C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
409–415
PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN
COATING ON A MACHINE COMPONENT
VPLIVNI PROCESNI FAKTORJI HITROSTI NANOSA TiN
PREVLEKE NA STROJNI ELEMENT
Charnnarong Saikaew
Department of Industrial Engineering, Faculty of Engineering, Khon Kaen University, 123 Friendship Highway, Mueang Khon Kaen District,
Khon Kaen 40002, Thailand
Prejem rokopisa – received: 2018-09-07; sprejem za objavo – accepted for publication: 2018-12-17
doi: 10.17222/mit.2018.211
In this work, a titanium nitride (TiN) coating applied with the oblique-angle DC-magnetron sputtering technique was systema-
tically studied using designed experiments. The TiN layer was applied on an upper hook, which is a machine component of a
fishing-net weaving machine. The goal was to investigate the influence of sputtering process factors on the deposition rate and
to find appropriate operating conditions for statistically significant factors in order to improve the thin-film manufacturing
process, raising the quality of the TiN coating. Five process factors including the oblique angle, rotational speed, sputtering DC
current, operating pressure and Ar to N2 flow-rate ratio were simultaneously investigated using the 2
5–1
fractional factorial
design method. A normal probability plot of effects, and main and interaction-effect plots of the process factors were con-
structed in order to identify the significant process factors and the appropriate operating conditions. The main factors including
the oblique angle, sputtering DC current, operating pressure, gas-mixing ratio, interactions between the oblique angle and
sputtering DC current, and interactions between the oblique angle and gas-mixing ratio were found to be statistically significant
process factors. Moreover, the appropriate operating conditions for the significant process factors were obtained with the
graphical method.
Keywords: TiN, deposition rate, statistical analysis, ANOVA, coating
Avtor opisuje sistemati~no {tudijo na~rtovanih preizkusov nanosa titan nitridne (TiN) prevleke s postopkom po{evnokotnega DC
magnetronskega napr{evanja. TiN prevleka je bila nane{ena na zgornji kavelj, ki je strojni element naprave za navijanje ribi{ke
mre`e. Cilj {tudije je bil raziskati vpliv procesnih parametrov napr{evanja na hitrost nana{anja prevleke in ugotoviti primerne
pogoje delovanja statisti~no pomembnih faktorjev za izbolj{anje kvalitete procesa izdelave tanke TiN prevleke. Isto~asno je bilo
raziskovanih pet (5) procesnih faktorjev, in sicer nagibni kot, hitrost vrtenja, DC (enosmerni) elektri~ni tok napr{evanja, delovni
tlak in razmerje med hitrostjo pretoka Ar in N2. Uporabljena je bila 2
5–1
frakcionirana faktorska metoda. Konstruirani so bili
grafi~ni prikazi normalne verjetnosti vplivov ter glavnega in interakcijskega u~inka pomembnih procesnih faktorjev in ustreznih
pogojev delovanja naprave. Avtor ugotavlja, da so statisti~no pomembni naslednji procesni faktorji: nagibni kot, hitrost vrtenja,
jakost enosmernega elektri~nega toka napr{evanja, delovni tlak ter razmerje med hitrostjo pretoka plinov in interakcije med
kotom nagiba in DC elektri~nim tokom napr{evanja ter kotom nagiba in razmerjem hitrosti pretoka plina. Nadalje je avtor s
pomo~jo grafi~ne metode dobil ustrezne pogoje delovanja naprave glede na pomembnost procesnih faktorjev.
Klju~ne besede: TiN, hitrost nanosa prevleke, statisti~na analiza, ANOVA, prevleka
1 INTRODUCTION
Titanium nitride is one of extremely hard ceramic
materials, widely used as a coating to harden and protect
cutting and sliding surfaces due to its excellent charac-
teristic properties such as friction coefficient, hardness,
abrasive wear and corrosion resistance under various
working conditions.
1
It has a cubic structure of the NaCl
type with a high modulus of elasticity of 250–450 GPa
and a high Vickers hardness of 18–21 GPa.
2
However, its
surface and material properties are considerably depen-
dent on its production process. The most common me-
thods for applying a TiN coating are physical vapor
depositions (PVD) including sputtering, filtered cathodic
arc, electron-beam evaporation and chemical vapor depo-
sition (CVD).
