October 28, 2005 11:13 00754

Surface Review and Letters, Vol. 12, No. 4 (2005) 631–643

c World Scientific Publishing Company

THE EFFECT OF NITROGEN GAS FLOW RATE ON THE

PROPERTIES OF TiN-COATED HIGH-SPEED STEEL
(HSS) USING CATHODIC ARC EVAPORATION
PHYSICAL VAPOR DEPOSITION (PVD) TECHNIQUE

ALI MUBARAK∗ and ESAH BINTI HAMZAH†

Department of Materials Engineering, Faculty of Mechanical Engineering,
Surf. Rev. Lett. 2005.12:631-643. Downloaded from www.worldscientific.com

Universiti Teknologi Malaysia, 81310,

Skudai, Johor, Malaysia
by UNIVERSITY OF VIRGINIA on 06/23/14. For personal use only.

∗
mubarak74@mail.com
†
esah@fkm.utm.my
MOHD RADZI HJ. MOHD TOFF‡ and ABDUL HAKIM BIN HASHIM§
Coating Materials Programme,
Advanced Materials Research Center (AMREC),
SIRIM Berhad, Lot 34, Jalan Hi-Tech 2/3,
Kulim Hi-Tech Park, 09000 Kulim,
Kedah, Malaysia
‡
mradzit@sirim.my
§
hakim@sirim.my

Received 27 May 2005

Cathodic arc evaporation (CAE) is a widely-used technique for generating highly ionized plasma
from which hard and wear resistant physical vapor deposition (PVD) coatings can be deposited.
A major drawback of this technique is the emission of micrometer-sized droplets of cathode
material from the arc spot, which are commonly referred to as “macroparticles.” In present
study, titanium nitride (TiN) coatings on high-speed steel (HSS) coupons were produced with a
cathodic arc evaporation technique. We studied and discussed the effect of various nitrogen gas
flow rates on microstructural and mechanical properties of TiN-coated HSS coupons. The coat-
ing properties investigated in this work included the surface morphology, thickness of deposited
coating, adhesion between the coating and substrate, coating composition, coating crystallogra-
phy, hardness and surface characterization using a field emission scanning electron microscope
(FE-SEM) with energy dispersive X-ray (EDX), X-ray diffraction (XRD) with glazing incidence
angle (GIA) technique, scratch tester, hardness testing machine, surface roughness tester, and
atomic force microscope (AFM). An increase in the nitrogen gas flow rate showed decrease in the
formation of macro-droplets in CAE PVD technique. During XRD-GIA studies, it was observed
that by increasing the nitrogen gas flow rate, the main peak [1,1,1] shifted toward the lower
angular position. Surface roughness decreased with an increase in nitrogen gas flow rate but was
higher than the uncoated polished sample. Microhardness of TiN-coated HSS coupons showed
more than two times increase in hardness than the uncoated one. Scratch tester results showed
good adhesion between the coating material and substrate. Considerable improvement in the
properties of TiN-deposited thin films was achieved by the strict control of all operational steps.

Keywords: Deposition; TiN; physical vapor deposition (PVD); cathodic arc; micro-
structure; hardness; surface roughness; high-speed steel (HSS).

