Tribology International 62 (2013) 124129

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Mechanical and tribological behavior of W/WCN bilayers grown by pulsed

vacuum arc discharge
R. Ospina a, D. Escobar a,b, E. Restrepo-Parra a,b,n, P.J. Arango a, J.F. Jurado b
a
b

Laboratorio de Fsica del Plasma, Universidad Nacional de Colombia Sede Manizales, Km. 9 via al Magdalena, Manizales, Colombia
PCM-Computational Applications, Universidad Nacional de Colombia Sede Manizales, Colombia

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 20 May 2012
Received in revised form
15 December 2012
Accepted 20 January 2013
Available online 16 February 2013

This study investigates W/WCN coatings grown by means of a repetitive pulsed vacuum arc discharge
while varying the substrate temperature from room temperature (RT) to 200 1C. The coatings were
grown using a cathode with W (6N) and WC (6N) targets for the W and WCN layers, respectively, and
an anode that contains stainless-steel 304 as a substrate. The lms grown at RT and at 150 1C possessed
a lower percentage of carbon obtained from energy dispersive spectroscopy. This characteristic was
related to the hardness, the coefcient of friction and the adherence. These lms also possessed the best
mechanical and tribological properties. Several wear mechanisms were identied, such as delamination
and plowing out of abrasive and adhesive particles.
& 2013 Elsevier Ltd. All rights reserved.

Keywords:
Hardness
Wear
Coefcient of friction
Adherence

1. Introduction
The mechanical, tribological and thermal properties of several
metals can be signicantly improved by controlling the incorporation of interstitial elements, such as boron, nitrogen and
carbon [1]. The main interest for studying the properties of
binary and ternary metals containing carbides and nitrides
centers on improving their functional properties and technological applications [2].
Although both W and WC coatings have been used for a
number of applications, not much is known about coatings with
carbon concentrations in an intermediate range below that of
stoichiometric WC [3]. Only tungsten carbide coatings have
thus far been used as coatings for mechanical purposes [4]. The
primary W(N/C) coatings were deposited onto high-speed steel
due to the good wear properties of cemented M2 (AISI) and were
then heat treated (via quenching and tempering) to form carbides
in the bulk state [5]. Gouy-Pailler and Pauleau [6] determined that
the increase in hardness of coatings containing tungsten and
small amounts of carbon was due to isotropic dilatation of the
a-W structural lattice. More recently, Quesnel et al. [7] formed W
layers containing small amounts of carbon for use in W/WC
multilayers as erosion-resistant coatings.

n
Corresponding author at: Laboratorio de Fsica del Plasma,
Universidad Nacional de Colombia Sede Manizales, Km. 9 via al
Magdalena, Manizales, Colombia. Tel./fax: 57 6 887 9495.
E-mail address: erestrepopa@unal.edu.co (E. Restrepo-Parra).

0301-679X/$ - see front matter & 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.triboint.2013.01.014

The microstructure and mechanical properties of nanolayered

W/WC thin lms were studied by Abdelouahdi et al. [8], who
grew lms by reactive sputtering radio frequency on a Si (100)
substrate. The hardness and Youngs modulus were determined
from nanoindentation tests with a Berkovich tip. There has also
been increased interest in WNxCy thin lms for diffusion-barrier
applications [9,10]. Ternary refractory-metal materials such as
WNxCy have some advantage over binary compounds because the
addition of a third element to transition-metal nitrides disrupts
the crystal lattice and induces the formation of amorphous
ternary solid solutions that have a higher recrystallization temperature [11]. The addition of C to WNx also lowers the lm
resistivity [12]. There are also reports in the literature on the
structure and chemical composition of WNxCy, as was presented
by our research group [13]. In our work, W/WCNx coatings were
produced by using a repetitive pulsed vacuum arc discharge on
stainless-steel 304 substrates varying the substrate temperature
from room temperature to 200 1C. C and N concentration dependence on the substrate temperature was studied by EDS. Moreover, x-ray diffraction characterization showed phases of W and
a-WCN (hexagonal). Raman spectra presented two peaks corresponding to D (disorder) and G (graphite) bands in the region of
11001700 cm  1 due to the amorphous carbon. However, the
mechanical properties of this material have not sufciently been
studied and analyzed.
In this paper, the microstructure and mechanical properties
of WCN coatings that were deposited by repetitive pulsed vacuum
arc discharge and formed by varying the substrate temperature (TS) on stainless-steel 304 as substrates were analyzed.

R. Ospina et al. / Tribology International 62 (2013) 124129

The hardness and the coefcients of friction and adherence were

studied to determine the optimal processing conditions.

