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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 1 Introduction


on treated medical grade stainless steel 316L by elec-
trophoretic deposition. Two independent variables including Stainless steel (316L SS) has been used extensively as med-
deposition voltage and time span were evaluated in order to ical implants due to its biocompatibility, low corrosion rate
investigate their effect on substrates’ corrosion potential and and excellent mechanical properties [1]. Corrosion resistance
coating mass. After deposition, coated substrates were post- of 316L-SS is resulted from formation of nano-scale pas-
treated in a vacuum furnace at 800 ◦ C. The experimental plan sive layer which acts as corrosion barrier [2]. Notwithstand-
was based on a central composite design to create a precision ing the passivation phenomenon, 316L-SS is prone to corro-
of the mathematical models. The precision of mathematical sion in physiological environments. Consequently, mechan-
model and relative parameters were evaluated by variance ical integrity and bio-compatibility of 316L-SS could be
analysis. Optimum parameters value, considered as simul- adversely affected by bio-corrosion [3].
taneous minimum ion release and maximum coating mass, Hydroxyapatite (HA; the main inorganic component of
were predicted at the deposition voltage of 25.93 V and depo- human bone and tooth) has been widely applied as coating
sition time span of 159 s. The validity of the model generated on various biomedical orthopaedic and dental implants to
by response surface methodology was evaluated by compar- improve biocompatibility and bioactivity [4]. HA is consid-
ing the predicted and experimental results. In addition, close ered as an excellent choice for coating metallic implants due
agreement between experimental and predicted results was to its excessive bioactivity as well as acting as a pattern for
observed. formation and growth of neighbouring bone tissues [5,6].
As a result, many researchers have studied the advantages of
Keywords Electrophoretic deposition · Nano- coating on 316L-SS implants. Coating on passivated surface
hydroxyapatite · 316L SS · Response surface methodology 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
M. Assadian · M. Rezazadeh Shirdar · Mohd. H. Idris (B) · deposit HA on implants’ surface-including plasma spray,
S. Izman · D. Almasi · M. M. Taheri pulsed laser-deposition, sol–gel, biomimetic, pulsed laser-
Department of Materials, Manufacturing and Industrial deposition and electrochemical deposition [9–11]. Elec-
Engineering, Faculty of Mechanical Engineering,
trophoretic Deposition (EPD) technique, compatible with a
Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor,
Malaysia broad range of applications, recently attracts great interest to
e-mail: hsbullah@fkm.utm.my process advanced materials [12].
Wide range of EPD applications, namely high efficiency,
M. M. Taheri · M. R. Abdul Kadir
short processing time, cost effectiveness, basic equipment
Medical Implant Technology Group (MEDITEG),
Faculty of Bioscience and Medical Engineering, and simple set up, prove it as a significant method in materials
Universiti Teknologi Malaysia, 81310 Skudai, Johor, Malaysia processing. EPD is capable of fabricating porous and struc-

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Table 1 Compositions of 316L


Elements C Mn P S Si Cr Ni Mo Fe
stainless steel
Composition (%) 0.026 2.107 0.016 0.031 0.731 17.012 11.978 2.019 Balance

turally homogeneous coatings on complex implants [13]. SS, the result was obtained using atomic-absorption spec-
Porous coatings are beneficial to successful bio-integration, troscopy (AAS).
being penetrated by bone tissue into a coating [14].
The characteristics of EPD process depends on various 2.2 Electrophoretic Deposition
parameters such as the electrical nature of electrodes, the
electrical settings of the coating cells (deposition voltage), EPD was performed by a regulated DC power supply
deposition time span and concentration of the suspension. (LEADERLPS-164A). Substrates were set as the cathode,
According to Laxmidhar et al., the mass of the deposited and a graphite electrode was used as the anode in a constant
particles, the thickness of the films can be directly controlled nano-HA concentration. Although the powder in suspension
by the deposition potential, the deposition time span and con- can be deposited more quickly with higher deposition poten-
centration of the suspension [12]. The impact of these para- tial, but the quality of deposited coating could be deterio-
meters on crystallization behaviour and corrosion behaviour rated [12].
needs to be investigated in order to find out optimal sets of Therefore, selected deposition voltage and time span were
conditions for HA layer deposition with desirable thickness, based on the minimum value that deposition occurs and max-
morphology, crystallinity and properties [15,16]. imum which would not lead to peeling of the coated layer.
Deposition of HA coating on stainless steel and sim- The electrolyte was prepared by liquefying 2.5 g. of nano-
ilar alloys has been studied by many researchers. Most HA powder (Sigma Aldrich 677418) in 100 ml ethanol. The
researchers have reported their experimental results based on pH of the solution was adjusted to 4.7 by adding nitric acid
the effect of one factor (parameter) at one time (OFAT). In (HNO3). Deposition was carried out at room temperature
this way, the relationship of each parameter and their inter- (25 ◦ C). After EPD, all substrates were dried at room tem-
action effect that influences coating mass (Cmass ) and cor- perature for 24 h. In order to increase bonding strength and
rosion potential (E corr ) of substrate’s surface could not be density of the coat as well as reduce surface porosity, the
established in the form of mathematical model. coated substrates were sintered in a vacuum furnace at 800 ◦ C
This study aims to evaluate the effects of EPD parame- for 1 h [20].
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 2.3 Coating Characterisation
is conducted. Although there are various analysis and opti-
misation methods to investigate similar processes [17,18], in The structures of the deposited layers were analysed using X-
this study, Response Surface Methodology (RSM) was used ray diffraction (XRD; Scintag diffractometer), and their mor-
to statistically design the experiments and analyse informa- phology was analysed using scanning electron microscopy
tion. The eventual aim of this research is to create an empiri- (SEM; Jeol JSM-6300 and Hitachi Tabletop SEM TM3000).
cal model to predict the maximum nano-HA Cmass and min- The electrochemical test of the coated substrates was per-
imum E corr based on a set of EPD parameters. 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
2 Experimental Details corrosive media and the temperature of the solution was kept
and maintained at 37 ◦ C. The SBF contained 8.045 g/l NaCl,
2.1 Substrate Preparation 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 ,
316L-SS was cut, from an as-fabricated ϕ10 mm bar, into 0.072 g/l Na2 SO4 , and TRIS. Scanning rate was set to 1 mV/s.
discs of 2 mm thickness. Substrates were polished by sand To evaluate substrates Cmass , they were weighted by a micro-
papers of 320, 600, 800, 1,200 grit to remove of damaged weight balance with ±0.0001 g accuracy.
layer resulted from cutting process. Subsequently, the sub-
strates were ultrasonically cleaned in acetone for 10 min. 2.4 Experimental Design
Then, the substrates were immersed in 20 % sulphuric acid
(H2 SO4 ) for 1 h at room temperature to produce a passive Two factors, deposition voltage and time span of EPD were
layer [19]. Table 1 shows the chemical composition of 316L- considered as variable parameters in this study. The low, mid-

