond stylus (tip radius 200 ␮m) was
traversing the coating while the normal load was contin-
uously increased. All the coated samples were scratched
with a loading rate of 10 N/min and a scratching speed of
1 mm/min. Four scratches were performed for each coating.
The critical normal load (FN,C ), i.e. the load at the first
coating failure, was determined by monitoring a sharp in-
crease in the friction force and acoustic emission (AE),
respectively, during the scratch process. All the coatings dis-
played relatively high critical normal loads, and ultimately
failed by a mixture of adhesive and cohesive failures. The
critical load was found to decrease in order TiN/TaN, TiN,
TiN/NbN and TiN/TiAlN, TiN/CrN, see Table 1. At and
above the critical load, TiN/CrN and TiN displayed small
cohesive chippings at the rim of the scratch. In the case of
TiN/NbN and TiN/TaN, the critical load corresponded to
semicircular cohesive failures, which are typical for brittle
materials. For loads higher than the critical load, TiN/NbN
and TiN/TaN also displayed areas of exposed substrate.
3. Test results and discussion
Fig. 2 shows the depth profiles of the erosion crater of the
TiN coating, measured after various test duration. During the
first 21 min the wear of the coating was gradual and slow,
generating a smooth surface, where after the coating was
penetrated and severe damage of the substrate commenced.
At each test interval the distance between the original and
the worn surfaces at the deepest position was measured and
designated as the wear depth.
The TiN coating proved to have much higher erosion re-
sistance than the HSS material as can be seen from the wear
depth variation with test duration in Fig. 3. For the TiN coat-
ing the wear depth increased linearly at a moderate slope
until the coating is penetrated after about 21 min when it
increased significantly. The slope of the initial part of the
wear curve of the coating was calculated by means of the
least-squares method, and defined as the coating wear rate
in this study.
The presumptive time of coating penetration tp is esti-
mated as the time when the extrapolated initial wear curve
reaches a wear depth corresponding to the measured coating
thickness. On the other hand, the wear depth curve drawn
from high slope points means the wear curve of substrate
material beneath the coatings. The time at which both wear
curves of coating and substrate intersect is designated as the
experimental penetration time te of the coating, see the il-
lustration in Fig. 3. For TiN, the slope of the high wear rate
curve-section was almost identical to that of the uncoated
substrate. In addition, tp and te were found to be almost the
same (20.7 and 21.1 min, respectively).
In order to confirm the reproducibility of the wear rate of
the TiN coating, additional four 15 min tests were carried

Fig. 2. Surface profiles along the center-line of the square erosion scar Fig. 3. Maximum crater depth of the substrate (HSS) and the TiN coating
of the TiN coating after various test duration. as a function of test duration.
864 Y. Iwai et al. / Wear 251 (2001) 861–867

Fig. 7. Wear rates for all coatings.

Fig. 4. Reproducibility of the wear rate for the TiN coating.

Fig. 5. Wear depth vs. time for all coatings.

Fig. 6. Relation between the experimental time for coating penetration te Fig. 8. Representative SEM photographs of the worn surface of eroded
and the presumptive time for coating penetration tp . substrate material (HSS) (a), TiN (b) and TiN/CrN (c)
Y. Iwai et al. / Wear 251 (2001) 861–867 865
866 Y. Iwai et al. / Wear 251 (2001) 861–867

out, and the corresponding wear rates are plotted in Fig. 4.

The mean-value and standard deviation of the five tests were
0.136 and 0.0065 ␮m/min, respectively. Their relative error,
i.e. the value of S.D./mean-value, was 4.8%. Consequently,
our test was found to be highly reproducible.
There are strong deviations in wear rate among the in-
vestigated coatings, as seen in Fig. 5. However, the gen-
eral shape of the wear curves is the same. In addition, it
was seen that te completely agrees with tp for all coatings,
see Fig. 6, which means that our test is able to determine
the durability and wear rate of thin hard coatings indepen-
dently of the substrate. This is the great benefit of using our
equipment. Therefore, it is possible to compare the wear
resistance between various coatings accurately. The wear
rate was found to decrease in the order TiN/CrN, TiN/TaN,
TiN/NbN, TiN/TiAlN, TiN, see Fig. 7. Fig. 11. Wear rate vs. hardness for all coatings.