2. Experimental details
Both the W and WCN layers were deposited using a repetitive
pulsed vacuum arc discharge in a reaction chamber made of
stainless steel. In this chamber, there are two facing electrodes,
a cathode with W (6N) and WC (6N) targets for the W and WCN
layers, respectively. Moreover, samples of 304 stainless steel with
1.3 cm diameter and 2 mm thickness were employed. The substrates were polished and cleaned using an ultrasonic cube.
A high power source designed for generating pulses with different
active and passive times was used to produce a discharge
between the electrodes, and each coating was produced with
four pulses. The active time is limited to the minimum time
necessary for arc formation under a given set of working conditions such as the target material, working gas and pressure. The
inactive arc time can take any theoretical value; however, it is
necessary to take into account that the minimum value is
subjected to the arc extinction time under the given working
conditions (mainly the target material and the working gas).
Initially, the reaction chamber was evacuated to 10  3 Pa; then,
layers were deposited onto the substrates by varying the substrate temperature (TS) using argon as the working gas for the W
layer and a mixture of argon and nitrogen (1:1) for the WCN layer
at 300 Pa with 280 V between the electrodes and a current of
100 A. Both, the W and WCN layers were deposited on the
substrates with four pulses at 1 s and 2 s as passive and active
time respectively. The W layer was grown at RT, while the TS
varied between room temperature (RT) and 200 1C during the
deposition process for the WCN layer. The temperature was kept
constant, being monitored during the entire experiment. This
system is thoroughly described in a previous work published by
our group [14].
A Nanovea Microphotonics nanoindenter was employed for
mechanical characterization of the materials. This indenter consists of a Berkovich-type diamond tip coupled to an IBIS head
(Fischer-Cripps Lab) and a Nanovea Series displacement control
frame. The applied load was varied between 3 mN and 5 mN. IBIS
software for controlling, correcting and analyzing the results was
employed. A scratch test was performed using Micro-Test equipment. The indentation hardness is dened as the mean contact
pressure and is given by HFmax/Ap, where Fmax is the maximum
normal load and Ap is the projected contact area at that load [15].
A Rockwell C indenter was used with a 200-mm radius, a variable
load between 0 N and 90 N, a load application velocity of 1 N/s
and a distance of 5 mm. The coefcient of friction (COF) was
measured with a pin on disc (POD) CSEM instruments tribometer
with a sphere of alumina (Al2O3) that was 6 mm in diameter, a
scratch velocity of 10 cm/s, a radius of 3 mm, a distance of 100 m
and an applied load of 1 N. Energy dispersive spectroscopy (EDS)
was carried out for semi-quantitative elemental analysis. Morphological analysis was carried out with scanning electron microscopy (SEM; Philips XL-30TMP) with a standard probe at energy
of 20 kV with a magnication of 200  .

3. Results and analysis

3.1. Compositional analysis
Diffraction patterns and the analysis of the W/WCN bilayers
obtained by varying the substrate temperature were presented in
a previous work. This analysis identied phases such as W,

125

W2(C,O) and a-WCN (hexagonal) [13,16]. With EDS, the W coating composition was analyzed and the result is presented in
Table 1. Furthermore, the percentages of W, N and C as a function
of TS for WCN coatings were also obtained and are included in
Table 1. These values showed a competition between the percentages of C and N. Initially, an increase in carbon is observed with
increasing TS, thereby generating the formation of CC, CN, CQC
and CQN bonds that cause amorphization of the sample, in
agreement with Kukie"ka et al. [17].
3.2. Morphological characterization
Table 1 lists the values of the W/WCN bilayers thickness as a
function of TS and it also included the thickness of the W layer.
During the thin lm deposition process, there are several
growth mechanisms such as adsorption, nucleation, coalescence
and resputtering. Initially, the thickness of the lm decreases with
increasing TS, which is in agreement with a previous study by Pal
and Jacob [18]. These authors produced WO3 lms on silicon
substrates and stated that the observed behavior is caused by an
increase in the vapor pressure of the deposited material. This
behavior can also be attributed to the resputtering process, which
is important because the atoms gain enough energy at sufcient Ts
to return to the plasma; as a result, less material is deposited, as
reported by Beena et al. [19]. Additionally, the surface morphology
can be described by the average roughness (Ra), which is the most
widely used surface parameter in the industry [20]. The surface
roughness of the lms decreases with increasing TS, as shown
in Table 1. The decrease in surface roughness as a function of TS can
be attributed to the increased diffusion of surface atoms [21].
3.2.1. Nanoindentation test
The mechanical characterization of materials at small length
scales has been widely studied and reported in the literature.
There are several micro- and nano-scale testing techniques for
studying the mechanical properties of materials of interest to the
scientic and industrial communities. The most common technique for determining the hardness of thin lms is the nanoindentation method [22]. A characteristic load and unload curve for the
indentation process for a sample grown at 150 1C is shown
in Fig. 1. In this curve, a maximum load of 1 mN can be obtained
with a penetration depth of 60 nm. The hardness was determined
using the unload curve and nanotribometer software. The hardness values of the W layer and the W/WCN bilayers as a function
of TS are shown in Table 2. In all cases, the hardness of the
W/WCN coatings is greater than that shown by the substrates
with and without W interlayer. Thicker lms (grown at RT and
150 1C) possessed the greatest hardness. These samples also
showed the highest nitrogen percentage according to Table 1.
However, the lm with the least hardness was that grown at 50 1C
Table 1
Percentages of carbon, nitrogen, tungsten, thickness and roughness values for W
layers and W/WCN bilayers depending on TS.
TS (1C) C (wt%)