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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


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
Fig. 2 XRD of 316SS sintered at 800 (V = 20 V, t = 1 min) 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
tionship between response “y” and set of independent vari- calculation of a statistic that are free to vary is called degree
ables {x1 , x2 , . . ., xn }. Since the response function is not lin- of freedom (DOF). The null hypothesis tested in the ANOVA
ear, the second-order model is employed [28]. Equation 1 table is that all of the predictor variable coefficients are equal
demonstrates the mathematical expression of the second- to zero. The null hypothesis is that there are no coefficients
order model. to be estimated. The alternative hypothesis is that there are

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

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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 with graduated colours—cool blue for lower desirability and
of nano-HA particles in coating emulsion [20]. By increasing green for higher. The optimal setting suggests that these out-
the time span of deposition, the cathode (substrate) is covered comes can be achieved by varying the deposition voltage to
more and more by deposited layer which results in a steep 26 V and coating time span to 159 s, setting the parameters
resistance increase that retards further deposition owing to accordingly, the Cmass and E corr are 0.04147 g. and −0.2649
current decline [29]. (V av. SCE), respectively.
The desirability plot, generally, represents the optimal
region that satisfies the required preset conditions. As it was 3.3 Electrochemical Behaviour
mentioned, the main aim of this study is the deposition of
HA coating later onto 316L-SS surface in an optimum EPD In general, nano-HA coating layer decreases ion release of
process conditions to minimise ion release of substrate mate- implant material. The coated substrates show nobler state
rial. Therefore, maximum Cmass with a relatively crack-free than uncoated one that may be contributed to the more sta-
coated layer simultaneous with maximum E corr is consid- ble behaviour. Based on Fig. 8a, b, applying high deposition
ered as desirable conditions. Figure 7 shows the desirability voltage in constant deposition time span as well as applying
plot that fulfils these requirements. Figure 7 shows a graph higher deposition time span in constant deposition voltage

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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 the other two confirmation experiments are conditions that
and thick coating layer. Increasing the thickness of the nano- have not been conducted previously. The predicted and the
HA layer, in other words, the Cmass improves the E corr of experimental values of these four runs are presented in
substrate until the coating cracks. Regarding to Figs. 3b, d, Tables 11 and 12. The range of error percentage between
e and 6, increasing cracks area leads to high ion release. the actual and predicted values is, 2.8–5.6 %, for Cmass and
Cracks initiate from pitting and hydrogen evolution holes in 2.1–4.8 % for E corr which indicates that the model can pre-
the coating layer and cause high oxidation process. dict data accurately in the experimental matrix and that there
is an acceptable correlation between the predicted and exper-
imental values.
3.4 Validation of Experimental Results

The adequacy of both developed regression models are ver- 4 Conclusion


ified by a series of confirmation test. Four confirmation
experiments were performed. The first two tests are among In this study, the effect of two EPD parameters including
the EPD conditions that were performed previously, while 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–
gel technique for coating of metallic substrates by hydroxyapatite
2 30 180 −0.3602 −0.3678 0.0076 2.1 using the Taguchi method. Mater. Sci. Pol. 31(3), 424–433 (2013)
3 15 60 −0.3012 −0.3157 0.0145 4.8 6. Sutha, S., et al.: In-vitro bioactivity, biocorrosion and antibac-
4 25 120 −0.223 −0.2123 0.0107 4.7 terial activity of silicon integrated hydroxyapatite/chitosan com-
posite coating on 316L stainless steel implants. Mater. Sci. Eng.
C 33(7), 4046–4054 (2013)
7. Kannan, S.; Balamurugan, A.; Rajeswari, S.: H2 SO4 as a passivat-
ing medium on the localised corrosion resistance of surgical 316L
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