A METHOD FOR TRIBOLOGICAL TESTING OF THIN

HARD COATINGS
R. MICHALCZEWSKI, W. PIEKOSZEWSKI, M. SZCZEREK and W. TUSZYNSKI
Institute for Terotechnology (ITeE), ul. Pulaskiego 6/10, 26-600 Radom, POLAND;
e-mail: waldemar.tuszynski@itee.radom.pl

SUMMARY
The authors have elaborated a new method for tribological testing of thin, hard antiwear coatings, using a ball-on-disc
tribosystem, under conditions of dry sliding. Al2O3 ball is pressed against the disc rotating in the horizontal plane. The
investigated coatings are deposited on steel discs. A novelty of the method is the removal of wear debris from the
contact zone through a draught of dry argon. This helps to reduce the scatter of results. All test conditions have been
precisely defined, particularly: the kind of motion, air relative humidity, ambient temperature, sliding speed, load,
substrate material, substrate hardness and roughness, and coating thickness. The authors used the method to investigate
various PVD coatings (deposited by the vacuum-arc method), i.e. single layer: TiN, Ti(C,N), CrN, Cr(C,N), and
multilayer: Cr(C,N)/CrN/Cr and Cr(C,N)/(CrN+Cr2N)/CrN/Cr. It has been shown that CrN coatings exhibit the best
antiwear properties. Friction coefficients for CrN and Cr(C,N) coatings are much smaller than for widely used TiN.
Multilayer coatings have better antiwear properties than single layer ones.

