Surface Engineering

ISSN: 0267-0844 (Print) 1743-2944 (Online) Journal homepage: http://www.tandfonline.com/loi/ysue20

Bias influence on titanium interlayer for titanium

nitride films

G. C. Lain, F. Cemin, C. M. Menezes, C. Aguzzoli, I. J. R. Baumvol, S. S. Tomiello

& C. A. Figueroa

To cite this article: G. C. Lain, F. Cemin, C. M. Menezes, C. Aguzzoli, I. J. R. Baumvol, S. S.

Tomiello & C. A. Figueroa (2016) Bias influence on titanium interlayer for titanium nitride films,
Surface Engineering, 32:4, 279-283, DOI: 10.1179/1743294415Y.0000000097

To link to this article: http://dx.doi.org/10.1179/1743294415Y.0000000097

Published online: 25 Feb 2016.

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 Bias influence on titanium interlayer
for titanium nitride films
G. C. Lain1,2,3, F. Cemin1, C. M. Menezes1, C. Aguzzoli1, I. J. R. Baumvol4,
S. S. Tomiello1,2,3 and C. A. Figueroa*1,2,3
This work investigates the deposition of TiN thin films by cathodic arc evaporation on stainless
steel AISI 304 substrate for decorative applications. The applied voltage bias on the substrate
during the Ti interlayer deposition was varied, and several properties were determined. The
chemical profile, crystalline structure and microstructural properties were analysed by glow
discharge optical emission spectroscopy, glancing angle X-ray diffraction and SEM techniques
respectively. In addition, nanoindentation and sliding tests were performed in order to evaluate
the hardness and scratch resistance of TiN thin films. The results showed that the applied voltage
bias during the Ti interlayer deposition step could modify some properties of the TiN thin films.
Downloaded by [Tulane University] at 06:33 12 April 2016

Indeed, lower oxygen contents and higher critical loads to start a plastic deformation
(scratch resistance) of the TiN thin films are achieved at higher applied voltage biases during the
Ti interlayer deposition. A higher scratch resistance is capable of imparting a long term durability
of metallic pieces for decorative applications.
Keywords: Voltage bias, Ti interlayer, Oxygen content, TiN, Cathodic arc, Scratch resistance

Introduction process parameters such as deposition temperature, de-

Titanium nitride (TiN) coatings have been widely studied
in the last four decades due to their mechanical, tribologi-
cal, chemical and decorative properties.1 In the case of
decorative applications, physical vapour deposition (PVD)
technologies have emerged as a clean alternative to tra-
ditional wet and electroplating processes, which usually
produce high level of pollutants and toxic chemical waste.2
Moreover, TiN coatings have a spotlight position due to its
gold-like colour that is being used to highlight cutlery sets
and sanitary products and even in jewelry as a substitute of
gold thin films.3–4
Among the PVD technologies, cathodic arc evapor-
ation (CAE) is a very attractive technique to produce
decorative thin films and coatings. Cathodic arc evap-
oration can provide hard coatings with high adhesion at
high deposition rates, which allow to produce films with
good properties in fast processes, meeting the needs of
the decorative coating market at low cost.1 Thin film and
coating depositions by CAE involve several steps, where
the surface substrate is cleaned and prepared for inter-
layer and functional layer depositions.5,6 Therefore, the
properties, chemical composition and structure of thin
films deposited by CAE techniques depend on the
1
Centro de Ciênciafs Exatas e Teacnologia, Universidade de Caxias do
Sul, 95070-560 Caxias do Sul, RS, Brazil
2
Plasmar Tecnologia Ltda., 95030-775, Caxias do Sul, RS, Brazil
3
Fineza Ltda., 95070-350, Caxias do Sul, RS, Brazil
4
IF, Universidade Federal do Rio Grande do Sul, Porto Alegre
91509-970, Brazil
*Corresponding author, email cafiguer@ucs.br
position pressure, gas mixture and substrate bias vol-
tage.3,6,7
TiN coatings are easily removed from a substrate with-
out an adhesion interlayer. TiN coatings have intrinsic
compressive stress and, usually, a different thermal
expansion coefficient and chemical incompatibility with
the substrate.8,9 These physicochemical incompatibilities
nucleate mismatches between the TiN coating and the
substrate, which induce the premature delamination of the
coating. Generally, metallic interlayers are deposited
between the coatings/thin film and the substrate in order to
mitigate such a mechanical behaviour. The interlayer acts
as a gradient of both chemical composition and physical
properties that impart better adhesion of the coatings/thin
film.7,11–13 In particular, pure titanium interlayers are
deposited for improving the adhesion of TiN coatings/thin
films on steels.10,11
Most of works in the literature analysed the deposition
parameters of the TiN thin film.13 However, only few
works have been performed in this area with TiN
about the influence of the applied voltage bias on the Ti
interlayer deposition step. In this context, many questions
remain open such as the chemical, mechanical and
tribological properties of TiN thin film due to different
Ti adhesion interlayers. In particular, the use of low
deposition temperatures (70–150uC) would allow to
understand the tribological behaviour of the TiN/Ti/sub-
strate system for decorative applications.
In this work, the influence of the applied voltage bias
during the Ti interlayer step on both the TiN thin film
deposition and the correlation with the structural and
chemical properties of the TiN/Ti/substrate system were