631
 October 28, 2005 11:13 00754
632 A. Mubarak et al.
1. Introduction
The flexibility of coating processes, especially of
the physical vapor deposition (PVD) method, well
supported by the superior and controllable prop-
erties of modern coatings are, responsible for the
worldwide application of coated tools and many oth-
ers. Coatings are widely used to improve the per-
formance of industrial tools. The bond structure
in transition metal nitrides consists of a mixture
of covalent, metallic and ionic components, and is
responsible for high hardness, excellent wear resis-
tance, as well as chemical inertness. The inclu-
sion of macroparticles and the formation of pitting
Surf. Rev. Lett. 2005.12:631-643. Downloaded from www.worldscientific.com
defects have been considered detrimental features of
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cathodic arc evaporated (CAE) coatings since the
commercialization of these coatings for cutting-tool
and corrosion-protection applications in the early
1980s.1,2 Ti-based hard coating is widely used in
tools, dies and mechanical parts to enhance their
lifetime and performance due to its attractive prop-
erties such as high hardness, high wear resistance
and chemical stability. Among these coatings, Ti-N
and Ti-Al-N are widely used in tools and other hard
surfaces. The deposition of the TiN layers has been
extensively studied because of its interesting golden
color, high hardness, and corrosion resistance of its
film. Over the years, various chamber configurations
and deposition techniques have been developed to
reduce the amount of coating defects.3−5
2. Experiment Procedure
2.1. Surface finish
The samples used for this research are high-speed
steel (HSS) coupons (30-mm diameter, 5-mm thick-
ness). Before charging the samples for deposition,
surface finish is one important parameter to opti-
mize the coating properties. For this purpose, we
used standard grinding and polishing methods to a
surface mirror of 1 µm. Prior to coating, all sam-
ples are subjected to a standard ultrasonic cleaning
in a commercial solvent for 30 minutes before they
are positioned in the deposition chamber. Samples
for SEM-interface study were cut using a Precision
Cutter Accustom-50 Machine. These were mounted
(cold mounting) and polished to a surface of 1 µm
and subjected to standard ultrasonic cleaning. Sam-
ples were then coated with platinum (Pt) using a
polaron sputter coater for SEM surface and interface
studies.
2.2. Coating deposition
In the present work, TiN coatings have been reac-
tively deposited on HSS coupons (substrates) using
a multi-source cathodic arc PVD coating system
that comprise two vertically-mounted titanium arc
sources. The coating system used for this present
study is made of Hauzer Techno Coating Europe BV,
type HTC 625/2 ARC. Two pure titanium rectangu-
lar targets of dimensions 400 mm × 130 mm × 15 mm
were installed on the opposite side of a rectan-
gular deposition chamber. The HSS coupons were
then loaded into the vacuum chamber as shown in
Fig. 1. The average distance between the high purity
(> 99.99 at%) titanium arcs and the substrate holder
was about 180 mm. The turntable substrate holder
was rotated continuously by its axis to provide a uni-
form coating and to form the desired phase; the rota-
tion speed was set to 40% of total. The chamber was
evacuated to a pressure of 4 × 10−6 mbar and then
filled with nitrogen gas in the range of 10−3 mbar.
The substrates were biased at a −1000 V potential
and subjected to metal ion etching for 5 minutes
using two titanium arc sources operating at arc cur-
rents of 100 A. It has been demonstrated that the
metal ion bombardment favors local epitaxial film
growth, which enhances adhesion between coating
N2 gas
Water-cooled
Electrodes
Door
Cathode Substrates Arc
(Target)
Rectifier
Substrate holder
To vacuum pump
DC Bias Supply
Fig. 1. A schematic diagram of the CAE PVD system.
 October 28, 2005 11:13 00754
The Effect of Nitrogen Gas Flow Rate on TiN-Coated HSS
and substrate.6 During deposition, the substrates
were biased with a dc power source to induce proper
ion bombardment on the growing surface to assist the
formation of desirable structure, grain size and film
density. The delivery of gas was by manifolds located
adjacent to the cathodes and gas pressure could be
measured using Baratron and Penning gauges.
For the deposition of the TiN coatings, nitrogen
was introduced into the coating chamber and single-
layer coatings were deposited at arc currents of 100 A
(both cathodes) and a substrate bias potential of
−50 V. A constant nitrogen gas flow rate regulated
by a mass flow controller was introduced into the
chamber before arc ignition, during each experiment.
Surf. Rev. Lett. 2005.12:631-643. Downloaded from www.worldscientific.com
A more detailed list of deposition process parameters
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is given in Table 1.
2.3. Evaluation of coating
properties
The following quantitative and qualitative tech-
niques were used to evaluate the coatings deposited
on polished HSS coupons:

Phase (structure) identification, d-spacing, crystal
orientation of the as-deposited films was identified
with an XRD (Bruker Model D8 Advance X-Ray
Diffractrometer System) using GIA technique.

Surface morphology and interface studies were
done using FE-SEM (Model LEO-1525), which
also enabled a measurement of macroparticle char-
acteristics: size; shape; and distribution.

The thickness of the coatings was measured using
SEM via cross-sections.

The adhesion between the coating and substrate
was observed using SEM via cross-sections.