Keywords: Test method, ball-on-disc tribosystem, wear, friction, PVD coatings

1 INTRODUCTION reproducibility of test results, one must keep the same

Thin hard antiwear coatings deposited by the PVD
process (physical vapour deposition) are used mainly to
enhance life of friction pairs. Apart from ‘traditional’
areas of their successful application, i.e. for enhancing
of life of cutting tools, coatings are also applied in
various technical devices like transmissions, engines,
pumps and compressors [1]. In view of completely
different working conditions in such devices, a great
diversity of PVD coatings is in use; needless to say that
all the time new coatings appear in the market [2].
But by now there has been a lack of a uniform, widely
accepted method for investigation of tribological
properties of thin hard coatings. This brings about the
incomparability of results obtained at various
laboratories; e.g. for TiN - steel couples friction
coefficient values vary between 0,1 to 1,2 [3]. Also
measures of antiwear properties of PVD coatings
significantly differ from one another. For example, in
the work [4] the researchers report larger wear for CrN
than TiN coating. Completely different results are
presented in [5], [6] and [7], where CrN coating exhibits
better antiwear properties than TiN.
Due to the above described situation, tribological testing
of coatings deposited on cutting tools [8], under real
working conditions, may prove much more reliable than
laboratory testing. However, such an approach may be
unacceptably costly in case of a necessity for testing of
coatings deposited on e.g. casting moulds [9]. Thus, to
compare and assess thin hard coatings, it is highly
required to elaborate and disseminate a uniform method,
carried out under laboratory conditions.
The first step towards achieving of this goal was the
international research project VAMAS (Versailles
Advanced Materials and Standards) realised in three
stages by the G-7 countries. Experiments conducted in
the eighties on ceramics shown that to obtain good
test conditions, especially the relative humidity, which
has later been expressed in the ASTM G 99-90 and DIN
50324 standards [10], [11].
Poor reproducibility of test results obtained at various
laboratories comes from an influence of many factors on
measures of tribological properties. This matter - with
respect to PVD coatings - is considered in [4]. From that
work it is apparent that friction and wear characteristics
depend among others on the kind and preparation of the
substrate, coating deposition parameters, kind of motion
during tribological tests and test conditions.
As a result of an overview of the literature, the authors
gathered in four groups such factors as have the most
significant influence on the tribological results for thin
hard coatings.
Factors relating to the substrate:
substrate hardness [12], [13],
substrate roughness [14], [15], [16].
Coating thickness [17].
Kind of motion (sliding or rolling) [18].
Test conditions:
counterbody material [19],
action of wear debris [19], [20],
air relative humidity [21], [22],
ambient temperature [12], [16],
sliding speed [12], [21], [23], [24], [25],
load [25], [26],
friction pair vibrations (depending on the
stiffness and construction of the loading unit,
tribosystem spatial configuration, axial run-out
and sliding speed) [22], [27], [28].
The particular analysis of the results reported in the
literature suggests that all of the mentioned factors have
a significant effect on the friction coefficient and/or
wear. This practically means that only results obtained
under identical or close test conditions are comparable.
Thus, the coatings to be compared should have close
thickness, be deposited on the substrates of the
approximate hardness and roughness, be rubbed against
the same counterbody material, at identical motion (e.g.
sliding) and under close conditions (speed, load, relative
humidity, etc.).
Unfortunately, the existing standards like ASTM G 99-
90 or DIN 50324 [10], [11], concerning tests using a
pin-on-disc or ball-on-disc tribosystem, do not precise
all of the above mentioned factors. These standards
advise only the kind of motion (sliding), and suggest the
range of rotational speeds, pin (ball) diameters and
general requirements referring to the construction of the
tester loading unit to reduce vibrations.
Taking the above remarks into consideration, the
authors have elaborated a method for tribological testing
of thin hard engineering coatings. They have precisely
defined almost all of the mentioned factors. The method
is based on the experience gained during the realisation
of the VAMAS-TWA 1 and COST 516 Tribology
projects [3], [29].
In the present work the authors have employed the new
method to compare tribological properties of various
coatings deposited by the PVD process (vacuum-arc
method) like TiN, Ti(C,N), CrN, Cr(C,N),
Cr(C,N)/CrN/Cr and Cr(C,N)/(CrN+Cr2N)/CrN/Cr.
2 TEST METHODOLOGY
2.1 Substrate and coating preparation
Four single layer coatings were employed: TiN,
Ti(C,N), CrN and Cr(C,N) as well as two multilayer
ones: Cr(C,N)/CrN/Cr and Cr(C,N)/(CrN+Cr2N)/
CrN/Cr; Cr(C,N) was the outer layer. All of them were
deposited by the PVD process (vacuum-arc method) on
the steel substrate (discs). The single layer coatings were
2 µm thick. The thickness of particular layers of
Cr(C,N)/CrN/Cr was 1,5, 1,5 and 0,3 µm respectively.
In the Cr(C,N)/(CrN+Cr2N)/CrN/Cr coating the Cr(C,N)
layer was 1,5 µm thick, (CrN+Cr2N) together with CrN
0,85 µm, and Cr 0,3 µm.
The discs were made of hardened and tempered hot-
work tool steel (WCL) with hardness not lower than
HRC 50. Such steel is used for manufacturing of casting
moulds, forging dies and punches. Prior to coating
deposition the discs had been ground and lapped to the
roughness of 0,05 µm (Ra).
2.2 New test method
In general, the developed method conforms to the
requirements during the realisation of the VAMAS-
TWA 1 project [3] (performed in 1993) as well as the
standards: ASTM G 99-90 [10] and DIN 50324 [11].
The unlubricated ball-on-disc tribosystem was chosen
for tribological investigations.
A novelty of the method is the removal of wear debris
from the contact zone through a draught of dry argon
(2 dm3 min-1) - Figure 1.
Ar
Figure 1: The ball-on-disc tribosystem with an Ar jet
The stationary ball, 10 mm in diameter, was pressed
from above at the load 10 N against the disc rotating in
the horizontal plane at the speed of 0,1 m s-1. Track
radius was 18 mm. Ambient temperature was 23°C and
the air relative humidity 50%. Before testing, the
specimens had been washed in an ultrasonic washer with
toluene (for 10 min) and then hexane (5 min).
For tribological assessment of the tested coatings, the
wear volume and friction coefficient were computed.
The wear volume (in mm3) was calculated by
multiplication of the average cross sectional area
(measured using stylus profilometry in three planes
every 120° - Figure 2) by the wear track perimeter. The
friction coefficient was calculated from actual values in
this part of the friction characteristic that corresponded
to steady friction.
1,5
Profile depth [µm]
1,0
0,5
0,0
-0,5
-1,0
-1,5
0,0 0,5 1,0 1,5 2,0 2,5
Traverse length [mm]
Figure 2: Example of the wear track cross section
measured on TiN coating
It was assumed that the coatings should be investigated
at such a distance as there is no sign of their wearing
away. For this purpose, prior to final investigations, the
linear wear of each coating versus sliding distance was
analysed; the linear wear was obtained through profiling
in various sectors of the wear track and its maximum
value was assessed. For example, some TiN coatings at
about 1000 m distance were worn away, i.e. measured
linear wear exceeded the coating thickness (2 µm),
Figure 3. To prevent from this situation, the maximum
sliding distance for TiN coatings was assumed 500 m;
from Figure 2 it can be seen that at this distance the
maximum linear wear of TiN coating is c.a. 0,6 µm.
 4 a)
T iN
3 1,2 12
Lin. wear (µm)