Ñ 2016 Institute of Materials, Minerals and Mining

Published by Taylor & Francis on behalf of the Institute
Received 03 April 2015; accepted 17 June 2015
DOI 10.1179/1743294415Y.0000000097 Surface Engineering 2016 VOL 32 NO 4 279
 Lain et al. Bias influence on titanium interlayer for titanium nitride films
analysed. In addition, nanoindentation and sliding tests
were performed in order to evaluate the scratch
resistance of the TiN thin films.
Experimental
Square samples of 20 mm side were cut from the same
0.5 mm thick AISI 304 sheet [C, 0.08; Mn, 2.00; P, 0.045;
S, 0.03; Si, 1.00; Cr, 18.00–20.00; Ni, 8.00–10.5; balance
Fe (wt-%)]. Before PVD deposition, the samples were
mirror polished by standard metallographic techniques
and were cleaned in ultrasonic bath with alkaline
detergent and rinsed in deionised water.
The deposition process took place in an industrial PVD
equipment by cathodic arc, composed of 12 Ti round
cathodes (diameter of 80 mm), working on DC current of
90 A. The substrate bias was applied by a pulsed DC
source. The chamber has a volume of 3.5 m3.
The deposition process was divided into three steps. The
first step was the sputtering cleaning in an Ar atmosphere
during 300 s and an applied voltage bias of 1100 V at a
working temperature of 125uC. The second step started
when the base pressure reached 3.5|1022 Pa for Ti
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interlayer deposition and during the deposition an Ar
atmosphere fixed at 2.0 Pa was used. The processing time
and temperature for Ti interlayer deposition were 45 s and
125uC respectively. This second step is the focus of our
work because we changed the applied voltage bias from 0 to
2300 V during the Ti interlayer deposition. The third and
final step was the TiN thin film deposition. For all the
samples, the TiN film films were deposited in the same
conditions. The temperature was kept constant at 125uC,
the atmosphere was pure N2 at 4.0|1021 Pa, the applied
voltage bias was fixed at 2100 V and the deposition time
was 120 s.
The crystalline structure of the films were characterised
by glancing angle X-ray diffraction (XRD) at an incidence
angle of 1u. The samples were rotated during the analysis in
order to reduce the grain orientation and texture effects.
A Shimadzu XRD-6000 diffractometer with Cu Ka
(l ¼ 1.5418 Å) radiation was used. The 2h angle ranged
from 30 to 80u at a 2u min21 speed. The morphology and
microstructure of the TiN/Ti/substrate system were
analysed by scanning electron microscopy using a
Shimadzu Superscan SSX-550 in secondary electron mode.
For SEM analysis, the samples were analysed in cross-
section. The thicknesses of both Ti interlayer and TiN film
were measured directly from the SEM analysis. The glow
discharge optical emission spectroscopy technique was
used for determining the chemical profile of the TiN/Ti/
substrate system from surface to bulk. These analyses were
made in a GD-Profiler 2 from Horiba Scientific.
The nanoindentation technique was employed to measure
the hardness of the TiN thin films using a NanoTest 600
from Micro Materials Ltd. The measures were performed
using a Berkovich diamond indenter, with a loading rate of
0.01 mN s21 and a final depth of 30 nm. Finally, the scratch
resistance of the films was measured with the same equip-
ment for the nanoindentation analysis, but using a nano-
scratch module with a 90u conical diamond tip of 50 mm
diameter. The sliding tests started with a constant load of
0.01 mN during the first 100 mm of sliding, followed by a
loading rate of 0.3 mN s21 up to reach a final normal load of
