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Chemical Engineering Research and Design

j our nal homepage: www. el sevi er . com/ l ocat e/ cher d

Design of experiments for statistical modeling and

multi-response optimization of nickel electroplating process

Maria Poroch-Seritan

a

, Sonia Gutt

a

, Gheorghe Gutt

a

, Igor Cretescu

b,

,

Corneliu Cojocaru

b,

, Traian Severin

a

a

S tefan cel Mare University of Suceava, Faculty of Food Engineering, 9 Universit atii street, 720225, Suceava, Romania

b

Gheorghe Asachi Technical University of Ias i, Department of Environmental Engineering and Management, 71 Mangeron Blvd.,

700050, Iasi, Romania

a b s t r a c t

The central composite experimental design and response surface methodology have been employed for statistical

modeling and analysis of the results dealing with nickel electroplating process. The empirical models developed in

terms of designvariables (current density J (A/dm

2

), temperature T (

todescribe the process responses, i.e. cathode efciency Y(%), coating thickness U(m), brightness V(%) andhardness

W(HV). The graphical representations consistedof 2Dcontour plots and3Dsurface plots have beenusedfor exploring

and analysis of response surfaces in order to identify the main, quadratic and interaction effects. The multi-response

optimization of nickel electroplating process has been carried out by means of desirability function approach. To

this end, a genetic algorithm has been used for mathematical optimization of the multi-response problem. The

optimization algorithm has conducted to a set of equivalent solutions named Pareto optimal set. The conrmation

runs have been employed in order to make a decision about the optimal solution approved by experiment. Thus,

the optimum conditions of nickel electroplating has been dened in this work as J* =5.35 (A/dm

2

), T* =33.44 (

C) and

pH* =6.22 and respectively the responses conrmed by experiment were Y=79.120.18 (%), U=52.770.48 (m),

V=26.120.45 (%) and W=371.61.77 (HV). In such conditions the quality of nickel electroplating deposit was the

best one in accordance with experimental results.

2010 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Keywords: Electroplating; Experimental design; Response surface method; Desirability function; Genetic algorithm

1. Introduction

Nickel electroplating is used extensively for decorative, engi-

neering and electroforming purposes. Decorative applications

account for about 80% of nickel consumption in plating while

20% is consumed for engineering and electroforming aims (Di

Bari, 2000).

The environmental aspects related to electroplating indus-

try such as waste minimization, toxicity of electroplating

metals and reduction of both chemicals and water con-

sumption have been deeply approached by different authors

(Abou-Elela et al., 1998; Babu et al., 2009; Fang and Chan, 1997;

Kuntay et al., 2006).

E-mail addresses: icre@ch.tuiasi.ro (I. Cretescu), cojocaru c@yahoo.com (C. Cojocaru).

Received24 November 2009; Receivedinrevisedform11 May 2010; Accepted28 May2010

In the last decades, many scientic and technical studies

have been carried out to account for the effects of factors

on electroplating performance and to address the enhance-

ment of nickel electroplating process (Abd El Wahaab et

al., 1986; Dolgikh et al., 2009; Njau et al., 1998; Tsuru et

al., 2002; Hoffmann et al., 2008; Gupta et al., 2002; Yoshida

et al., 2003, 2004; Abdel-Hamid, 1998; Wang et al., 2008;

Shpanko et al., 2004; Badarulzaman et al., 2009; Balakai et

al., 2009; Sotskaya and Dolgikh, 2008; Mohanty et al., 2001;

Ciszewski et al., 2004; Oliveira et al., 2006; Orinakova et al.,

2006). However, it is worth to mention that most of such

investigations dealt with conventional methodology of exper-

imentation in which one factor is varied while others are xed

at constant levels. The classical methods of experimentation

0263-8762/$ see front matter 2010 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

doi:10.1016/j.cherd.2010.05.010

chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147 137

Nomenclature

a

i1

, a

i2

, coefcients for desirability function

b

0

, b

i

, b

ii

, b

ij

regression coefcients for polynomial equa-

tions

b vector of regression coefcients

d individual desirability function

D overall desirability function

D

F ratio of variances (Fischer test)

g population size for GA (integer number)

I current intensity

i and j subscripts (integer variables)