N (wt%)

W (wt%)

Thickness
(mm)

Roughness
(mm)

RT

W
0.057 0.02

98.67 0.4

0.32 7 0.08

0.27 0.01

RT
50
100
150
200

W/WCN
14.73 7 1.85
21.65 7 1.3
25.13 7 1.4
18.11 7 0.9
29.61 7 1.8

5.72 70.51
2.18 70.19
3.25 70.10
6.21 70.25
2.36 70.11

69.047 1.3
62.38 71.6
58.707 1.2
63.707 1.9
55.11 71.7

0.91 7 0.02
0.87 7 0.02
0.82 7 0.04
1.33 7 0.03
0.65 7 0.01

0.137 0.01
0.117 0.01
0.107 0.02
0.057 0.02
0.037 0.01

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R. Ospina et al. / Tribology International 62 (2013) 124129

1.2

HSS

1.0

COF (adim.)

W
0.8

200 C

0.6

100 C

0.4
50 C

150 C

0.2

RT

0.0
0
Fig. 1. Loadunload curve of the W/WCN bilayer grown at 150 1C, obtained by
nanoindentation.

20

40
60
Distance (m)

80

100

Fig. 2. Plot of the friction coefcient vs. sliding distance for HSS substrates, HSS/W
and W/WCN coatings grown at different values of TS.
Table 2
Wear, adherence and hardness of the HSS substrates, HSS/W and the W/WCN
bilayers as a function of TS.
Material

COF
(adim.)

Maximum
depth (nm)

Wide
(nm)

Hardness
(GPa)

Lc1
(N)

Lc2
(N)

HSS
W
TS
RT
50 1C
100 1C
150 1C
200 1C

1.0 70.5
0.7 70.1
W/WCN
0.35 7 0.06
0.35 7 0.08
0.35 7 0.06
0.32 7 0.05
0.65 7 0.10

700 710
190 7 8

210 7 7
490 7 10

6.37 0.3
7.17 0.2

287 2

43 7 4

650 7 12
700 714
590 7 10
210 7 15
750 7 10

235 7 9
200 75
330 7 8
130 7 4
370 7 6

167 2
7.57 0.4
107 1
187 2
97 1

327 1
97 1
207 2
477 3
197 2

36 7 3
28 7 2
27 7 2
63 7 3
27 7 2

and contained a lower percentage of nitrogen. The amount of

WCN phase tends to increase with increased nitrogen content in a
lm, as reported in a previous study from our group [16]. The
hardness of single phase WCN can reach values of 45 GPa, as
reported by Vencl et al. [15]. The decrease in the hardness of lms
in this study compared to those in the literature could be due to
polycrystalline behavior caused by the formation of different
phases. This decrease could also be caused by a combination of
amorphous and crystalline phases, which is supported by the
broadening of XRD peaks [23,24] and as is reported in [15]. On the
other hand, as is well known, thickness has a strong inuence on
mechanical properties. As is observed in Table 1, the coatings
thickness varies as a function of Ts; then, as a future work, we
propose to carry out studies of coatings with similar thickness in
order to evaluate the inuence of the thickness on several
properties.
3.3. Pin on disc test
Tribological tests were carried out to identify the sliding
conditions, which lead to failure of the coated systems under
testing [25]. Fig. 2 plots the coefcient of friction (COF) as a
function of the sliding distance for the substrate (steel HSS),
substrate/W and W/WCNx when they undergo sliding against
alumina balls during the ball-on-disc tests. The abrupt initial
increase in the COF was due to the sudden increase in contact
area and the increased incidence of adhesion. It is evident that the
coefcient of friction rapidly increases initially; it then decreases

at a sliding distance of nearly 50 m and then increases slowly.