th ic k n e s s

Total lin. wear W (µm)

f

Friction coefficient f
1,0 10
2
0,8 8
W
1 0,6 6
0,4 4
0 0,2 2
0 2 00 40 0 6 00 800 1 00 0 12 00 0,0 0
S lid in g d istan c e (m ) 0 50 100 150 200 250 300 350 400 450 500
Figure 3: The linear wear of 2 µm thick TiN coating Sliding distance (m)
versus the sliding distance
b)
The similar procedure of maximum sliding distance
determination was carried out for the other investigated 1,2 12

Total lin. wear W (µm)

f

Friction coefficient f
coatings. It must be added here that the maximum 1,0 10
sliding distance extremely differed between them; the 0,8 8
shortest value was observed for Ti(C,N) coatings: 15 m, 0,6 6
W
and the longest for CrN: over 6000 m. So, to compare 0,4 4
the tested coatings, the wear rate (in mm3 km-1 N-1) was
0,2 2
calculated for each of them by dividing the coating wear
0,0 0
volume by sliding distance and load.
0 50 100 150 200 250 300 350 400 450 500
For each coating tests were repeated five times. To
Sliding distance (m)
discard any outlying result, Dixon’s test was performed
(at 5 % significance level). Figure 5: The influence of wear debris on the friction
and wear characteristics for the Al2O3 - TiN tribo-
2.3 Test rig system: a) wear debris present in the contact zone,
The experiments were conducted using a special ball- b) wear debris removed (by draught of dry Ar) from the
on-disc tester, known as T-10, intended for precise contact zone
investigation of thin hard coatings. The tester was Thus, the new test method for investigation of thin hard
equipped with a computer-aided specialised system of coatings assumes the wear debris removal. The authors
control and measurements, which made it possible to tried two ways of achievement of this goal - through a
acquire on-line data from different transducers. draught of dry Ar and by changing of the tribosystem
The T-10 tester and its control-measurement system spatial configuration (changing of the position of the
have been designed and are manufactured at ITeE in disc axis from vertical to horizontal).
Radom. They are shown in Figure 4.
3.1.1 Wear debris removal through the draught of
dry Ar
The removal of wear debris from the contact zone
caused a significant reduction in the TiN coating wear
and decrease in the scatter of results, Figure 6. An
influence of a wear debris action on the friction
coefficient value was not observed. In this and the next
figures the confidence intervals, calculated at 95%
probability, have been added.

3.1.2 Wear debris removal by changing of the

tribosystem spatial configuration
Changing of the tribosystem spatial configuration did
not make wear debris remove from the contact zone; at
Figure 4: The ball-on-disc T-10 tester together with the 50% relative humidity it adheres to the disc surface. As
control-measurement equipment can be seen from Figure 7, the TiN coating wear and
friction coefficient, in spite of changing of the position
3 RESULTS AND DISCUSSION of the disc axis from vertical to horizontal, remains the
3.1 Investigation of an effect of wear debris same as in case of the vertical axis and no Ar draught
removal (Figure 6). This enables the authors to conclude that the
Ar draught is a much more efficient way of getting rid of
The presence of wear debris in the contact zone made wear debris than changing of the spatial configuration.
tribological characteristics unstable (Figure 5 a). When
they were removed, the stability was significantly
improved (Figure 5 b).
 a) 3.2 Comparison of tribological characteristics of
the tested coatings
0,012
The wear rates and friction coefficients for the tested
Wear rate (mm km N )
-1

0,009 coatings are shown in Figures 8 and 9 respectively.