The elemental composition of coated and
uncoated samples was analyzed using EDX.

The hardness of uncoated and coated samples
were measured using a micro-Vickers hardness
testing machine (Model-H31, Mitutoyo).
Table 1. Deposition parameters.
Substrate N2 gas Coating Substrate
temperature (C◦ ) flow rate thickness bias
250 100 sccm ≈ 4.7 µm −50 V
250 150 sccm ≈ 4.7 µm −50 V
250 200 sccm ≈ 4.7 µm −50 V
633

The surface roughness of uncoated and coated
samples was measured using a surface roughness
tester (Model-Surftest SJ-301, Mitutoyo).

Surface characterization of coated samples was
done using AFM (Model SPM-9500J2, Shimadzu
Corporation).

Adhesion, scratch test, and critical load Lc (N)
were determined by optical observation of the
scratch track (CSM-Instruments, REVETEST).
3. Results and Discussion
3.1. X-ray diffraction (XRD) with
grazing incidence angle (GIA)
Conventional θ–2θ scanning is not suitable for char-
acterizing thin films, because the X-ray path through
the thin films is too short to produce adequate
diffraction intensities relative to the substrate.7
Phase and crystal structures of the as-deposited films
were identified with an X-ray diffractometer, using
CuKα radiation, λ = 0.15406 nm with a Ni filter,
operated at 40 kV and 40 mA, and grazing angle of
1◦ . Scans were recorded in the 2θ ranges from 20 to
90 degrees, with a step size 0.020◦ and a dwell time
of 1 second. Since the path length of X-rays in a
film increased due to the grazing incidence, the rela-
tive intensity associated with the film was enhanced
while that of the substrate decreased. The structure
of the TiN film was identified as having a cubic B1
structure, and the nitrogen atoms occupied all the
octahedral interstitial sites in the fcc metal lattice.
According to the Hägg rule,8 the structure of the
transition metal nitrides is determined by the ratio
(r) of the atomic radius of nitrogen (rx ) to the atomic
radius of the transition metal (rme ), r = rx /rme . If
r is less than 0.59, a simple structure such as B1
or simple hexagonal would be formed. The atomic
radius of nitrogen to titanium is 0.504.8 From Fig. 2,
the prominent high-intensity peak [1,1,1] of titanium
and nitrogen can clearly be seen, as an indication of
desired coatings. The XRD pattern of as-deposited
TiN film is shown in Fig. 2, at various nitrogen gas
flow rates. The main peak [1,1,1] in Fig. 2 showed a
clear indication of fcc crystal structure and shifted
to lower angular position with an increase in nitro-
gen gas flow rates. At a nitrogen gas flow rate of
100 sccm, the value of d-spacing was 2.4518, while
at a nitrogen gas flow rate of 200 sccm, the value of
 October 28, 2005 11:13 00754

634 A. Mubarak et al.

[2,2,0]
[1,1,1]

[2,0,0]

[2,2,2]
[3,1,1]
80
18
d=2.45

70

60
Lin (Cps)

50
95
d=2.11
40

30
05
d=1.50

20

71
d=1.27
10 50
d=1.22

0
20 30 40 50 60 70 80 90
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2-Theta - Scale
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(a)
[1,1,1]

[2,0,0]

[3,1,1]

[2,2,2]
[2,2,0]
60
51
d=2.45

50

40

24
d=2.12
Lin (Cps)

30

05
20 d=1.50

02
d=1.28
10
61
d=1.22
26
d=4.39
0
20 30 40 50 60 70 80 90
2-Theta - Scale

(b)
[1,1,1]

[2,0,0]

[2,2,0]

[3,1,1]

[2,2,2]

