Arab J Sci Eng
DOI 10.1007/s13369-014-1544-2
RESEARCH ARTICLE - MECHANICAL ENGINEERING
Optimisation of Electrophoretic Deposition Parameters in Coating
of Metallic Substrate by Hydroxyapatite Using Response Surface
Methodology
Mahtab Assadian · Mostafa Rezazadeh Shirdar ·
Mohd. Hasbullah Idris · S. Izman · Davoud Almasi ·
Mohammad Mahdi Taheri · Mohammed Rafiq Abdul Kadir
Received: 11 June 2014 / Accepted: 30 November 2014
© King Fahd University of Petroleum and Minerals 2015
Abstract Hydroxyapatite bioactive coating was deposited
on treated medical grade stainless steel 316L by elec-
trophoretic deposition. Two independent variables including
deposition voltage and time span were evaluated in order to
investigate their effect on substrates’ corrosion potential and
coating mass. After deposition, coated substrates were post-
treated in a vacuum furnace at 800 ◦ C. The experimental plan
was based on a central composite design to create a precision
of the mathematical models. The precision of mathematical
model and relative parameters were evaluated by variance
analysis. Optimum parameters value, considered as simul-
taneous minimum ion release and maximum coating mass,
were predicted at the deposition voltage of 25.93 V and depo-
sition time span of 159 s. The validity of the model generated
by response surface methodology was evaluated by compar-
ing the predicted and experimental results. In addition, close
agreement between experimental and predicted results was
observed.
Keywords Electrophoretic deposition · Nano-
hydroxyapatite · 316L SS · Response surface methodology
M. Assadian · M. Rezazadeh Shirdar · Mohd. H. Idris (B) ·
S. Izman · D. Almasi · M. M. Taheri
Department of Materials, Manufacturing and Industrial
Engineering, Faculty of Mechanical Engineering,
Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor,
Malaysia
e-mail: hsbullah@fkm.utm.my
M. M. Taheri · M. R. Abdul Kadir
Medical Implant Technology Group (MEDITEG),
Faculty of Bioscience and Medical Engineering,
Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia
1 Introduction
Stainless steel (316L SS) has been used extensively as med-
ical implants due to its biocompatibility, low corrosion rate
and excellent mechanical properties [1]. Corrosion resistance
of 316L-SS is resulted from formation of nano-scale pas-
sive layer which acts as corrosion barrier [2]. Notwithstand-
ing the passivation phenomenon, 316L-SS is prone to corro-
sion in physiological environments. Consequently, mechan-
ical integrity and bio-compatibility of 316L-SS could be
adversely affected by bio-corrosion [3].
Hydroxyapatite (HA; the main inorganic component of
human bone and tooth) has been widely applied as coating
on various biomedical orthopaedic and dental implants to
improve biocompatibility and bioactivity [4]. HA is consid-
ered as an excellent choice for coating metallic implants due
to its excessive bioactivity as well as acting as a pattern for
formation and growth of neighbouring bone tissues [5,6].
As a result, many researchers have studied the advantages of
coating on 316L-SS implants. Coating on passivated surface
of 316L-SS is considered to ensure the biocompatibility and
corrosion resistance [7].
Coating a thin-layer is a process including adsorption,
nucleation and growth of a new phase [8]. In the past few
decades, many coating methods have been employed to
deposit HA on implants’ surface-including plasma spray,
pulsed laser-deposition, sol–gel, biomimetic, pulsed laser-
deposition and electrochemical deposition [9–11]. Elec-
trophoretic Deposition (EPD) technique, compatible with a
broad range of applications, recently attracts great interest to
process advanced materials [12].
Wide range of EPD applications, namely high efficiency,
short processing time, cost effectiveness, basic equipment
and simple set up, prove it as a significant method in materials
processing. EPD is capable of fabricating porous and struc-
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Table 1 Compositions of 316L
Elements C Mn
stainless steel
Composition (%) 0.026 2.107
turally homogeneous coatings on complex implants [13].
Porous coatings are beneficial to successful bio-integration,
being penetrated by bone tissue into a coating [14].
The characteristics of EPD process depends on various
parameters such as the electrical nature of electrodes, the
electrical settings of the coating cells (deposition voltage),