The coefcient of friction maintains a similar value at similar
levels. Samples with a W coating possessed higher coefcients of
friction and resulted in less wear, whereas the W/WCNx samples
exhibited lower coefcients of friction. This is due to adhesion
between the sample and the disc and also possibly due to (i) an
increase in interface heating as a function of the applied load, (ii)
a higher temperature that softens the matrix material thereby
increasing its owability, (iii) greater formation of mechanically
mixed layers, which leads to increased surface smoothening
under higher applied loads and (iv) a greater degree of surface
smoothening of the counter surface due to a greater degree of
material transfer from the counter surface to the specimen [26].
Having into a count that W and WCN are strongly resistant to the
high temperatures; then, the possible most relevant causes that
produce the decrease of COF are (iii) and (iv), because they are
related to the material mixture and transfer.
The HSS and HSS/W  systems behave like steels with both a
high tungsten percentage and metallic phases, as reported by
Kupalova et al. [27]. In this case, polishing was performed; the
COF increased due to adhesion and abrasion of the wear particles.
As the number of these particles increases, the particles become
trapped between the tribological pair, thus producing high wear
and increasing the COF. This phenomenon is visualized at sliding
distances of 10 m and 50 m for HSS and HSS/W, respectively.
For all of the systems presented in Fig. 2, over the rst segment
of sliding distance (approximately 20 m), they exhibited plowing
and removal of surface asperities, which act as a third body. These
asperities can be welded to the coating or penetrate into it
because of the hardening caused by plastic deformation; the
asperities can also act as a rolling agent. After the initial sliding
distance, the systems behave differently. Concerning the bilayers,
it is striking that during the steady-state friction stage, all of the
W/WCNx bilayers showed much lower coefcients of friction than
the substrate (average value of 0.35). Moreover, the coefcients of
friction were generally lower for the WCNx coating than for the W
coating. For the WC/C coating, the literature reports a signicant
decrease in the coefcient of friction as low as 0.29, compared
with the substrate [25].
W/WCN coatings have a particulate system that generates
micro-cuttings along the wear track, as shown in Fig. 3. This

R. Ospina et al. / Tribology International 62 (2013) 124129

127

Fig. 3. SEM micrographs obtained for the W/WCN bilayers grown by varying TS, following a pin on disc test.

gure shows micrographs of the W/WCN coatings grown at RT,

50 1C, 100 1C, 150 1C and 200 1C. After the sliding distance
increases, the particles become trapped between the tribological
pair and causes plowing (especially for the lms grown at 50 1C,
100 1C and 150 1C). In the coatings grown at 200 1C, the asperities
are removed gradually (between 0 m and40 m), and a signicant
change in the COF is observed (Fig. 2). The removal of asperities
creates a mirror-like polished surface, where particles with
laminar wear (spallations) are observed, as shown in Fig. 3(e).
The force of friction decreases due to a decrease in the deformation and the plowing out of the asperities. However, the particles
cannot be easily attached to surfaces from which asperities were
removed. The fractures caused by the asperities decrease after
approximately 50 m (steady-state), which thereby decrease the
production of particles that act as a third body. This process
results in a COF that is 0.65 lower than either HSS or HSS/W and
that is higher than the other W/WCN coatings presented here. The
WCN coatings grown at 200 1C showed irregular behavior with an
increase in the coefcient of friction after approximately 50 m of
sliding. This occurrence was likely caused by the exposure of W
inside the wear track due to the lower adhesion of the coating,
as stated later. One explanation for the low COF could be that,
during the rst part of the test, the main wear mechanism was a
tribochemical process that caused slow removal of the material
from the coating; this material, in turn, formed a lubricating layer
on the contact. Slippery transfer layers have been reported in the
literature when steel or ceramic balls slide against diamond-like
coatings [28,29]. In this study, the transfer layers contained a high
proportion of carbon and could also contain metal oxides. These
layers can act as a lubricant and could be responsible for a very
low wear and friction coefcients. Therefore, the best coating for
sliding applications against hard ceramic counterparts was the
one with low carbon content in the top layer. These coatings
combine low friction and fatigue resistance with adequate resistance to sliding and abrasive wear, thereby leading to a long
lifetime [30]. Furthermore, the W/WCN bilayer that possesses the
highest carbon concentration also exhibits a high COF. However,
all W/WCN systems deposited at different values of TS have
tribochemical reactions in the sliding tracks that are characterized by OH ions due to the relative humidity of the experiment
(55%). There is also a possible formation of subproducts, such as