60

50

40
Lin (Cps)

01
d=2.46
30 75
d=2.11

38
20 d=1.50

10 76
d=1.27
30
d=1.22

0
20 30 40 50 60 70 80 90
2-Theta - Scale

(c)
Fig. 2. XRD patterns of TiN films by GIA method at various nitrogen gas flow rates: (a) 100 sccm, (b) 150 sccm and
(c) 200 sccm.
 October 28, 2005 11:13 00754
The Effect of Nitrogen Gas Flow Rate on TiN-Coated HSS
d-spacing was 2.4601. The increase in d-spacing and
shifting of the main peak [1,1,1] to lower angular
position in TiN-coated HSS coupon basically indi-
cates an increase in intrinsic stress, whereas, peaks
like [2,0,0] and [2,2,0] showed reflections from the
crystalline metallic titanium.
3.2. Scanning electron microscope
with energy dispersive X-ray
(SEM/EDX)
Surface morphology of the coatings was observed
using a field emission scanning electron microscope
Surf. Rev. Lett. 2005.12:631-643. Downloaded from www.worldscientific.com
(FE-SEM) model LEO-1525. SEM micrographs at
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nitrogen gas flow rates of 100 sccm and 200 sccm
are shown in Fig. 3. Increasing the partial pressure
(a)
(b)
Fig. 3. SEM micrographs of TiN coating at nitrogen gas
flow rates of (a) 100 sccm and (b) 200 sccm.
635
of the reactive gas during deposition can decrease
the number of macroparticles in reactively CAE
coatings.9−11 It was noted that by increasing the
nitrogen gas flow rate, macrodroplets decreased
[Figs. 3(a) and 3(b)]. In TiN deposition, the com-
pound layer of TiN, which has been shown to form
on the surface of the Ti cathodes, has a significantly
higher melting point (2030◦C) compared with the Ti
cathode (1660◦ C).12 This has in turn been shown to
reduce the number of Ti macroparticles deposited in
subsequent TiN coatings.12,13 The thickness of the
deposited coating was about 4.7 µm and can be seen
in Fig. 4(a), whereas, the adhesion between the sub-
strate and coating material can be seen in Fig. 4(b),
which was dense and uniform with the substrate.
The result of energy dispersive X-ray (EDX) anal-
ysis of substrate and deposited coating can be seen
in Figs. 5(a) and 5(b). In Fig. 5(b), a deposited
coating (TiN) can be seen clearly as a high inten-
sity peak. From Table 2, it can be concluded that
by increasing the nitrogen gas flow rate, atomic and
weight percentages of nitrogen gas in TiN coatings
also increased and vice versa. Tables 2 and 3 rep-
resent the elemental composition of substrate and
deposited coating by EDX.
3.3. Hardness
The easiest way to prepare superhard coatings is the
application of energetic ion bombardment during
the deposition, as by Musil.14−16 Substrate hardness
and coating hardness was measured using a micro-
Vickers hardness testing machine. Microhardness of
the uncoated HSS coupon was about 355 HV. After
being coated with TiN, the microhardness increased
to about 929 HV (at N2 gas flow rate of 200 sccm),
which is 261% the hardness of the uncoated one. The
hardness enhancement results from a complex syner-
gistic effect of the decrease of crystallite size, densi-
fication of grain boundaries, built in of compressive
stress and formation of radiation damage (Frenkel
pairs, etc.) upon energetic ion bombardment.17
3.4. Surface roughness
The results of quantitative surface roughness tests
on uncoated and coated HSS coupons are reported
in Table 4. The most commonly-used parameters
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636 A. Mubarak et al.

(a)
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(a)

(b)
Fig. 5. Elemental composition analysis of (a) HSS
coupon and (b) TiN coating by EDX.

Table 2. Elemental composition of HSS

coupon by EDX.

Element Weight % Atomic %

C 2.58 11.15
V 1.06 1.08
Cr 2.82 2.82
Fe 89.69 83.46
(b) Mo 1.55 0.84
W 2.31 0.65
Fig. 4. SEM micrographs showing (a) thickness of TiN Totals 100.00
deposited coating ≈ 4.7 µm and (b) adhesion between the
coating material and substrate at N2 gas flow rate of
200 sccm.
the 0.25–0.49 µm range and is significantly higher
than in the case of the uncoated polished sample,
for characterizing the roughness of PVD coatings i.e. 0.02 µm. The main limitation of Ra is that it
is the average roughness (Ra),18,19 also known as gives no indication of the surface texture, namely
arithmetic average (AA). It is calculated as the area macrodroplets and pitting defects that can have a
between the roughness profile and its mean line, or significant influence on the performance of the coat-
the integral of the absolute value of the roughness ing, particularly for wear resistance applications. Rz
profile height over the evaluation length. Using this and Rq indicate the average maximum height of the
parameter, the roughness of the CAE TiN-coated roughness profile and the root-mean-square (RMS)
HSS coupons defined by the Ra parameter is within roughness of the profile.
 October 28, 2005 11:13 00754

The Effect of Nitrogen Gas Flow Rate on TiN-Coated HSS 637

Table 3. Elemental composition of TiN coating

by EDX.