deposition time span and concentration of the suspension.
According to Laxmidhar et al., the mass of the deposited
particles, the thickness of the films can be directly controlled
by the deposition potential, the deposition time span and con-
centration of the suspension [12]. The impact of these para-
meters on crystallization behaviour and corrosion behaviour
needs to be investigated in order to find out optimal sets of
conditions for HA layer deposition with desirable thickness,
morphology, crystallinity and properties [15,16].
Deposition of HA coating on stainless steel and sim-
ilar alloys has been studied by many researchers. Most
researchers have reported their experimental results based on
the effect of one factor (parameter) at one time (OFAT). In
this way, the relationship of each parameter and their inter-
action effect that influences coating mass (Cmass ) and cor-
rosion potential (E corr ) of substrate’s surface could not be
established in the form of mathematical model.
This study aims to evaluate the effects of EPD parame-
ters including deposition voltage and time span on nano-
hydroxyapatite (nano-HA) Cmass and substrates’ E corr . In
addition, to achieve a desirable Cmass and E corr , optimisation
is conducted. Although there are various analysis and opti-
misation methods to investigate similar processes [17,18], in
this study, Response Surface Methodology (RSM) was used
to statistically design the experiments and analyse informa-
tion. The eventual aim of this research is to create an empiri-
cal model to predict the maximum nano-HA Cmass and min-
imum E corr based on a set of EPD parameters.
2 Experimental Details
2.1 Substrate Preparation
316L-SS was cut, from an as-fabricated ϕ10 mm bar, into
discs of 2 mm thickness. Substrates were polished by sand
papers of 320, 600, 800, 1,200 grit to remove of damaged
layer resulted from cutting process. Subsequently, the sub-
strates were ultrasonically cleaned in acetone for 10 min.
Then, the substrates were immersed in 20 % sulphuric acid
(H2 SO4 ) for 1 h at room temperature to produce a passive
layer [19]. Table 1 shows the chemical composition of 316L-
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Arab J Sci Eng
P S Si Cr Ni Mo Fe
0.016 0.031 0.731 17.012 11.978 2.019 Balance
SS, the result was obtained using atomic-absorption spec-
troscopy (AAS).
2.2 Electrophoretic Deposition
EPD was performed by a regulated DC power supply
(LEADERLPS-164A). Substrates were set as the cathode,
and a graphite electrode was used as the anode in a constant
nano-HA concentration. Although the powder in suspension
can be deposited more quickly with higher deposition poten-
tial, but the quality of deposited coating could be deterio-
rated [12].
Therefore, selected deposition voltage and time span were
based on the minimum value that deposition occurs and max-
imum which would not lead to peeling of the coated layer.
The electrolyte was prepared by liquefying 2.5 g. of nano-
HA powder (Sigma Aldrich 677418) in 100 ml ethanol. The
pH of the solution was adjusted to 4.7 by adding nitric acid
(HNO3). Deposition was carried out at room temperature
(25 ◦ C). After EPD, all substrates were dried at room tem-
perature for 24 h. In order to increase bonding strength and
density of the coat as well as reduce surface porosity, the
coated substrates were sintered in a vacuum furnace at 800 ◦ C
for 1 h [20].
2.3 Coating Characterisation
The structures of the deposited layers were analysed using X-
ray diffraction (XRD; Scintag diffractometer), and their mor-
phology was analysed using scanning electron microscopy
(SEM; Jeol JSM-6300 and Hitachi Tabletop SEM TM3000).
The electrochemical test of the coated substrates was per-
formed using the potentiodynamic corrosion test machine
(Parstat-2263). Based on the ASTM Standard (G-5) Simu-
lated Body Fluids (SBF), pH value of 7.4 was used as the
corrosive media and the temperature of the solution was kept
and maintained at 37 ◦ C. The SBF contained 8.045 g/l NaCl,
0.355 g/l NaHcO3 , 0.225 g/l KCl, 0.231 g/l K2 HPO4 .3H2 O,
0.311 g/l MgCl2 .6H2 O, 39 ml 1 M-HCl, 0.292 g/l CaCl2 ,
0.072 g/l Na2 SO4 , and TRIS. Scanning rate was set to 1 mV/s.
To evaluate substrates Cmass , they were weighted by a micro-
weight balance with ±0.0001 g accuracy.
2.4 Experimental Design
Two factors, deposition voltage and time span of EPD were
considered as variable parameters in this study. The low, mid-
Arab J Sci Eng