3
Among these, sputtering is the most
widely used method due to its well-controlled process
and high-quality thin-film coating. TiN is normally pro-
duced with reactive sputtering, during which sputtered Ti
atoms are reacted with nitrogen ions to form TiN mole-
cules.
4
Oblique-angle-deposition (OAD) or glancing-angle-
deposition (GLAD) technique is a modified deposition
method, in which the substrate is tilted at different angles
with respect to the normal of the deposition direction and
rotated at an appropriate speed.
5
Typically, properties
and structures of TiN coatings for various applications
using this technique depend on coating conditions
including oblique angle, Ar pressure, Ar to N
2
flow-rate
ratio.
6–9
The main advantage of this technique is the
ability to control the diameter, shape and density of
nanostructures by varying the deposition conditions con-
sisting of oblique angle, rotation speed, operating
pressure, gas-mixing ratio and sputtering power. The
technique is used for a TiN hard coating to produce a
high-density nanocolumnar structure that can have an
Materiali in tehnologije / Materials and technology 53 (2019) 3, 409–415 409
UDK 621.941:519.233.4 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 53(3)409(2019)
*Corresponding author e-mail:
charn_sa@kku.ac.th

extreme hardness, low friction coefficient and very high
wear resistance.
10
Fishing-net companies in Thailand and outside Thai-
land (owned by Thai people) have confronted the prob-
lem of high-cost spare parts of fishing-net weaving
machines. In this study, a TiN layer was applied on an
upper hook, which is a component of a fishing-net weav-
ing machine as illustrated in Figure 1. The TiN coating
applied using the OAD technique with DC magnetron
sputtering was systematically studied through designed
experiments in order to improve the manufacturing-pro-
cess quality of the TiN coating on the machine compo-
nent. Five process factors including oblique angle,
rotational speed, sputtering DC current, pressure, and Ar
to N
2
flow-rate ratio were simultaneously investigated
using the fractional factorial design method. The depo-
sition rate was a response used to achieve the effects of
the process factors.
2 MATERIALS AND EXPERIMENTAL PART
A cast stainless-steel upper hook was made with
lost-wax casting and machined with turning and milling
operations. The chemical composition of the workpiece
material was 62.28 % Fe, 6.91 % Ni, 21.99 % Cr, 3.12 %
Cu, 1.94 % Mn, 2.2 % Si, and 1.56 % Al. A vibratory
finishing machine with mixed ball-burnishing media in
different sizes ranging from 5 mm to 8 mm was used for
surface finishing.
In this study, an eight-step method of planning and
conducting the experiment was used as described below:
Setting the objectives: The main objectives of this
study were to investigate the effects of the sputtering-
process factors on the deposition rate of the TiN coating
on the upper hook and to obtain appropriate operating
conditions of the statistically significant process factor(s)
of the TiN coating. A high deposition rate was preferred
to increase the thin-film manufacturing throughput.
Identifying the important process factors: Consider-
ing the TiN oblique-angle sputtering process, we identi-
fied five main process factors that control the coating
behavior including oblique angle, rotational speed,
sputtering DC current, pressure, and Ar to N
2
flow-rate
ratio.
Determining the upper and lower limits of the pro-
cess factors: For the current sputtering system, the
ranges of the oblique angle, rotation speed, sputtering
DC current, pressure, and Ar to N
2
flow-rate ratio were
70° and 80°, 32 min
–1
and 64 min
–1
, 0.35 A and 0.45 A,
40 Pa and 80 Pa, and 0.5 and 1.33, respectively.
Developing of the design matrix: The 2
5–1
fractional
factorial design for this study consisted of 16 factorial
runs. The defining relation for this design was I =
ABCDE where A represented the oblique angle, B was
the rotation speed, C denoted the sputtering DC current,
D was the pressure, and E represented the Ar to N
2
flow-rate ratio. Every main effect was associated with
a four-factor interaction, and every two-factor interaction
was aliased with a three-factor interaction. Therefore, the
design was resolution V. The design provided good
information regarding the main effects and two-factor
interactions.