Element N2 = 100 N2 = 150 N2 = 200

sccm sccm sccm

N (wt%) 21.61 22.64 24.13

Ti (wt%) 78.39 77.36 75.87
Total 100.00 100.0 100.0

N (at%) 48.50 50.01 52.11

Ti (at%) 51.50 49.99 47.89
Total 100.0 100.0 100.0
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Table 4. Surface roughness of CAE PVD using a

surface roughness tester.
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Fig. 6. SEM surface micrograph of TiN coating show-

ing macrodroplets and pitting defects at nitrogen gas flow
N2 gas Ra (ISO) Rz (ISO) Rq (ISO)
rate of 100 sccm.
flow rates µm µm µm

Uncoated 0.02 0.23 0.03

200 sccm 0.25 3.58 0.43
150 sccm 0.33 4.04 0.50
100 sccm 0.49 5.10 0.71
The surface roughness increase resulting from
deposition of the TiN coatings should be attributed
to the PVD process character-cathodic arc evapo-
ration and occurrence of the characteristic micro-
droplets, due to deposition of the pure titanium
droplets, coming from the sputtered target, and
pits developing due to the titanium microparticles
dropping out, immediately after finishing the coat-
ing deposition process. Therefore, the surfaces of
the coatings demonstrate inhomogeneities connected
with shaped occurrences of the droplet-shaped and
elongated microparticles, originating probably from
their sputtering when they hit the substrate sur-
face during the coating deposition process (Fig. 6).
The increase in surface roughness in such a fash-
ion of polished coupons by TiN coatings can be
explained by a large number of macroparticles and
pitting defects, which can be seen in surface rough-
ness profiles Figs. 7 and 8. Harris et al.20 calculated
the roughness of the TiN Coatings on HSS twist drill,
and found that it increased from 0.104 to 0.116 µm as
the chamber pressure decreased from 1.2 to 0.1 Pa.
Golombek et al.21 measured surface roughness Ra,
parameter value 0.59 µm, TiN-coated cement car-
bides using the CAE technique.
3.5. Atomic force microscopy
(AFM) studies
The scanning probe microscope (SPM) is the general
name of a microscope which can observe surfaces at
high magnification by scanning the sample surface
while using a microprobe to detect whatever inter-
action is taking place. SPMs include the scanning
tunneling microscope (STM) and the atomic force
microscope (AFM). The AFM is a microscope that
scans sample surfaces with a microtip (cantilever)
to enable high-magnification observation of three-
dimensional forms. AFM analysis provided us the
surface roughness as a function of the lateral length
scale and an estimation of the columnar grain size.
AFM is also suitable for quantitative study of surface
roughness and scaling parameters.22 The topog-
raphy of the surface samples was observed using
the scanning probe microscope (model SPM-9500J2,
Shimadzu Corporation), with an AFM that was
controlled via the Microsoft Windows 95 OS. An
optical microscope was coupled allowing the visual-
ization of the region in which the AFM images would
be taken. The standard scanning range enabled mea-
surements of 30 µm and up to a height of 5 µm. Inci-
dence strength and position of the laser beam on
the detector could be discerned at a glance. Images
were obtained using a commercial Si3 N4 cantilever
operating in contact mode. Prior to the investiga-
tions of TiN coatings, the excellent performance of
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638 A. Mubarak et al.