200 mN and, approximately, a total sliding distance of 770
mm. The sliding velocity was 1 mm s21 during all the
280 Surface Engineering 2016 VOL 32 NO 4
experiment, and the lateral force was registered as a function
of normal load and sliding distance. For each sample, five
measures were made and the scratch resistance was defined
as the load necessary to observe the transition from elastic to
plastic deformation of the film, which was determined by the
lateral force in combination with direct observation from
optical microscopy images of the scratches. The Lc
abbreviation was defined as the critical load to start a scratch
at the TiN thin film surface.12
Results and discussion
Microstructure and crystalline structure
Figure 1 shows the cross-section SEM image of the TiN/Ti/
substrate system for the sample obtained with an applied
voltage bias of 2100 V in the Ti interlayer deposition. One
can see that the outermost layer is constituted by a TiN thin
film followed by a Ti interlayer and the substrate. By direct
observation of the SEM images, it is possible to determine
the thickness of both layers, which was of 250 nm for the Ti
interlayer and 450 nm for the TiN thin film in the sample
described above. It is important to remark that the thick-
ness in both layers was measured for all the samples, and
they were roughly constants independently of the applied
voltage bias during the Ti interlayer deposition. Moreover,
a region of the TiN thin film was cracked during the cutting
procedure, and a typical columnar structure is evident
(see Fig. 1 on the left). Taking into account the working
pressure and temperature deposition of our thin films, the
observed columnar structure is in agreement with the
Thornton’s zone model of microstructure for thin films,
and this typical microstructure was, also, confirmed by
several authors.13,14,15,16
Figure 2 shows the XRD diffraction patterns of the
TiN/Ti/substrate system at different applied voltage biases
during the Ti interlayer deposition. By means of the XRD
analysis, it was possible to determine the presence of TiN
with the following planes: (111), (200), (220) and (311).
These typical planes and intensities indicate the formation
of TiN thin films with a face centred cubic crystalline
structure without a preferential orientation.17 Moreover,
it is also possible to see the (111) and (200) planes of an
austenitic structure (c-Fe) from SS 304 substrate (austenitic
stainless steel) and the (110) and (200) planes from a’-Fe.
This last crystalline structure is due to the polishing
process, which caused a mechanical deformation in the
outermost layers of the substrate, transforming the original
austenite to martensite structure.18 However, the Ti
interlayer seems to be amorphous. The XRD analysis allow
to conclude that the crystalline structure of the TiN film
films did not change with the different applied voltage
biases during the formation of the Ti interlayer.
Chemical structure of the TiN/Ti/substrate
system
Figure 3 shows the chemical composition profile of the
TiN/Ti/substrate system for the sample obtained at an
applied voltage bias of 2300 V during the Ti interlayer
deposition. One can see three different chemical regions,
the outermost layer constituted by TiN, an intermediate
layer of Ti and the substrate (AISI 304 steel). In addition,
it is possible to see a relatively high signal of oxygen in both
the TiN thin film and the Ti interlayer. This is due to the
relatively high base pressure (1022 Pa) and the low tem-
perature process (125uC) in which the samples were made.