Applying the TiN coating as per the design matrix:
The oblique-angle coating system consisted of a high-
vacuum chamber equipped with a 3" target magnetron
gun, 600 W radio-frequency generator, 400 W DC-power
supply and a turbomolecular pump. The TiN was depo-
sited on the upper hook using DC magnetron sputtering
of pure titanium under a mixture of argon (Ar) and
nitrogen (N
2
). The TiN deposition experiments were
systematically carried out in accordance with the 2
5–1
fractional factorial design. There were five samples for
each condition and the experiments were run in a random
order to avoid a statistical bias in the analyses. The dist-
ance between the substrate (i.e., the upper hooks) and the
target (i.e., titanium) was held constant at 5 cm. An
oblique-angle sputtering device and an oblique-angle-
sputtering schematic diagram are illustrated in Figure 2.
Recording the response: The film thickness was
measured with a white-light interferometric optical profi-
ler (Polytech model 2000). The deposition rate was
calculated from the film thickness and deposition time.
The surface microstructure was examined by means of a
scanning electron microscope (SEM). SEM measure-
ments (Hitachi model S-4700) were performed in the
secondary electron mode at an accelerating voltage of
10 kV.
Analyzing the results using the graphical tools for a
data analysis and interpretation: Analysis of variance
(ANOVA) was used to investigate the effects of the five
sputtering-process factors on the average deposition rate.
Graphical tools included a normal probability plot of the
effects and the main and interaction effect plots of the
significant process factors.
11,12
Determining an appropriate operating condition for
the system: The objective of this analysis was to maxi-
mize the deposition rate in order to increase the manu-
facturing throughput of the machine component. The
C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
410 Materiali in tehnologije / Materials and technology 53 (2019) 3, 409–415
Figure 1: Fishing-net weaving machine and the upper hooks

main and interaction effect plots as well as response
surface and contour plots were used to obtain the
appropriate statistically significant process factor(s).
3 RESULTS AND DISCUSSION
Table 1 shows the matrix design consisting of the
five sputtering-process factors together with the corres-
ponding responses (deposition rates). In Table 1, A, B,
C, D and E represent the factors including the oblique
angle, rotational speed, sputtering DC current, pressure,
and Ar to N
2
flow-rate ratio, respectively.
Table 1: 2
5–1
experimental design for the deposition rate
Factor Dep. rate
ABCDE
70 32 0.35 40 1.33 3.8
80 32 0.35 40 0.50 1.8
70 64 0.35 40 0.50 2.6
80 64 0.35 40 1.33 2.4
70 32 0.45 40 0.50 4.0
80 32 0.45 40 1.33 3.0
70 64 0.45 40 1.33 6.2
80 64 0.45 40 0.50 2.2
70 32 0.35 80 0.05 3.2
80 32 0.35 80 1.33 3.5
70 64 0.35 80 1.33 5.1
80 64 0.35 80 0.50 3.2
70 32 0.45 80 1.33 7.3
80 32 0.45 80 0.50 3.0
70 64 0.45 80 0.50 5.2
80 64 0.45 80 1.33 4.2
Figure 3 illustrates the probability plot of the
deposition-rate data set. The probability plot shows that
the plotted points approximately formed a straight line
and fell within the C.I. The AD statistic was small with a
high p-value compared to the level of significance ( =
0.05). This confirmed that the normal probability distri-
bution fitted the data set of the deposition rate very well.
The adequacy of the underlying model should be
checked before performing the statistical analysis and
interpretations of the ANOVA. The primary diagnostic
tool is a residual analysis.
13
Figure 4a illustrates the
normal probability plot of residuals for the deposition
rate of the TiN coating on the upper hooks. Generally,
the normal probability plot of residuals does not show
anything particularly troublesome, although some resi-
duals bend down slightly on the left side.
If the model is adequate and the assumption is satis-
fied, the residuals should be structureless. The residuals
should be unrelated to any other factors including the
predicted response. A plot of residuals versus predicted
values is employed to check the non-constant variance.
Figure 4b does not show any violation of the assumption
of homogeneity of variances because the plot does not
look like an outward-opening funnel or megaphone.
The plot of residuals versus run order or time is used
to check the independence assumption. Figure 4c dis-
plays the residuals and the time sequence of data collec-
tion for the deposition-rate data. There is no reason to
suspect there was a violation of the independence
assumption since the plot does not have a pattern such as
the sequence of positive and negative residuals.
A normal probability analysis of effects was used to
identify the statistically significant main effects and
interaction effects on the deposition rate of the TiN
coating. The main and interaction effects of the process
factors were plotted against the cumulative normal pro-
bability (in percent) in this analysis.
