Materials Research Bulletin 58 (2014) 39–43

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Materials Research Bulletin

journal homepage: www.elsevier.com/locate/matresbu

The tribological performance of laser surface treated CrZrSiN thin films

DongJun Kim, JoungHyun La, SungMin Kim, Sang-Yul Lee *
Center for Surface Technology and Applications, Korea Aerospace University, 76 Hanggongdae-ro, Deogyang-gu, Goyang-si, Gyeonggi-do 412-791, Republic of
Korea

A R T I C L E I N F O A B S T R A C T

Article history: It has been reported that it is possible to significantly improve tribological properties by combining
Available online 28 March 2014 surface texturing and PVD hard coatings. In this study, as a part of a continuing effort to investigate the
feasibility of combining laser surface texturing and a hard coating to improve tribological properties, hard
Keywords: CrZrSiN films were coated on laser surface textured substrates. The influence of the surface texturing
A. Nitrides
with different pattern dimensions on the tribological behaviors of the laser surface textured CrZrSiN films
A. Thin films
were evaluated under both oil lubrication and dry conditions. Under the oil lubrication condition, CrZrSiN
B. Sputtering
C. Electron microscopy
films with narrow texturing showed a five-fold reduction in the average coefficient of friction over the
D. Surface properties films without texturing. However, wide texturing resulted in a degrading of the tribological performance
of the CrZrSiN films. This suggested that optimizing the dimensions of texturing on the substrate surfaces
would be the critical factor in improving the tribological performance of laser surface treated substrates
under an oil lubrication condition. Under the dry condition without oil lubrication, however, a negative
effect of the laser surface texturing on the friction behavior of the CrZrSiN thin films was observed from
the films with both types of pattern dimensions, suggesting that oil lubrication should be provided to
improve the tribological performance of laser surfaced textured surfaces.
ã 2014 Elsevier Ltd. All rights reserved.

1. Introduction dimensions on the tribological behaviors of the CrZrSiN films

Much improved tribological properties became possible with
the emergence of surface texturing. Depressions made on surfaces
act not only as sources to trap wear debris but also as reservoirs for
liquid lubricants [1,2]. Among the many techniques to produce
surface texturing, laser surface texturing (LST) [3–5] has received a
lot of attention because it is very fast and environmentally friendly,
and it also makes it easy to control the shape and size of the
depressions on the surface.
Recently, Lee and coworkers reported an attempt to combine
LST and hard coating to improve the tribological properties in a dry
sliding condition, and their results showed that AlCrSiN films with
honeycomb-structured LST were characterized by a reduction of
the coefficients of friction (CoF) by approximately 15% in the dry
condition [6].
In this study, as a part of a continuing effort to investigate the
feasibility of combining LST and hard coating to improve
tribological properties, hard CrZrSiN films were coated on laser
surface textured substrates with honeycomb-structured LST, and
the influence of surface texturing with different pattern
* Corresponding author. Tel.: +82 107 3500166; fax: +82 231 583770.
E-mail addresses: sylee@kau.ac.kr, rhino5864@gmail.com (S.-Y. Lee).
with LST were evaluated under both oil lubrication and dry
conditions.
2. Experimental detail
In this work, a 20 W power laser marking system (YLP-20, 20 W)
was used to apply surface laser texturing on an AISI H13 steel
substrate. The detailed operating conditions of the system can be
referred to in a previous publication [6]. A honeycomb-structured
pattern with different dimensions was made on the steel substrate,
as shown in Fig. 1. The spatters, which formed during the LST
process, were polished away using SiC #400, and closed field
unbalanced magnetron sputtering was used to deposit the 2 mm-
thick CrZrSiN thin films on the polished steel substrate with
honeycomb-structured LST. A single magnetron source installed
with a segment Cr–Zr–Si segment target (volume ratio: (Cr + Zr):
Si = 11:1) was used. Prior to film deposition, the base pressure of
the sputtering chamber was pumped down to less than 2.0  10 3
Pa, and pre-sputtering was carried out by placing a shutter
between the targets and substrate for ten minutes to clean the
target surface at an Ar pressure of 0.4 Pa. After the target was
cleaned, film deposition was performed in an Ar–N2 mixture
atmosphere by fixing the Ar pressure at 3.0 mtorr and N2 pressure
at 1.2 mtorr. During the deposition, the target power was