Table 2 Pre-treatment factor and their levels shows a cross-sectional view of coating. Deposition by 10 V
Parameters Symbol Levels for 30 s, leads to accumulation of nano-HA layer with con-
nected and branched cracks (Fig. 1a). Moreover, the sub-
Low (−1) Centre point (0) High (1)
strate coated by 30 V for 180 s shows micro holes resulted by
Voltage (V) A 10 20 30 high hydrogen evolution due to the high deposition voltage
Coating time (min) B 30 105 180 (Fig. 1b). Hydrogen evolution on the substrates’ surface dur-
ing high deposition voltage EPD coating causes formation
of pits and porosities. During sintering, cracks commence to
Table 3 Experimental plan
grow from the pits caused by high deposition voltage coating
Sample no. Run Voltage (V) Coating [21]. In addition, coarse particles and thick brittle coatings—
time (s)
leading to deep and broad cracks—are deposited during high
1 4 10 30 deposition voltage [22]. It is reported that increasing the
2 14 10 30 Cmass will decrease the adhesion between surface and coated
3 2 30 30 layer and leads to coating peel off [23]. 316L-SS thermal
4 10 30 30 expansion coefficient is 45 % higher than nano-HA, conse-
5 3 10 180 quently, the substrate places high compression stress on the
6 5 10 180 coating after densification. The compression stresses result
7 7 30 180 in cracks on the coating surface [24]. Eventually, based on the
8 11 30 180 morphology of different sintered EPD coatings, represented
9 6 10 105
in Fig. 1, the substrate coated by 20 V and for 105 s seems
to point out a suitable condition to achieve relatively smooth
10 9 30 105
and crack-free coating (Fig. 1c, d).
11 13 20 30
Figure 2 illustrates the XRD pattern of nano-HA coated
12 16 20 180
316L-SS deposited by 20 V, for 105 s and sintered at
13 17 20 105
800 ◦ C. The strongest peaks of nano-HA are detected at
14 12 20 105
26.1◦ , 31.7◦ , 32.4◦ , 33.1◦ , 34.2◦ , 47◦ , and 49.8◦ of 2θ—
15 15 20 105
corresponding to reflections (002), (211), (112), (300), (202),
16 1 20 105
(222) and (213) planes, respectively [25,26]. The presence
17 18 20 105 of the peaks approves the existence of nano-HA. Existence
18 8 20 105 of impurity phase like closed-packed Tetra Calcium Phos-
phate (TCP; Ca3(PO4)2O), detected at 34.4◦ , 25.7◦ , 28.9◦
and 43.8◦ of 2θ, indicates structural transformation in crys-
dle and high levels of these two factors are given in Table 2.
tallinity or stoichiometry [27].
Design of Experiment software was employed for planning
E corr and Cmass of substrates coated by three different
the design of experiments and analysis of data. The Cmass and
deposition voltages and for three different time span are
E corr were investigated with standard RSM design known as
shown in Table 4. In order to find the mathematical rela-
the central composite design (CCD). The factorial portion
tionship between the parameters and responses and also to
is determined as full factorial design with all combination
analyse and optimise the process, these experimental results
of the factors at three levels. Star points are located on the
were imported to the Design Expert software.
faces of the cube in the design with two replicates. The star
points correspond to α-value of 1, and this design is com-
monly referred to as a “face-centred.” The centre points are
3.2 Response Surface Analysis Results
points with all levels set to coded level 0; the midpoint of
each factor range is repeated three times. Table 3 shows the
RSM is a useful mathematical and statistical technique for
experimental plan, eighteen performances, for two factors
modelling and evaluating the effects of factors at differ-
and three levels.
ent levels and the factors interactions. This technique is
applied in an experimental design to provide mathemat-
3 Results and Discussion ical and statistical technique for modelling and analysis
of engineering problems. RSM is considered as a useful
3.1 Experimental Results method when the response is influenced by several vari-
ables. Due to the unknown relationship between response
The surface morphology of substrates after sintering was and independent variables, the first step in RSM is to deter-
analysed by SEM as shown in Fig. 1a–c. Besides, Fig. 1d mine a proper approximation for the true functional rela-