J current density

k iteration indicating the current population in

GA

L number of signicant regression coefcients

m integer number (m<g)

m

p

experimental amount of nickel deposition

m

t

theoretical amount of nickel deposition

n number of variables

n

0

number of experiments in center point

N number of experimental runs in CCD

p level of signicance

R reection (relative percent)

R

s number of responses

S

2

0

error mean square

S

2

res

residual mean square

S

intensity of sample

T temperature

t time of electrolysis

U average thickness of metallic layer (experimen-

tal value)

value)

V brightness of metallic coating (experimental

value)

W hardness of metallic coating (experimental

value)

X matrix of experimental design

x vector of variables (coded values)

x

(k)

cj

chromosome (vector of variables in GA)

x

(k)

pj

parent chromosome (vector of variables in GA)

y response (general term)

y

0i

response recorded in the center point

y

0

average value of response

y predicted values of response

y response vector

Y cathode efciency (experimental value);

sion model);

z actual value of design variable

z

0

center point of design variable (actual value)

z interval of variation for design variable

* superscript indicating optimal value

Greek letters

axial point or star point in CCD;

wavelength

1

,

2

degree of freedoms

valid region (initial region of experimentation)

usually ignore the interaction effects between variables (fac-

tors) and lead to the counterfeit optimal conditions. In order

to overcome this issue the response surface methodology

(RSM) may be used. This methodology (RSM) is a collec-

tion of mathematical and statistical techniques useful for

developing, improving, and optimizing processes that can

be used to assess the relative signicance of several inde-

pendent variables (factors) even in the presence of complex

interactions. According to RSM strategy, the tting of exper-

imental data to a proper response surface model must be

performed based on statistical design of experiments. After-

wards, the developed mathematical model is used to establish

the optimum operational conditions of the process under

investigation.

Few studies related to implementation of experimental

design for nickel plating process have been reported in litera-

ture (Oraon et al., 2006; Hu and Bai, 2001a, 2001b).

Oraon et al. (2006) have applied the response sur-

face method for predicting of electroless nickel plating

process. In this respect, authors have used a central

composite design (CCD) for experimentation. It has been

observed that reducing agent (NaBH

4

), source of metal

(NiCl

2

6H

2

O) and temperature signicantly affect the deposi-

tion.

The authors (Hu and Bai, 2001a) have studied the com-

position control of electroplated nickelphosphorus deposits.

To this end, the inuences of electroplating variables, such

as temperature, current density, pH, NaH

2

PO

2

H

2

O concentra-

tion and agitation rate, on the phosphorus content of NiP

deposits electroplated from a Watts nickel bath modied with

NaH

2

PO

2

H

2

O were systematically compared using fractional

factorial design (FFD).

In addition, the same authors (Hu and Bai, 2001b) have

optimized hydrogen evolving activity on nickelphosphorus

deposits using experimental strategies. In this regard, the

effects of electroplating variables on the hydrogen evolving

activity of NiP deposits were systematically examined using

fractional factorial design (FFD), path of steepest ascent, and

central composite design(CCD) coupledwiththe response sur-

face method (RSM). The FFDstudy indicated that the mainand

interactive effects of temperature, pH, and NaH

2

PO

2

H

2

O con-

centration are the key preparation factors inuencing the NiP

cathode.

The implementation of statistical experimental design

techniques for electroplating process assisted by develop-

ing of empirical models may conduct to an enhanced

electroplating performance and to reduction of overall

costs of experimentation. To the best of our knowledge,

there is a lack of reports in the literature regarding

multi-response optimization of nickel electroplating process.

Therefore, this work deals with statistical modeling and

multi-response optimization of nickel electroplating process

in order to improve the cathode efciency as well as to

obtain the best characteristics of the electroplated covers

in terms of thickness, brightness and hardness of metallic

layer.

138 chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147

Table 1 Chemical composition of Watts-type bath used

for nickel electroplating.