1 Cross-section SEM image of TiN/Ti/substrate system for sample obtained with applied voltage bias of 2100 V in Ti interlayer
deposition. Columnar structure of TiN thin film is also stressed
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2 X-ray diffraction patterns of TiN thin films deposited at
different applied voltage biases during Ti interlayer
deposition
3 Chemical composition profile of TiN/Ti/substrate system
for sample obtained at applied voltage bias of 2300 V
during Ti interlayer deposition
In order to evaluate the influence of the applied
voltage bias during the Ti interlayer deposition on the
chemical structure of both the TiN thin film and the Ti
interlayer, Figs. 4 and 5 show the N/Ti signal ratio in the
TiN thin films and the oxygen signal in both the TiN
thin film and the Ti interlayer respectively as a function
Lain et al. Bias influence on titanium interlayer for titanium nitride films
4 N/Ti signal ratio in deposited TiN thin film at different
applied voltage biases during Ti interlayer deposition.
Dashed line is guide for eyes
of the applied voltage bias. On the one hand, the N/Ti
signal ratio in the TiN films is roughly the same at
different applied voltage biases during the formation of
the Ti interlayer (see Fig. 4). On the other hand, the
higher the applied voltage bias in the Ti interlayer de-
position, the lower the relative oxygen content in both
the TiN thin film and the Ti interlayer (see Fig. 5).
Consequently, the applied voltage bias during the Ti
interlayer deposition controls not only the oxygen
content in the Ti interlayer but also the oxygen content
in the subsequent step of the TiN thin film deposition.
The phenomenon described above can be understood by
the gettering effect caused by the Ti atoms produced in the
plasma atmosphere. These Ti reactive atoms can react with
the oxygen molecules present in the chamber, helping to
remove this contaminant from the deposition environ-
ment.19 Thus, the gettering effect modifies the oxygen
concentration in the chamber atmosphere leading to
change the oxygen content in both the TiN thin film and the
Ti interlayer. It is important to remark that Ti atoms are
more reactive with oxygen than nitrogen, and, conse-
quently, the oxygen concentration changes in the residual
gas that were introduced by different applied voltage bias
could be detected only in the oxygen content of both the
TiN coating and the Ti interlayer but not in the N/Ti signal
ratio as shown in Figs. 5 and 4 respectively.
Surface Engineering 2016 VOL 32 NO 4 28 1
 Lain et al. Bias influence on titanium interlayer for titanium nitride films
5 Oxygen signal in deposited TiN thin films and Ti
interlayers at different applied voltage biases during Ti
interlayer deposition. Dashed line is guide for eyes
Mechanical and tribological behaviours
Downloaded by [Tulane University] at 06:33 12 April 2016
Figure 6 shows the hardness of the TiN thin films as a
function of the applied voltage bias during the Ti interlayer
deposition. It is clearly seen that there is no significant
changes in this property, even considering the higher
oxygen content in the TiN thin film deposited at relative
low applied voltage biases. In fact, it has already been
shown that the hardness of TiN thin films is deeply
connected with the crystallographic orientations of the
polycrystalline structure.20 Taking into account that the
crystallographic orientations of the TiN thin films depos-
ited in our experiments did not change with the applied
voltage bias during the Ti interlayer deposition, we would
not expect a variation in the TiN thin film hardness
(as shown in Fig. 6). One must stress that the oxygen signal
is qualitative and maybe such an oxygen content range does
not change the hardness of TiN coatings.
The scratch resistance analyses were made as descri-
bed in the experimental section. Figure 7 shows a scratch
analysis made for the sample deposited at an applied
voltage bias of 2300 V during the Ti interlayer
6 Hardness of TiN thin films at different applied voltage
biases during Ti interlayer deposition. Dashed line is
guide for eyes
282 Surface Engineering 2016 VOL 32 NO 4
7 Lateral force versus sliding distance for sample
deposited at applied voltage bias of 2300 V during Ti
interlayer deposition. At bottom, optical microcopy image
of wear track superimposed with above performed sliding
test. Critical load Lc is related to beginning of plastic
deformation (scratch) at TiN thin film surface
deposition. In Fig. 7, a representative sliding curve
(lateral force verus sliding distance) and the obtained
wear track (optical microscopy) for such a sample are
shown. One can see that we defined a critical load Lc in
the transition lateral force between the elastic and
the plastic deformation at the TiN thin film surface. The
transition point is obtained by direct observation of the
optical microscopy images and is related to the scratch
resistance of the TiN thin films at the microscale.
Figure 8 shows the critical load Lc to start the plastic
deformation of TiN thin films as a function of the applied
voltage bias during the Ti interlayer deposition. One can
see that the critical load to scratch a TiN thin film at the
microscale increases with the increasing of the applied
voltage bias during the Ti interlayer deposition following a
linear behaviour. Surprisingly, a previous change in the
deposition process (bias in the interlayer deposition) could
affect a posterior mechanical property in the TiN thin film.
Although the oxygen content in the TiN thin film
depends on the applied voltage bias (see Fig. 5) in the same
8 Critical load Lc to start plastic deformation in TiN thin
films at different applied voltage biases during Ti
interlayer deposition. Dashed line is guide for eyes