(a)
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(b)

(c)

(d)
Fig. 7. Surface profiles of CAE PVD coatings measured using a surface roughness tester (EVA-L = 4.0 mm, λc = 0.8 mm
× 5). (a) Uncoated HSS (ver. 0.2 µm/cm, hor. 200.0 µm/cm); (b) N2 gas flow rate = 100 sccm (ver. 5.0 µm/cm, hor.
200.0 µm/cm); (c) N2 gas flow rate = 150 sccm (ver. 2.0 µm/cm, hor. 200.0 µm/cm); (d) N2 gas flow rate = 200 sccm
(ver. 5.0 µm/cm, hor. 200.0 µm/cm).
 October 28, 2005 11:13 00754

The Effect of Nitrogen Gas Flow Rate on TiN-Coated HSS 639

Average Roughness, 0.6

0.5
0.4
0.3 Ra
Ra

0.2
0.1
0
uncoated 100 150 200
Nitrogen gas flow rate, sccm

Fig. 8. Average roughness of uncoated and TiN-coated

HSS coupons.

the AFM was confirmed by imaging a standard sam-

ple for calibration provided by the manufacturer. We
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only selected typical AFM images consisting of a (a)

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well-defined scan area of 10 µm × 10 µm morphology.

In the present work, AFM with contact mode
has been used to investigate the modifications of
TiN-coated HSS coupons at various nitrogen flow
rates. Figure 9 shows three-dimensional (3D) images,
whish are clear indications of reduction of macro-
droplets with an increase in nitrogen gas flow rate.
Typical AFM 3D images, illustrating the surface
morphology of the TiN film deposited at various nitr-
goen gas flow rates can be seen in Figs. 9(a), 9(b)
and 9(c). It has been reported that the difference
between the structures is attributed to differences in
the preferential growth direction and anisotropy.23
It was noted from Table 5 that the value of Rms
changed from 215.678 nm to 93.195 nm when the (b)
nitrogen gas flow rate increased from 100 sccm to
200 sccm. Chico et al.24 obtained a Rms of 0.98 Å
for the unimplanted surface and 1.92 Å for the
N-implanted region in AISI 304 austenitic stainless
steel.

3.6. Adhesion
The film-to-substrate adhesion strength was mea-
sured quantitatively using a scratch tester. A dia-
mond indenter (Rockwell type) of 200 µm radius
applied an initial load of 0.9 N onto a sample. The
sliding velocity was 1.13 mm/min. The load was
increased gradually by 20 N/min. Scratch length
during each scratch was 5 mm. In the scratch test,
critical load, Lc, could be used to calculate the adhe- (c)
sion strength. In order to obtain the magnitude Fig. 9. 3D AFM images of 10 µm × 10 µm surface at
of the critical load, acoustic signal, friction curve nitrogen gas flow rate of (a) 100 sccm (b) 150 sccm and
and microscope observation were utilized. Acoustic (c) 200 sccm.
 October 28, 2005 11:13 00754

640 A. Mubarak et al.

Table 5. Surface parameter values of TiN-coated

HSS at various nitrogen gas flow rates.

Parameters 100 sccm 150 sccm 200 sccm

Length-X 10 µm 10 µm 10 µm
Length-Y 10 µm 10 µm 10 µm
Area 100 (µm)2 100 (µm)2 100 (µm)2
Ra 178.778 nm 167.874 nm 68.859 nm
Ry 1.108 µm 1.245 µm 862.669 nm
Rz 637.907 nm 658.478 nm 778.473 nm
Rms 215.678 nm 208.279 nm 93.195 nm
Rp 586.998 nm 695.467 nm 405.002 nm (a)
Rv 521.270 nm 549.654 nm 457.667 nm
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signals produced by the delamination of the film

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could be used to characterize the critical load, Lc.