Chemical composition Concentration (g/L)

Nickel chloride, NiCl

2

6H

2

O 40.5

Nickel sulfate, NiSO

4

6H

2

O 292.5

Boric acid, H

3

BO

3

31.5

2. Experimental

Electroplating experiments were carried out using a Watts-

type bath. Details of the bath composition employed are

given in Table 1. All chemicals used in electroplating exper-

iments were of analytical reagent grade. Solution of sodium

hydroxide (0.01N) was used for pH adjustment. The home

made electrochemical cell was employed for nickel electro-

plating experiments. The dimensions of cell are as follows:

13.9cm (length) 12.5cm (width) 10cm (height), correspond-

ing to a volume of 1.75L. In addition, the cell was equipped

with a cathode (made of 99.98% purity copper) and an

anode (made of 99.7% purity nickel). The cathode dimen-

sions are of 8.0cm (height) 9.8cm (length) 0.1cm (width)

while the dimensions of anode were of 10.0cm(height) 4.0cm

(length) 0.3cm (width). The immersion surface of cathode

was of 0.6dm

2

and respectively the anodic immersion sur-

face was of 0.25dm

2

. The above-described cell was connected

in galvanostatic regime to the GWINSTEK GPR-1810HD power

supply, having a digital control of current and voltage.

The temperature of electrolyte solution was kept constant

using the Lauda E100 thermostatic bath. Before each elec-

troplating experiment the cathode surface was prepared

accordingly.

The performance of nickel electroplating process was esti-

mated in terms of four responses, namely, cathode efciency,

Y (%); average thickness of metallic layer, U (m); brightness

of metallic coating, V (%) and hardness of metallic coating, W

(HV).

The cathode efciency, Y (%), was determined by using Eq.

(1):

Y =

m

p

m

t

100 =

m

p

3.041 10

4

I t

(1)

where m

p

denotes the experimental amount of nickel depo-

sition (g); m

t

the theoretical amount of nickel deposition (g);

I the current intensity which cross the electrical circuit (A); t

time of electrolysis (s); 3.04110

4

(g/C) is the electrochemical

equivalent of nickel (Paunovic and Schlesinger, 2006; Popov et

al., 2002).

The thickness of metallic layer was measuredby means of a

PosiTector 6000 DeFesko Analyzer, based on non-destructive

physical method. To this end, seven local values of cathode

thickness were measured in order to determine the average

thickness of metallic layer, U (m).

The brightness of metallic cover V (%) was evaluated using

the HR 4000 CG-UV-NIR spectrometer (Ocean Optics Inc.,

Dunedin, FL) based on the reection property of the deposed

metallic layer. In this respect, the scanning with 0.025nm

resolutionhas beencarriedout for the entire wavelengthspec-

trumranged from200 up to 1100nm. Atungsten halogen light

source (UV-VIS-NIR Light Source DH-2000, Mikropack) was

used for this study. The experimental data were displayed and

stored using the operating software OOI Base32 from Ocean

Optics. The light from Light Source DH-2000 was conveyed to

the sample through an array of optical bers (QR400-7-UV/BX,

Ocean Optics Inc., Dunedin, FL).

The reection was quantied as a relative percent (R)

fromthe reectionof standard reference substance STAN-SSH

(STAN-SSH High-reectivity Specular Reectance Standard,

Ocean Optics Inc.), according to Eq. (2):

R =

S

100% (2)

where S

is the inten-

sity of standard reference substance at wavelength .

The reections were measured at the wavelengths, where

the visual sensibility is maximal one, i.e. 420nm (blue),

534nm (green) and 564nm (yellow), and by considering three

points from the electrode surface. The nal reported value of

brightness V (%) represents the average value of reections

determined based on nine measurements as described previ-

ously.

The hardness of metallic coating, W (HV), was measured

using the Shimadzu, HMV 2T, micro-hardness tester. The

loading weight was of 490.3mN and the load duration of 15s.

3. Results and discussion

3.1. Statistical modeling of electroplating process

The statistical method of experimentation was employed for

modeling and optimization of the electroplating process. The

applying of statistical method is useful to understand the

interaction effects between factors and to reduce the total

number of experimental runs by saving time and adjacent

costs.

The most signicant design variables (key factors) that

inuence the performance of nickel electroplating process

deals with current density, J (A/dm

2

); temperature, T (

C); and

pH value of the solution. The signicance of these factors as

well as their operating range was deduced based on the pre-

liminary experimental tests (not shown in the manuscript).

The importance of each selected factor is discussed briey in

the following.