manner of the critical load dependence above described
(see Fig. 8), we cannot connect these experimental facts
directly. However, it is well known that the presence of
oxygen in TiN thin films can act as a contaminant, dama-
ging the mechanical properties of the film.21 Indeed,
oxygen concentrations w29 at-% increase the width of the
wear track in Cr–Si–O–N films, probably due to low
toughness and high brittleness of Cr2O3.22 Taking into
account that TiO2 is less toughness and more brittle than
TiN, the presence of more oxygen in the TiN thin films
should degrade the elastic deformation resistance of these
films, leading to a lower capacity of the film to support
sliding normal loads on the surface.
One must summarise that the applied voltage bias could
modify the oxygen content in both the TiN coating and the
Ti interlayer. However, the TiN crystalline structure
depends only on processing temperature and pressure.17
The oxygen content in the TiN and Ti interlayer is a con-
sequence of the oxygen concentration in the residual gas of
the chamber during the process where the last is influenced
by the applied voltage bias.23 Nevertheless, the deposition
rate in both the both the TiN coating and the Ti interlayer
depends more strongly on the ion current density than the
applied voltage bias.23 Finally, these understandings about
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the applied voltage bias in the Ti interlayer deposition lead
to improve the resistance to the plastic deformation of TiN,
i.e. the scratch resistance of thin films with gold-like colour
for decorative applications.
Conclusion
In this work, we studied the influence of the applied voltage
bias during the Ti interlayer deposition on the structural,
chemical, mechanical and tribological properties of the
TiN/Ti/substrate system obtained by CAE.
The crystalline structure, N/Ti signal ratio and the
hardness of the TiN thin films do not change within the
experimental error for the applied voltage biases varying
from 0 to 2300 V.
We could demonstrate a straightforward correlation
between the applied voltage bias during the Ti interlayer
deposition with the oxygen content in both the TiN thin
films and the Ti interlayer. Moreover, such a bias has an
important role during the gettering effect caused by the
Ti reactive atoms, decreasing the available oxygen for
co-deposition.
Finally, the scratch resistance of the TiN thin films
increases linearly with the increasing of the applied voltage
bias during the Ti interlayer deposition, which is an
important process parameter for decorative applications.
We suggest that the oxygen incorporation in the TiN thin
films degrades the resistance to plastic deformation of such
films. These findings may modify the deposition
parameters of industrial processes and improve the
properties as the scratch resistance of gold-like colour thin
films for decorative applications.
Acknowledgements
The authors are grateful to UCS, INCT-INES-CNPq
(#554336/2010-3), CAPES (Brafitec 087/11), FAPERGS,
Plasmar Tecnologia Ltda. and Fineza Ltda. for
financial support. GCL, FC, IJRB and CAF are CNPq
fellows. CMM is CAPES fellow.
Lain et al. Bias influence on titanium interlayer for titanium nitride films
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