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Fig. 1 SEM images of sintered hydroxyapatite coated on 316 SS, a 10 V—30 s, b 30 V—180 s, c 20 V—105 s, d cross section 20 V—105 s
Fig. 2 XRD of 316SS sintered at 800 (V = 20 V, t = 1 min)
tionship between response “y” and set of independent vari-
ables {x1 , x2 , . . ., xn }. Since the response function is not lin-
ear, the second-order model is employed [28]. Equation 1
demonstrates the mathematical expression of the second-
order model.
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Arab J Sci Eng

k 
k 
k 
k
Y = β0 + βi X i + βii X i2 βi j · X i · X j
i=1 i=1 i i≤1 j
+··· + e (1)
where “i” determines the linear coefficients, “ j” specifies the
quadratic coefficients, “b” represents the regression coeffi-
cients, “k” is the number of experimental factors, and “e” is
the random error.
The stability of regression model is also estimated by
analysis of variance (ANOVA). The “F” value determines
the significance of model using the variance of all of the
terms at an appropriate level, α. In the first step, the proba-
bility of significance, known as the “ p” value, is determined.
The effect of the independent variable is significant if the
p value is equal to or less than the selected a-level, and the
insignificant variables are those with p values greater than
the selected α-level [28]. The number of values in the final
calculation of a statistic that are free to vary is called degree
of freedom (DOF). The null hypothesis tested in the ANOVA
table is that all of the predictor variable coefficients are equal
to zero. The null hypothesis is that there are no coefficients
to be estimated. The alternative hypothesis is that there are
Arab J Sci Eng

Table 4 Experimental results interaction between voltage ad coating time ( AB) and also B 2
Sample Run Voltage Coating Cmass (g) E corr are the significant terms of the model; however, A2 with the
no. (V) time (s) p value of 0.6823 is not significant. Therefore, an improved
model can be obtained by omitting this model term. Table 8
1 4 10 30 0.0082 −0.4657
shows the ANOVA table resulting from the reduced quadratic
2 14 10 30 0.0079 −0.4643
model for Cmass obtained by implementing the backwards
3 2 30 30 0.0173 −0.4117 elimination procedure to automatically reduce the number
4 10 30 30 0.01625 −0.4109 of terms. The model F value of 117.59 reveals that the model
5 3 10 180 0.031 −0.4483 is still significant. The “lack-of-fit F-value” of 0.62 implies
6 5 10 180 0.029 −0.4481 that the lack of fit is not significant relative to the pure error,
7 7 30 180 0.056 −0.3591 and it is desirable. There is a 65.93 % chance that a “lack-of-
8 11 30 180 0.054 −0.3602 fit F-value” this large could occur due to noise.
9 6 10 105 0.015 −0.436 Similarly, the ANOVA table for the second-order model
10 9 30 105 0.026 −0.2846 for the E corr is given in Table 9. The significant model terms
11 13 20 30 0.011 −0.4401 are A, A2 and B 2 based on the values of “Prob > F” <0.050
12 16 20 180 0.0405 −0.3444 as presented in Table 8. However, B and the interaction ( AB)
13 17 20 105 0.02 −0.02226 are not significant. Therefore, an improved model can be
14 12 20 105 0.019 −0.2301 obtained by omitting these model terms. Table 10 shows the
15 15 20 105 0.021 −0.2201 ANOVA table resulting from the reduced quadratic model
16 1 20 105 0.028 −0.2248 for E corr obtained by implementing the backwards elimina-
17 18 20 105 0.018 −0.2268 tion procedure to automatically reduce the number of terms.
18 8 20 105 0.02 −0.2245 However, hierarchical term (B) added after backward elim-
ination regression. The value of R 2 is 0.7865, which is very
close to 1. Likewise, the predicted and adjusted R 2 values are
in close agreement. The S/N ratio, which is presented with
“ p” coefficients to be estimated. Therefore, there are p-0 or adequate precision, is 8.572, and this indicates that the model
p degrees of freedom for testing the null hypothesis. This is desirable for navigating the design space (true when the
accounts for the regression DOF in the ANOVA table. The S/N ratio is >4).
model summary statistics for Cmass and E corr are given in The statistical models play an important role in analysing
Tables 5 and 6, respectively. These two tables reveal that the Cmass and E corr of nano-HA coating of 316L SS. The
the best models both factors are quadratic models. Thus, models are used for the prediction of results. The final
quadratic models were used for proper analysis. improved empirical models in terms of coded and actual
An ANOVA test was applied to provide an optimum com- factors for Cmass and E corr are given in Eqs. 2, 3 and 4, 5,
bination of the pretreatment parameters and consequently of respectively. Coefficients of the individual factors and their
the Cmass and E corr . The response surface quadratic model interactions in the regression model demonstrate how the
resulting from the ANOVA for the Cmass is presented in response changes relative to the intercept. The intercept in
Table 7. The significant model terms are those with a value coded factors is in the centre of our design, while in the actual
<0.050 for “Prob > F”. Voltage (A), coating time (B), the factors, it is usually far from the design space.