http://dx.doi.org/10.1016/j.materresbull.2014.03.018
0025-5408/ ã 2014 Elsevier Ltd. All rights reserved.
40 D.J. Kim et al. / Materials Research Bulletin 58 (2014) 39–43
Fig. 1. Two LST patterns used in this work, (a) narrow texturing and (b) wide texturing.
maintained at a pulsed DC 0.7 kW (frequency: 25 kHz, duty: 70%),
and the substrate bias voltage, target-to-substrate distance,
deposition temperature and substrate rotation speed were fixed
at 100 V, 90 mm, 120  C and 10 rpm, respectively.
The tribological properties of the laser surface treated CrZrSiN
films were evaluated using a ball-on-disk type tribometer with a
9.25 mm diameter Al2O3 ball as a counterpart material. The test
was performed at room temperature with a relative humidity of
45% with and without oil lubrication (5W30 engine oil) under an
applied normal load of 5.0 N. The sliding velocity was 0.25 m/s,
and the total sliding distance was 1000 m. During the test, the
CoF variation on the sliding distance was measured, and a wear
track formed on the specimen after the wear test was examined
with scanning electron microscopy. The debris trapped in the
patterns was analyzed using an EDS (JEOL/JSM-7001F).
3. Results and discussion
The cross-sectional and surface morphologies of the CrZrSiN
film coated on the LST surfaces are shown in Fig. 2. The film showed
a columnar microstructure with an rms value of approximately
1.43 nm. The chemical composition of the film was determined by
EDS analysis to be 28.6%Cr–10.0%Zr–4.2%Si–51.2%N in atomic
percentages, and the microhardness of the film was measured to be
approximately 33.5 GPa using a nanoindenter with the continuous
stiffness measurement (CSM) technique [7], which involves the
application of continuous loading-unloading indentations with a
frequency of 45 Hz.
From the wear tests against an Al2O3 counterpart ball at room
temperature under an oil lubrication condition, the CoF curves of
the laser surface textured CrZrSiN films deposited on the AISI H13
steel substrate are shown in Fig. 3. The results indicated that the
CrZrSiN film with narrow texturing showed an average CoF of
approximately 0.02, while the film with wide texturing showed a
Fig. 2. (a) Cross-sectional micrograph and (b) AFM surface morphologies of the CrZrSiN films.
CoF of approximately 0.12, which was higher than the films
without texturing (0.105). This suggested that the expected
beneficial effect of laser surface texturing could be realized only
with the optimum pattern dimension – i.e., there exists an ideal
pattern dimension for the best tribological performance of laser
textured surfaces. It was noted that the CrZrSiN films showed a
similar CoF (0.02) to that of DLC films under similar test
conditions [8].
After the wear tests against the counterpart Al2O3 ball, the
micrographs of the wear tracks produced on the laser surface
textured CrZrSiN films were recorded and are shown in Fig. 4.
During the wear test under the oil lubrication condition, abrasive
wear was observed from the films without texturing and those
with narrow texturing. The wear widths were approximately
160 mm and 125 mm, respectively. However, the films with wide
texturing showed that the width of the wear track was very wide
(475 mm), and a CrZrSiN film macro-failure was observed, as
indicated by the arrows in Fig. 4c. Traces of the film macro-failures
were not observed from the wear tracks from the films without
texturing or from those with narrow texturing, as shown in Fig. 4a
and b.
A close examination of the LST patterns was made after the
wear test. With respect to the films with narrow texturing, a
localized film failure near the laser surface patterns was
observed, as indicated by the arrows in Fig. 5a. Also found
were residual spatters from the laser surface texturing, which
were not removed completely during the mechanical polishing.
These localized failures of the film near the patterns, however,
did not seem to have a significant influence on the tribological
performance of the films; the CoF of the CrZrSiN film with
narrow texturing was measured to be very low (CoF = 0.02)
without any fluctuations, as shown in Fig. 3. The EDS analysis
from the pattern areas, as indicated by the circle in Fig. 5a,
showed that the pattern areas in the specimens with narrow
 D.J. Kim et al. / Materials Research Bulletin 58 (2014) 39–43 41

Fig. 3. Friction coefficient curves of the laser surface textured CrZrSiN films after wear test under oil lubrication condition.