Scratch adhesion testing was performed on a coated
sample to measure the critical load (Lc1) which
corresponds to the load where the first chipping
occurred. The failure behaviors of the films prepared
at various nitrogen gas flow rates were observed
above Lc = 60 N during the test. There was no spal-
lation, chipping and stripping in all samples. Four (b)
various images with various gas flow rates bearing
critical loads are shown in Figs. 10–12. Four dif-
ferent critical loads are shown in Figs. 10(a)–10(d),
Figs. 11(a)–11(d) and Figs. 12(a)–12(d), showing the
character of failure of the coating. Jacobs et al.25 has
identified four main failure events for TiN coatings on
HSS coupons: longitudinal cracks at the track edges
(Lc1), semicircular coating cracks inside the scratch
tracks (Lc2), cohesive chipping at the tracks edges
(Lc3), and spallation at the track edges (Lc4).
When the normal load applied on the indenter
increases, plough-like channels appear in the scratch (c)
trace [(a) of Figs. 10–12]. Cracks originate from the
plough-like channel and spread with the increas-
ing loads [(b) of Figs. 10–12]. As cracks expand
gradually, cracks between two plough-like channels
converge, thereby leading to cohesive chipping and
then spallation at the track edges [(c) of Figs. 10–
12]. Finally, the coating is subject to complete fail-
ure/delamination [(d) of Figs. 10–12]. When the load
increases gradually, the film delaminates from the
substrate at the margins of the scratch trace. Tang (d)
et al.26 observed two types of scratch modes in TiN
Fig. 10. Scratch trace of the crack taken from CSM-
coatings deposited on GCR 15-bearing steel using Revetest at nitrogen gas flow rate of 100 sccm (× 20 K).
plasma immersion ion implantation and deposition (a) Lc1 = 8.50 N; (b) Lc2 = 22.55 N; (c) Lc3 = 63.53 N;
technique. (d) Lc4 = 87.15 N.
 October 28, 2005 11:13 00754

The Effect of Nitrogen Gas Flow Rate on TiN-Coated HSS 641

(a)
(a)
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(b)
(b)

(c)
(c)

(d) (d)

Fig. 11. Scratch trace of the crack taken from CSM- Fig. 12. Scratch trace of the crack taken from CSM-
Revetest at nitrogen gas flow rate of 150 sccm (× 20 K). Revetest at nitrogen gas flow rate of 200 sccm (× 20 K).
(a) Lc1 = 17.26 N; (b) Lc2 = 36.47 N; (c) Lc3 = 63.25 N; (a) Lc1 = 16.29 N; (b) Lc2 = 34.26 N; (c) Lc3 = 64.07 N;
(d) Lc4 = 88.50 N. (d) Lc4 = 83.66 N.
 October 28, 2005 11:13 00754
642 A. Mubarak et al.
4. Conclusions
The objective of this present work is to see the
effect of nitrogen gas flow rates in the range of
100–200 sccm in TiN-deposited coating on HSS
coupons using the CAE technique. The microhard-
ness of the TiN-coated material showed more than
two times the increase in hardness compared to the
uncoated sample. SEM images showed uniform and
dense coating with substrate. EDX analysis showed
an increase in nitrogen content (both at% and wt%)
by increasing the nitrogen gas flow rate and vice
versa. Macroparticles of cathode material decreased
as nitrogen gas flow rate increased. These macro-
Surf. Rev. Lett. 2005.12:631-643. Downloaded from www.worldscientific.com
droplets are favored in terms of hardness properties
by UNIVERSITY OF VIRGINIA on 06/23/14. For personal use only.
but undesirable in the case of wear properties. From
XRD patterns, a main peak [1,1,1] can be clearly
seen, indicating fcc crystal structure. Surface rough-
ness decreased as nitrogen gas flow rates increased
and are favorable in the case of wear properties.
AFM study further boosts the surface roughness
results by increasing gas flow rates to decrease the
surface roughness of coating and vice versa. Scratch
test measurements showed that the intensive dam-
age in coating started at critical loads Lc ≥ 60 N
in the film prepared at various nitrogen gas flow
rates. During the study, it was noted that the data
obtained from surface tester and AFM were not
same. This is mainly because of the selection of dif-
ferent dimensions (evaluation length = 4 mm during
surface roughness testing and surface area = 100 µm
during AFM studies) and various surface on the
samples with different manufacturers. It was con-
cluded that the process parameters in PVD hard
coating played an important role in optimizing the
materials’ properties for specific applications.
Acknowledgments
This work has been financed by the Government of
Malaysia under award letter No. JPA(L) KD333487
(MTCP) and the Ministry of Science, Technology
and Innovation of Malaysia for the IRPA funding
Project No. 03-02-06-0067 SR0006/06-02. Mubarak
Ali would like to express his gratitude to Dr.
Parvez Akhter, Director General Pakistan Council of
Renewable Energy Technologies (Ministry of Science
and Technology, Government of Pakistan) for his
continual support.
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