13
Figure 5 illustra-
tes a normal probability plot of effects of the sputter-
ing-process factors on the deposition rate for the TiN
coating. It is worth noting that the effects that fall off
from each end of the straight line were deemed to be
statistically significant whereas those that fall roughly
along the straight line were deemed to be statistically
C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
Materiali in tehnologije / Materials and technology 53 (2019) 3, 409–415 411
Figure 3: Probability plot of deposition-rate values
Figure 2: Oblique-angle-sputtering schematic diagram

insignificant. The normal-probability data showed that
the four process factors, oblique angle (factor A), DC
current (factor C), pressure (factor D) and Ar to N
2
flow-rate ratio (factor E) had significant impacts on the
average deposition rate. Furthermore, interaction effects
between oblique angle and DC current (A × C)a n d
oblique angle and Ar to N
2
flow-rate ratio (A × E) were
statistically significant at a significance level of 0.05.
The result from Table 1 was analyzed with ANOVA,
which was employed for investigating the effects of the
five sputtering-process factors on the average deposition
rate of the TiN coating. Table 2 shows that the model
F-value of 87.85 with a very small p-value was adequate,
having a large coefficient of determination (R
2
)o f
0.9832; it was defined as the ratio of the explained
variation to the total variation and was a measure of the
degree of fit. The adjusted R
2
of 0.9720 and predicted R
2
of 0.9469 were in reasonable agreement where the
difference between the two values was less than 0.2.
Table 2 also shows that the sources of variation with a
p-value of less than 0.05 were considered to have a
statistically significant contribution to the average depo-
sition rate. The ANOVA results for a reduced model
obtained by selecting the statistically significant terms
with the 0.05 level of significance indicated that the most
statistically significant factor affecting the average
deposition rate was the oblique angle, which explained
the largest contribution, accounting for 37.64 % of the
total variability. The Ar to N
2
flow-rate ratio, DC current
and pressure had lower contribution levels; similarly, the
interaction of oblique angle and DC current, and the
interaction of oblique angle and Ar to N
2
flow-rate ratio
also had lower contribution levels.
In order to interpret the interaction effect effectively,
interaction plots were constructed as shown in Figure 6.
Here, non-parallel lines reveal that there were interac-
tions between the oblique angle and DC current as well
as between the oblique angle and Ar to N
2
flow-rate
ratio. The effect of the oblique angle on the deposition
rate was different at low and high levels of DC current.
This showed that the maximum deposition rate was
obtained when the oblique angle was at a low level (75°)
and the DC current was at a high level (0.45 A). Simi-
larly, the interaction effect plot also clearly indicated that
the maximum deposition rate was found when the
oblique angle was at a low level (75°) and the Ar to N
2
flow-rate ratio was at a high level (1.33).
To determine the appropriate operating conditions of
the significant process factors affecting the deposition
C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
412 Materiali in tehnologije / Materials and technology 53 (2019) 3, 409–415
Figure 4: Model adequacy checking of the residuals for deposition-rate values: a) normal probability plot of residuals, b) plot of residuals versus
predicted values, c) plot of residuals versus run order
Figure 6: Interaction plots of angle, DC current and Ar/N
2
for the
deposition rate of TiN coating
Figure 5: Normal probability plot of effects for the deposition rate of
TiN coating

rate for the TiN coating of the fishing-net weaving-
machine component, a numerical analysis using the res-
ponse surface methodology was carried out. After
performing the regression analysis, the empirical rela-
tionship between the deposition rate and the oblique
angle, pressure, DC current and Ar to N
2
flow-rate ratio
was:
R = 3.77 – 0.87A + 0.57C + 0.55D + 0.62E - 0.39AC –
0.26AE (1)
Response-surface plots and contour plots for the
deposition-rate response in terms of oblique angle and
DC current and oblique angle and Ar to N
2
flow-rate
ratio were constructed using Equation (1) as shown in
Figure 7. We can notice that the deposition rate was
higher in the region of a low oblique angle, high DC
current and high Ar to N
2
flow-rate ratio. The positive
signs for the coefficients of pressure, DC current and Ar
to N
2
flow-rate ratio in the fitted model for the deposition
rate indicated that the deposition rate increased with
increasing levels of the process factors. On the other
hand, the negative sign of the oblique angle showed that
the deposition rate increased with a decreasing level of
this factor. Furthermore, the negative signs for the
coefficients of the two interactions meant that an
increase in the deposition rate was obtained due to
simultaneous changes of the process factors in the oppo-
site directions. The contour plots and response-surface
plots also confirmed that the maximum deposition rate
was found when the oblique angle was at a low level
(75°), DC current at a high level (0.45 A) and Ar to N
2
flow-rate ratio also at a high level (1.33). Jing et al.
stated that the deposition rate of TiN deposited on a
316L stainless-steel substrate increased with a decreas-
ing inclination angle, which could be treated as a geome-
trical issue.