The current density, J (A/dm

2

), is a key factor for two main

reasons. Firstly, the current density controls the rate of depo-

sition (Rose and Whittington, 2002). Secondly, the current

density must be controlled within the correct operating range

in order to obtain sound deposits having uniform appearance

and free from burning or treeing. For optimum productivity

it will be desirable to operate with the desired current den-

sity and the available current. In practice, the size, shape or

weight of the work may limit the surface area that can be

loaded. In such cases, the current may need to be reduced

to achieve the desired current density. The control of current

density is particularly critical where work is being plated to

a specied thickness and the equipment operates on a xed

time cycle. Thus, in electroplating, current density and its dis-

tribution play a centrally important role in determining the

quality of the nal deposit (Paunovic and Schlesinger, 2006).

Changes in temperature can affect the performance of

nickel plating and other process solutions. Specically, tem-

perature can inuence the brightness range, throwing power,

ductility, hardness, internal stress and burning characteristics

(Di Bari, 2000; Rose and Whittington, 2002).

chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147 139

Table 2 Correspondence between actual and coded values of design variables.

Design variables Symbol Actual values of coded levels Step of variations

1 0 +1 +

J, current density (A/dm

2

) x

1

1.33 1.66 3.33 5 5.36 1.66

T, temperature (

C) x

2

11.77 15 30 45 48.22 15

Solution pH x

3

3.78 4 5 6 6.22 1

The solution pH is a measure of the hydrogen ion concen-

tration, or more simply the acidity, of a solution. In the case

of nickel solutions the pH has an important inuence on bath

performance. The pHcan affect the bright plating range, cath-

ode efciency, effects of impurities, throwing power, stress

as well as the physical properties of the deposit (Rose and

Whittington, 2002).

For statistical calculations the actual values of variables

were scaled-up (coded) according to Eq. (3) (Akhnazarova and

Kafarov, 1982; Myers and Montgomery, 2002):

x

i

=

z

i

z

0

i

z

i

i = 1, n (3)

where z denotes the actual value of design variable; z

0

the

center point of designvariable (actual value); z the interval of

variation; x the coded level of design variable (dimensionless

value) and n is the number of variables. Basically, the extent

of each variable involves three different coded levels from low

(1) to medium (0) and to high (+1). In addition, depending on

the type of experimental design, the axial levels () can be

considered.

The operating region and the levels of the design variables

(key factors) are giveninactual and coded values as it is shown

in Table 2. A central composite design (CCD) of orthogonal

type was employed in this study to perform the electroplating

experiments in a systematically manner by varying simulta-

neously all the factors (Table 3). The axial level (star point)

has been computed from the condition for a CCD to be an

orthogonal design and may be written in this case as fol-

lows (Akhnazarova and Kafarov, 1982; Khuri and Cornell, 1996;

Myers and Montgomery, 2002):

=

_

_

2

n

(2

n

+2n +1) 2

n

2

_

1/2

(4)

According to the experimental design a total number of 16

experimental runs were carried out. The CCDconsists of three

distinct regions: (i) full factorial design in which the factor lev-

els are coded to the usual low (1) and high (+1) values; (ii)

axial points localized on the axis of each variable at a distance

from the designed center; and (iii) center points that can be

replicated to provide an estimation of the experimental error

variance. Four responses have been determined experimen-

tallyinaccordance withdesignedruns inorder toascertainthe

performance of the electroplating process. These responses

are related to cathode efciency, Y (%); average thickness of

metallic layer, U (m); the brightness, V (%) and the hardness,

W (HV) of metallic cover.

Commonly, a quadratic response surface model with cross

terms canbe constructed to t the experimental data obtained

in accordance with CCD. The response surface model (RS-

model), known also as regression or empirical equation,

represents a polynomial approximation of experimental data

and is stated by the following relationship:

y = b

0

+

n

i=1

b

i

x

i

+

n

i=1

b

ii

x

2

i

+

n

i<j

b

ij

x

i

x

j

(5)

where y denotes the predicted response (e.g. predicted cath-

ode efciency), x

i

the coded levels of the design variables, and

b

0

, b

i

, b

ii

, b

ij

are the regression coefcients (offset term, main,

Table 3 Central composite orthogonal design applied for electroplating experiments.