WO and CO. For these bonds, there will be precipitation of

graphite at the grain boundaries, which generates a selflubricating system with debris that has poor hardness. This debris
is displaced toward the wear boundary tracks and does not cause
problems with micro-cutting that generate delamination (Fig. 3),
as reported by Cano et al. [31]. For better insight of the wear
mechanisms, a high quality SEM micrograph of the pin on disk
test performed on the sample grown at 150 1C was taken and is
shown in Fig. 4(a) and (b). The typical wear mechanisms observed
in Fig. 4 are delamination, fracture, plowing, micro-welding,
adhesion, abrasive particles and laminar particles. Moreover,
EDS analysis was performed on the center of the track and used
to quantify the increase in the percentage of oxygen from 3.7% to
14.9% due to oxidation from tribochemical reactions (Fig. 4(c)).
Table 2 lists the COF and the maximum depth and width of the
wear track obtained by prolometry for the different materials
studied here. Again, the W/WCN lm grown at 150 1C exhibited
the best behavior, having the lowest depth and width in the track.
This result is due to this system exhibiting the highest hardness
and the lowest COF; the combination of these two properties is
correlated to the wear [31].
3.4. Scratch test
Scratch tests were performed on the W and W/WCN lms
grown at different TS. Fig. 5(a) shows the COF as a function of the
applied load for the W/WCN sample grown at 150 1C. The lines
represent critical loads, Lc1 and Lc2. These loads were determined
from the zone where the load becomes independent of the COF.
In the rst stage of the scratch test, micro-cracks and akes
appear when the load is increased (Lc1). This behavior is indicative of a cohesive failure inside the examined coatings as a result
of deformation of the substrate. This deformation is caused by the
pressure of the penetrator. When the load is further increased,
wedge spallations begin to appear, developing laterally to the
movement of the penetrator. A further increase in the load leads
to damage in the form of bilateral coating spallations on the edges
of the scratch and local delamination inside the scratch (Lc1),
which, in the closing part, leads to the partial delamination of the
coating via intensication of spallations and formation of a band.
One can observe many cracks caused by the spreading and

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R. Ospina et al. / Tribology International 62 (2013) 124129

Fig. 4. (a,b) SEM micrographs of the wear track produced by a pin on disc test on samples grown at 150 1C; and (c) EDS analysis of the center of the track left by a pin on
disc test on the sample grown at 150 1C.

TS=150 C

COF (adim.)

0.3

0.2
Lc1 Cohesive

Lc1 Adhesive

0.1

0.0
0

20

40
Load (N)

60

80

Fig. 5. (a) Scratch test of the sample grown at 150 1C. Images of (b) the total scratch track, (c) region of Lc1 and (d) region of Lc2.

recurring spallation of the coating [32]. Fig. 5(b) shows a micrograph of the total scratch test track. The two zones of the critical
load and the nal behavior of the lm can be observed. Fig. 5(c)
and (d) shows the magnication of the Lc1 and Lc2 failures,
respectively.

The values obtained for the critical loads Lc1 and Lc2 are listed
in table 2. It is again observed that the W/WCN coating produced
at 150 1C presents the highest critical load (Lc1 and Lc2) values and
the best adhesion behavior. These results are caused by an
increase in resistance to deformation due to the greatest hardness

R. Ospina et al. / Tribology International 62 (2013) 124129

and a low coefcient of friction, compared to the W lm and other

lms grown at other values of TS. However, the roughness is
strongly correlated to the scratch test analysis [33].
In summary, there is a strong inuence of TS on the mechanical
and tribological properties of W/WCN coatings. It appears that
lms grown at 150 1C possess the lowest carbon percentage (thus,
the highest nitrogen concentration) and exhibit the best hardness,
lowest COF and highest adherence to the substrate.

4. Conclusions
W/WCN bilayers were grown using a repetitive pulsed vacuum
arc system by varying the substrate temperature. This study
focused on analysis of the mechanical and tribological properties
of these systems. The lm grown at 150 1C exhibited the highest
degree of hardness, the lowest COF and the highest adhesive and
abrasive loads (Lc1 and Lc2). In addition, the typical wear mechanisms identied were delamination, fracture, plowing, microwelding, adhesion, abrasive particles and laminar particles. Moreover, EDS analysis of the center of the track indicated an increase
in the percentage of oxygen from 3.7% to 14.9% due to oxidation
arising from the tribochemical process.

Acknowledgments
The authors gratefully acknowledge the nancial support of La
direccion Nacional de Investigaciones de la Universidad Nacional
de Colombia Sede Manizales during the course of this research
under the Project Produccion y Caracterizacion de recubrimientos
con aplicaciones industriales y biocompatibles.
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