Table 5 Model summary

statistics for Cmass Source SD R2 Adj. R 2 Pred. R 2 PRESS

Linear 5.119E−003 0.8792 0.8631 0.8151 6.017E−004

Interaction 4.314E−003 0.9199 0.9028 0.8676 4.309E−004
Quadratic 2.681E−003 0.9735 0.9624 0.9531 1.526E−004 Suggested

Table 6 Model summary

statistics for E corr Source SD R2 Adj. R 2 Pred. R 2 PRESS

Linear 0.12 0.0960 −0.0245 −0.1906 0.30

Interaction 0.13 0.0984 −0.0948 −0.3775 0.35
Quadratic 0.067 0.7889 0.7009 0.6080 0.100 Suggested

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 Arab J Sci Eng

Table 7 ANOVA for the

response surface quadratic Source Sum of squares df Mean square F value p value prob > F
model (coating mass)
Model 3.166E−003 5 6.335E−004 88.14 <0.0001 Significant
A-voltage 6.154E−004 1 6.154E−004 85.63 <0.0001
B-time 2.246E−003 1 2.246E−003 312.42 <0.0001
AB 1.324E−004 1 1.324E−004 18.43 0.0010
A2 1.265E−006 1 1.265E−004 0.18 0.6823
B2 1.075E−004 1 1.075E−004 14.96 0.0022
Residual 8.625E−005 12 6.732E−006
Lack of fit 1.892E−005 3 5.885E−006 0.77 0.5382 Not significant
Pure error 6.860E−005 9 7.622E−006
Cor total 3.254E−003 17
SD 2.681E−003 R2 0.9735
Mean 0.024 Adj R 2 0.9624
C.V. % 11.01 Pred R 2 0.9531
PRESS 1.526E−004 Adeq precision 29.499

Table 8 ANOVA for the

response surface quadratic Source Sum of squares df Mean square F value p value prob > F
model (E corr )
Model 0.20 4 0.040 8.97 0.0010 Significant
A-voltage 0.019 1 0.019 4.25 0.0617
B-time 5.410E−003 1 5.410E−003 1.21 0.2930
AB 6.0773E−004 1 6.073E−004 0.14 0.7190
A2 0.029 1 0.029 6.46 0.0258
B2 0.051 1 0.051 11.45 0.0054
Residual 0.054 13 4.176E−003
Lack of fit 0.020 4 4.972E−003 1.68 0.2396 Not significant
Pure error 0.034 9 3.822E−003
Cor total 0.25 17
SD 0.067 R2 0.7889
Mean −0.33 Adj R 2 0.7009
C.V. % 19.99 Pred R2 0.6080
PRESS 0.100 Adeq precision 7.335