3.1. Observation of worn surfaces

Fig. 8 shows representative SEM photographs of the worn
surface of substrate (a), TiN (b) and TiN/CrN (c). A char-
acteristic pattern of protruding carbides is seen in the HSS
substrate indicating a very mild, selective wear mechanism,
primarily attacking the softer steel matrix. The coatings were
worn gradually, and eventually the substrate was exposed
and eroded to show the surface characteristics as the worn
surface of the substrate specimen, see Fig. 8b and c. For TiN,
a smooth surface was produced and the substrate slightly
appeared on the whole worn surface, whereas for TiN/CrN
a very smooth worn surface was produced compared to that
of TiN, but the initial exposure of the substrate was more
local. Cutting traces and cracks, which usually are charac-
teristic of surfaces exposed to solid particle erosion [11],
were neither observed for the substrate nor the coatings. It is
concluded that the material is removed in the form of very
small fragments due to repeated attacks from the very small
eroding particles.
The micro-topography of the worn surfaces was quantified
by AFM, see Fig. 9. The original surface of TiN had a regular
variation in roughness, produced during the coating process,
see Fig. 9a. The higher parts of the original surface were
preferentially worn down to form a uniform and smooth
surface, see Fig. 9b. All tested coatings showed a smooth
worn surface similar to that of TiN, cf. Fig. 9c–f.
The evolution of equilibrium maximum peak-to-valley
roughness (Ry ) of the worn surface of the coatings is
shown in Fig. 10. For all coatings, the roughness was
rapidly reduced at the beginning of the test and reached a
constant-value, of the order of 0.1–0.5 ␮m, after less than
5 min. The homogeneous TiN and the TiN/TiAlN multilay-
ered coating with 0.1 ␮m lamella thickness, showed a higher
Ry compared to the three multilayers with 0.01/0.005 ␮m
lamella (TiN/NbN, TiN/TaN and TiN/CrN). These results
suggest that the size of the detached debris is of the order
of 0.1–0.5 ␮m.
The wear rate of the coatings does not simply correlate
to the coating hardness, see Fig. 11. The homogeneous TiN
and the multilayered TiN/TiAlN with relatively thick lamella

Fig. 10. Equilibrium maximum peak-to-valley roughness (Ry ) for all

coatings. Fig. 12. Wear rate vs. critical normal load for all coatings.
 Y. Iwai et al. / Wear 251 (2001) 861–867
proved to give a lower wear rate than expected form of their
hardness-values.
Nordin et al. [12] demonstrated a higher resistance for
multilayered TiN/TaN coatings when eroded with SiC par-
ticles (20–30 ␮m in size) that they believe is a result of the
superior toughness gained from the large number of inter-
faces. Some proportion of the impact energy is consumed
by crack deflection and correspondingly less energy is used
in the creation of wear fragments, as compared to homo-
geneous coatings.
However, in the present investigation, homogeneous TiN
and the coating with thick lamella (TiN/TiAlN) showed a
higher wear resistance than the thin lamella multilayered
coatings.
The reason for these unexpected results is probably found
in the very small scale of the wear fragments. Any crack in-
volved in the formation of the wear fragments in this very
mild erosion is smaller, or of the same order of magni-
tude as the inter distance between the thin lamella. Thus,
on this small scale, the interfaces rather play the role of de-
fects than improving the toughness of the coatings through
crack deflection. On the other hand, with the more homo-
geneous coatings, there is a chance for cracks to grow to
larger depths through successive impacts, before any par-
ticle is removed. Consequently, these fragments are larger,
explaining the higher roughness of the corresponding wear
surfaces, but they also appear a lot scarcer.
There is no correlation between the erosion rate of the
coatings and the critical normal load in scratch testing, see
Fig. 12. The simple explanation is found in the very small
scale by which the erosion occurs. There is virtually no
influence from the substrate material.
4. Conclusions
By using slurry jet, a new type of solid particle impact test,
fast and highly reproducible evaluation of wear properties of
thin coatings can be made. The following conclusions can
be drawn from this investigation:
• Linear wear is obtained for both coating and substrate
material, and the penetration through the coating into the
substrate is signified by a sharp increase in slope of the
wear versus time curve.
• The test is fast and easy to accomplish, and the wear oc-
curs on such a small scale that the erosion resistance of
coating and substrate materials is assessed independently.
867
These advantages of using our equipment are a great ben-
efit compared to other erosion tests.
• It is believed that this test can preferentially be used to
evaluate the interlamella strength of multilayered coatings
with thin lamella.
• For the coatings included in this study, homogeneous
TiN and a multilayered coating with coarse lamellae
(TiN/TiAlN) proved to have a higher erosion resistance
than multilayers with thin lamellae (TiN/NbN, TiN/TaN,
TiN/CrN).
Acknowledgements
This study was supported by a Grant-in-Aid administered
by the Ministry of Education of Japan (no. 11650149), and
The Swedish Research Counsil for Engineering Sciences
(TFR). The authors are grateful to Mr. Tetsuo Suehiro for his
experimental help, and also to Mr. Ulrik Beste for operating
a scanning electron microscope.
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