Fig. 4. Micrographs of wear tracks produced on laser surface textured CrZrSiN films after wear test under oil lubrication condition, (a) without texturing, (b) narrow
texturing, (c) wide texturing.

Fig. 5. SEM micrographs and EDS analysis results from the wear debris produced on laser surface textured CrZrSiN films after wear test under oil lubrication condition, (a)
narrow texturing and (b) wide texturing.

texturing consisted mostly of oil lubricant (mainly carbon
element) without much trace of wear debris. This residual oil
lubricant continuously provided lubrication to the surface for
excellent tribological performance. The fact that wear debris
could not be detected from these patterns by EDS analysis could
be attributed to this residual oil lubricant, which would have
prevented wear debris from being produced during the wear
test. On the contrary, from the films with wide texturing, which
showed extensive abrasive wear and even macro-failure in
Fig. 4c, the EDS analysis from the pattern areas, as indicated by
the circle in Fig. 5b, showed that not only the oil lubricant but
also the wear debris from the CrZrSiN films could be identified.
From the wear tests against an Al2O3 counterpart ball at room
temperature under a dry condition without oil lubrication, the CoF
curves of the laser surface textured CrZrSiN films deposited on the
AISI H13 steel substrate are shown in Fig. 6. It was interesting that
42 D.J. Kim et al. / Materials Research Bulletin 58 (2014) 39–43
Fig. 7. SEM micrographs and EDS analysis results from wear tracks produced on laser surface textured CrZrSiN films after wear test under dry condition without oil
lubrication, (a) narrow texturing and (b) wide texturing.
both films with texturing showed much higher CoFs than the CoF
exhibited by the film without texturing. Also noted was that the
initial increase in the CoF of the films with wide texturing was
much faster than that of the narrow texturing. This could be
explained by the fact that the films with wide texturing were
expected to fail much faster than those with narrow texturing. In
both cases the tribological improvement from performing LST
could not be expected at all under the dry condition without
lubrication. As the wear distance increased, both films with
texturing showed a continuous increase in CoF up to 0.9. Under the
dry condition without lubrication, the nitride H13 steel showed a
CoF of approximately 0.9 [9]. As the films with texturing wore off or
failed during the wear test, the CoF of the films with texturing
became identical to the CoF of the bare H13 steel. The films with
wide texturing wore off or failed much more quickly than those
with narrow texturing, showing a much faster increase in CoF
during the early stage of the tribological test.
From the wear tests against a counterpart Al2O3 ball under a dry
condition without lubrication, the micrographs of the wear tracks
produced on the laser surface textured CrZrSiN films and the EDS
analysis are summarized in Fig. 7. The results showed that during
the wear test under the dry condition without lubrication, the
CrZrSiN films on the laser surface treated surfaces were completely
worn off. Wear widths of approximately 710 mm and 1960 mm
were measured from the films with narrow texturing and with
wide texturing, respectively.
4. Conclusions
In this work, CrZrSiN coatings were successfully synthesized
and applied to the laser surface treated AISI H13 steel. From the
wear tests against an Al2O3 counterpart ball at room temperature
under 5W30 oil lubrication conditions, the CrZrSiN films with
narrow texturing showed an average five-fold reduction in CoFs
over the films without texturing. Wide texturing, however,
resulted in a degradation of the tribological performance of the
CrZrSiN films.
Under the dry condition without oil lubrication, however, a
negative effect of the laser surface texturing on the friction
behavior of the CrZrSiN thin films was observed from the films
with both types of pattern dimensions, suggesting that oil
lubrication is a critical factor for the improvement of the
tribological performance of laser surfaced textured surfaces.
Therefore, it could be concluded that the optimization of the
dimensions of texturing on the substrate surfaces as well as the oil
lubrication would be a critical factor in improving the tribological
performance of laser surface treated surfaces.
Acknowledgement
This research was supported by a grant from the Advanced
Technology Center (ATC) Program funded by the Ministry of Trade,
Industry and Energy of Korea.
 D.J. Kim et al. / Materials Research Bulletin 58 (2014) 39–43 43

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