Cmass = 0.021 + 7.845E − 003 A + 0.015B
+ 4.069E − 003AB + 6.240E − 003B 2
(2)
E corr = −0.21 + 0.044 A + 0.023B − 0.097A 2
+8.712E − 003AB − 0.13B 2 (3)
Cmass = 7.82890E − 003 + 2.14875E − 004 A
−1.41660E − 004B + 5.42500E − 006AB
+1.10933E − 006B 2 (4)
E corr = −0.96743 + 0.042987A + 5.10825E − 003B
−9.65710E − 004 A2 − 2.28482E − 005B 2 (5)
Figures 3 and 4 show normal probability plots of residual
in comparison with a function of the predicted responses
for Cmass and E corr , respectively. Considering the plots, the
residuals generally fall on a straight line, implying that the
errors are distributed normally.
The effect of electrophoretic deposition parameters on
Cmass and E corr was also investigated from the developed
RSM-based mathematical model. Figures 5 and 6 show 3D
plots of the Cmass and E corr , respectively. It is obvious that
both have curvilinear profile in accordance to the quadratic
model fitted and indicates that by increasing the deposition
voltage and time span in this EPD process, the Cmass of nano-
HA rise up although the effect of the coating time span is more
significant than that of the deposition voltage.
Nano-HA depositions mass rises with increasing deposi-
tion voltage and time span; however, the slops of rising are
different as time span alternates for various deposition volt-
ages. Increasing deposition time span reduces the slope of

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Arab J Sci Eng

Table 9 ANOVA for reduced

response surface quadratic Source Sum of squares df Mean square F value p value prob > F
model (E corr )
Model 3.166E−003 4 7.916E−004 117.59 <0.0001 Significant
A-voltage 6.154E−004 1 6.154E−004 91.42 <0.0001
B-time 2.246E−003 1 2.246E−003 333.56 <0.0001
AB 1.324E−004 1 1.324E−004 19.67 0.0007
B2 1.731E−004 1 1.731E−004 25.71 0.0002
Residual 8.751E−005 13 6.732E−006
Lack of fit 1.892E−005 4 4.730E−006 0.62 0.6593 Not significant
Pure error 6.860E−005 9 7.622E−006
Cor total 3.254E−003 17
SD 2.595E−003 R2 0.9731
Mean 0.024 Adj R2 0.9648
C.V. % 10.66 Pred R 2 0.9589
PRESS 1.336E−004 Adeq precision 33.390

Table 10 ANOVA for reduced

response surface quadratic Source Sum of squares df Mean square F value p value prob > F
model (E corr )
Model 0.20 4 0.050 11.97 0.0003 Significant
A-voltage 0.019 1 0.019 4.55 0.0525
B-time 5.410E−003 1 5.410E−003 1.30 0.2756
A2 0.029 1 0.029 6.92 0.0207
B2 0.051 1 0.051 12.26 0.0039
Residual 0.054 13 4.176E−003
Lack of fit 0.020 4 4.972E−003 1.30 0.3398 Not significant
Pure error 0.034 9 3.822E−003
Cor total 0.25 17
SD 0.065 R2 0.7865
Mean −0.33 Adj R 2 0.7208
C.V. % 19.32 Pred R 2 0.6123
PRESS 0.099 Adeq precision 8.572