14
Figure 8 shows the plot of experimental observations
and predicted values, used to investigate whether the
statistical model fits the experimental observations.
13
The
plot illustrates that most of the data points lie in a
straight line. This indicates that the statistical model fits
the experimental observations for the TiN coating on the
machine component.
C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
Materiali in tehnologije / Materials and technology 53 (2019) 3, 409–415 413
Figure 8: Relationship between the actual deposition rate and predic-
ted deposition rate
Figure 7: a) Response surface plot, b) contour plot for oblique angle
and DC current, c) response surface plot, d) contour plot for oblique
angle and Ar to N
2
flow-rate ratio
Table 2: ANOVA table for the deposition rate of TiN coating
Source of variation Sum of squares
Degree of
freedom
Mean square F-value p-value % contribution
Model 31.96 6 5.33 87.85 < 0.0001
A-Angle
12.24 1 12.24 210.82 < 0.0001 37.64
C-DC current
5.26 1 5.26 86.84 < 0.0001 16.20
D-Pressure
4.79 1 4.79 79.07 < 0.0001 14.75
E-Ar/N
2 6.17 1 6.17 101.73 < 0.0001 18.98
AC 2.40 1 2.40 39.60 0.0001 7.39
AE 1.10 1 1.10 18.06 0.0021 3.37
Residual 0.55 9 0.061
Total 32.50 15

Figures 9a and b show photographs of the upper
hooks before and after the TiN coating, respectively.
Before the coating, the upper hooks were silver, with the
small one being shinier. This was because the small one
was pre-coated with chromium. After the coating, the
upper hooks were of a dark yellowish color, indicating a
successful TiN coating.
Figure 10 shows typical SEM micrographs of the
upper hooks before and after the TiN coating. First, the
hook surface was very rough indicating many micro-
scratches and pits. After the coating, the hook surface
became smooth. Large pits and scratches were dimi-
nished whereas most of the fine scratches and pits
disappeared. Thus, the surface roughness of the upper-
hook surface could be significantly decreased by coating
it with sputtered TiN. The coating was expected to
provide a considerable improvement in the surface
quality regarding the wear resistance of the upper hook.
4 CONCLUSIONS
This work investigated the effect of sputtering
process factors on the average deposition rate in order to
enhance the manufacturing-process quality of a TiN
coating on a machine component of a fishing-net weav-
ing machine. A 2
5–1
fractional factorial design, ANOVA
and other statistical-analysis tools were used to find the
statistically significant process factors and to obtain the
appropriate operating conditions for the significant
factors. The results of this study can be summarized as
follows:
The oblique angle made the largest contribution to
the total variability at a 0.05 significance level.
The Ar to N
2
flow-rate ratio, DC current and pressure
had lower contribution levels.
The interaction of the oblique angle and DC current
and the interaction of the oblique angle and Ar to N
2
flow-rate ratio had lower contribution levels.
The highest deposition rate was found when the
oblique angle was 75°, DC current was 0.45 A and Ar to
N
2
flow-rate ratio was 1.33.
Further research should investigate the performance
of TiN by carrying out wear experiments on the machine
components of a real fishing-net weaving machine.
Moreover, appropriate operating conditions for the
process factors should be determined using the response
surface methodology coupled with the desirability
function approach, based on the data sets for the
deposition rate and wear rate.
15,16
Acknowledgement
The author gratefully acknowledges the Thailand
Research Fund (TRF), grant no. RSA 5980025, and the
Faculty of Engineering, Khon Kaen University for the
financial supports of this research.
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C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
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Figure 10: Typical SEM micrographs of the upper hooks: a) before
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C. SAIKAEW: PROCESS FACTORS AFFECTING DEPOSITION RATE OF TiN COATING ON A MACHINE COMPONENT
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