-1

N )
100000
3

-1
0,006 10000

-1
W ear rate (m m km
1000
0,003

3
100

-5
*10
0,000 10
1
0
b)
T iN ) )
C,N CrN C,N /Cr Cr
Ti( Cr( CrN rN/
, N)/ )/C
1,2 Cr(
C
C r2N
rN +
)/(C
C,N
Cr(
Friction coefficient

1,0
Figure 8: The wear rates of the tested coatings
0,8
1,2

Friction coefficient
0,6 1,0
0,8
0,4
0,6
Ar
0,4
0,2
TiN ,N) CrN C,N
) r
Figure 6: The influence of the wear debris action on the Ti(C Cr( N/C Cr
/Cr rN/
,N) )/C
(a) TiN coating wear rate, (b) friction coefficient Cr(C
Cr2N
rN+
)/(C
C,N
Cr(
Figure 9: The friction coefficients for the tested coatings
a)
From Figure 8 it is undoubtedly apparent that CrN
coatings exhibit the best antiwear properties. Similar
0,012
results, obtained under laboratory conditions, are
Wear rate (m m km N )
-1

0,009
published in [6] and [7], as well as in [5] (exploitation
-1

tests). Additionally, CrN and Cr(C,N) coatings show

3

0,006 much lower friction coefficient than TiN (Figure 9). The
very good behaviour of CrN and Cr(C,N) coatings is an
0,003 argument for their wider and wider application in the
industry [5], [7].
0,000
The lowest observed friction coefficient for Ti(C,N)
coatings comes from the necessity for their testing - due
b) to intensive wear - at a very short sliding distance
(15 m), at which the roughness of the Al2O3 ball surface
does not increase yet (this takes place for the other
1,2 tested coatings).
The greatest wear intensity observed for Ti(C,N)
Friction coefficient

1,0
coatings results from their surface defects (Figure 10 a),
0,8 which, going along with their highest nanohardness
(hence large brittleness) and poor adhesion to the
0,6 substrate [30], causes very fast coating cracking and
then breaking off. Completely different behaviour
0,4 exhibit TiN coatings - in spite of similar nanohardness,
owing to much lower number of surface defects (Figure
Ar
10 b) and better adhesion [30], they show incomparably
lower wear.
It is also observed (Figure 8) that multilayer coatings
Figure 7: The removal of wear debris by changing of have better antiwear properties than single layer ones,
the tribosystem spatial configuration: (a) TiN coating which is particularly apparent when comparing
wear rate, (b) friction coefficient Cr(C,N)/(CrN+Cr2N)/CrN/Cr and Cr(C,N). This proba-
bly results from a reduction in the crack propagation
intensity possible in multilayer coatings [31].
a)
b)
Figure 10: Optical microscope images of the surface of
(a) Ti(C,N) coatings, (b) TiN coatings
4 CONCLUSIONS
On the ground of the literature overview and results of
their own work, the authors state that to improve
reproducibility during the testing of thin hard coatings,
the following requirements should be met or actions
undertaken:
the substrate material should have approximate
hardness (e.g. HRC 50) and similar roughness
(e.g. Ra = 0,05 µm),
the thickness of investigated coatings should be
close to one another (e.g. 2 µm),
setting up of the identical kind of the motion
(e.g. sliding friction), and tribosystem kind and
configuration (e.g. ball-on-disc; 10 mm ball;
vertical disc axis; ball above the disc),
proper selection of the counterface material;
Al2O3 has been suggested,
determination of the optimum sliding distance
(even local wearing away of the coating ought
to be avoided),
removal of wear debris from the contact zone;
the draught of dry Ar (2 dm3 min-1) has been
proposed,
precise control of the air relative humidity and
ambient temperature; 50% and 23°C
respectively have been suggested,
carrying out of experiments at close sliding
speeds and similar loads (e.g. 0,1 m s-1 and
10 N respectively).
Using the developed method for testing of PVD
deposited coatings (arc-vacuum method), i.e.: single
layer TiN, Ti(C,N), CrN, and Cr(C,N), as well as
multilayer Cr(C,N)/CrN/Cr and Cr(C,N)/(CrN+Cr2N)/
CrN/Cr, the authors state also that:
CrN coatings exhibit the best antiwear
properties,
CrN and Cr(C,N) coatings show much lower
friction coefficient (rubbed against Al2O3) than
widely employed TiN,
multilayer coatings have better antiwear
properties than single layer ones.
To sum up, owing to relatively small scatter of obtained
results and very good resolution of the new method, it
can be used at coaters’ laboratories for investigation of
tribological properties of various thin hard coatings.
5 ACKNOWLEDGEMENTS
The authors wish to express their thanks to the scientific
group and their head Dr J. Walkowicz from the Plasma
Technology Centre in Radom for coatings deposition
and valuable advice concerning the substrate
preparation.
The work is partly financed by the Polish Committee for
Scientific Research; the Chairman’s Decision No.
476/E-105/SPUB/COST/T-7/DZ46/99.
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