Fig. 3 Normal probability plot

of the residuals for Cmass

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Fig. 4 Normal probability plot
of the residuals for E corr
Fig. 5 Effect of pretreatment
parameters on Cmass , 3D graph
weight gain curve. The phenomena is due to de-concentration
of nano-HA particles in coating emulsion [20]. By increasing
the time span of deposition, the cathode (substrate) is covered
more and more by deposited layer which results in a steep
resistance increase that retards further deposition owing to
current decline [29].
The desirability plot, generally, represents the optimal
region that satisfies the required preset conditions. As it was
mentioned, the main aim of this study is the deposition of
HA coating later onto 316L-SS surface in an optimum EPD
process conditions to minimise ion release of substrate mate-
rial. Therefore, maximum Cmass with a relatively crack-free
coated layer simultaneous with maximum E corr is consid-
ered as desirable conditions. Figure 7 shows the desirability
plot that fulfils these requirements. Figure 7 shows a graph
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Arab J Sci Eng
with graduated colours—cool blue for lower desirability and
green for higher. The optimal setting suggests that these out-
comes can be achieved by varying the deposition voltage to
26 V and coating time span to 159 s, setting the parameters
accordingly, the Cmass and E corr are 0.04147 g. and −0.2649
(V av. SCE), respectively.
3.3 Electrochemical Behaviour
In general, nano-HA coating layer decreases ion release of
implant material. The coated substrates show nobler state
than uncoated one that may be contributed to the more sta-
ble behaviour. Based on Fig. 8a, b, applying high deposition
voltage in constant deposition time span as well as applying
higher deposition time span in constant deposition voltage
Arab J Sci Eng
Fig. 6 Effect of pretreatment
parameters on E corr , 3D graph
Fig. 7 Desirability plot
leads to increasing E corr possibly due to the morphology
and thick coating layer. Increasing the thickness of the nano-
HA layer, in other words, the Cmass improves the E corr of
substrate until the coating cracks. Regarding to Figs. 3b, d,
e and 6, increasing cracks area leads to high ion release.
Cracks initiate from pitting and hydrogen evolution holes in
the coating layer and cause high oxidation process.
3.4 Validation of Experimental Results
The adequacy of both developed regression models are ver-
ified by a series of confirmation test. Four confirmation
experiments were performed. The first two tests are among
the EPD conditions that were performed previously, while
the other two confirmation experiments are conditions that
have not been conducted previously. The predicted and the
experimental values of these four runs are presented in
Tables 11 and 12. The range of error percentage between
the actual and predicted values is, 2.8–5.6 %, for Cmass and
2.1–4.8 % for E corr which indicates that the model can pre-
dict data accurately in the experimental matrix and that there
is an acceptable correlation between the predicted and exper-
imental values.
4 Conclusion
In this study, the effect of two EPD parameters including
deposition time span and voltage on dependent variable such
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Fig. 8 Electrochemical of 316SS after electrophoretic deposition

Table 11 Confirmation experiments for Cmass References

No. V t Actual Cmass Predicted Cmass Residual Error (%)
1. Gao, F.; Sherwood, P.: Photoelectron spectroscopic studies of the
1 10 30 0.0079 0.00835 0.00045 5.6 formation of hydroxyapatite films on 316L stainless steel pretreated
with etidronic acid. Surf. Interface Anal. 44(13), 1587–1600 (2012)
2 30 180 0.0521 0.05401 0.00179 3.4
2. Dhar, S.; Mitra, P.; Duari, B.: Corrosion behaviour of hydroxya-
3 15 60 0.0089 0.01143 0.00253 2.8 patite coatings on borate and phosphate passivated 316L stainless
4 25 120 0.0271 0.02845 0.00130 4.7 steel in Ringer’s solution. Paintindia. 62(6), 63–66 (2012)
3. Rose, A.L., et al.: Mutual influence of sodium dodecyl sulphate and
calcium propionate in biocidal activity and corrosion inhibition of
carbon steel. Arab. J. Sci. Eng. 37(5), 1313–1325 (2012)
Table 12 Confirmation experiments for E corr 4. Sasaki, M., et al.: Formation of hydroxyapatite on nickel-free high-
No. V t Actual E corr Predicted E corr Residual Error (%) nitrogen stainless steel by chemical solution deposition method in
neutral/alkaline solution. Key Eng. Mater. 529, 237–242 (2013)
1 10 30 −0.4843 −0.5014 0.0171 3.5 5. Pourbaghi-Masouleh, M.; Asgharzadeh, H.: Optimization of sol–
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