N Design variables Responses (experimental values)

Current density Temperature Solution pH Y (%) U (m) V (%) W (HV)

J (A/dm

2

) x

1

T (

C) x

2

pH x

3

1 5 +1 45 +1 6 +1 100 47.85 24.71 346.00

2 1.66 1 45 +1 6 +1 99.48 35.86 1.99 289.20

3 5 +1 15 1 6 +1 85.56 33.43 17.91 218.10

4 1.66 1 15 1 6 +1 99.10 42.57 21.76 336.00

5 5 +1 45 +1 4 1 99.27 30.29 2.50 228.10

6 1.66 1 45 +1 4 1 99.70 38.86 3.96 237.90

7 5 +1 15 1 4 1 97.05 38.00 9.36 214.00

8 1.66 1 15 1 4 1 98.67 41.43 16.38 273.00

9 5.36 + 30 0 5 0 100 43.57 37.13 343.70

10 1.33 30 0 5 0 98.18 35.86 3.49 271.70

11 3.33 0 48.22 + 5 0 97.07 33.57 4.15 237.10

12 3.33 0 11.77 5 0 99.73 38.29 11.00 211.50

13 3.33 0 30 0 6.22 + 96.99 58.29 15.39 502.90

14 3.33 0 30 0 3.78 100 34.14 25.19 318.40

15 3.33 0 30 0 5 0 99.10 33.71 3.27 248.00

16 3.33 0 30 0 5 0 98.82 34.30 4.20 252.5

140 chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147

Fig. 1 Comparison between experimental data and mathematical models related to cathode efciency Y (%) and brightness

V (%) of metallic layer.

quadratic and interaction or cross effects). The least square

estimations of the regressioncoefcients have beencomputed

by means of ordinary least squares (OLS) method and can be

written as follows (Akhnazarova and Kafarov, 1982; Myers and

Montgomery, 2002; Bezerra et al., 2008):

b =(X

T

X)

1

X

T

y (6)

where b is a vector of regression coefcients, X the design

matrix of the coded levels of input variables, and y is a col-

umn vector of response determined experimentally according

to the arrangement points into CCD.

Based on experimental design results (Table 3) the regres-

sion models have been constructed by means of OLS-method

in order to determine the functional relationship for approx-

imation and prediction of responses. Thus, the second-order

RS-models with coded variables obtained for Ni electroplating

process are as follows:

Y = 97.99 1.174x

1

+1.355x

2

1.297x

3

+1.906x

1

x

2

1.371x

1

x

3

+1.446x

2

x

3

(7)

U = 38.42 +3.695x

3

3.055x

2

2

+3.918x

2

3

+1.999x

1

x

2

+2.249x

2

x

3

(8)

V = 17.2 +4.68x

1

3.704x

2

5.462x

2

2

+4.016x

1

x

2

+3.419x

1

x

3

(9)

W = 299.2 +42.04x

3

72.85x

2

2

+53.49x

2

3

+27.99x

1

x

2

(10)

subjected to: x

i

; ={x

i

|x

i

+}; i = 1, 3

Note that, the term denotes the valid region (region of

experimentation) where the regression models are valid over.

The signicance of regressioncoefcients was testedusing the

statistical Students t-test. Thus, inEqs. (7)(10) only the signif-

icant terms were retained. Figs. 1 and 2 show the comparison

between experimental data and predicted data provided by

regression models.

For testing the goodness-of-t of regression equations, the

statistical Fisher F-test was employed considering the signif-

icance level of p=0.05. In this regard, one must compute the

error mean square and residual mean square. The error mean

square (S

2

0

) that has been calculated by using the repeated

observations (Akhnazarova and Kafarov, 1982; Gavrilescu and

Tudose, 1999):

S

2

0

=

1

n

0

1

n

0

i=1

(y

0i

y

0

)

2

(11)

where n

0

is the number of experiments in center point (repro-

ducibility), y

0i

denotes the values of response recorded in the

center point and y

0

is the average value of y

0i

. The residual

mean square (S

2

res

) has been computed as (Akhnazarova and

Kafarov, 1982; Gavrilescu and Tudose, 1999):

S

2

res

=

1

N L

N

j=1

(y

j

y

j

)

2

(12)

Fig. 2 Comparison between experimental data and mathematical models related to hardness W (HV) and thickness U (m)

of metallic layer.

chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147 141

Table 4 Statistical test for evaluation of model adequacy.

Model Signicant

level

Degrees of

freedom

Fischer test

(calculate value)

Fischer test

(tabulate value)

Model

adequacy

Y (x

1

, x

2

, x

3

) p=0.05

1

= N L = 8

2

= N

0

1 = 1 F

c

=

S

2

conc.

S

2

0

= 215.7 F

tab(p,1,2)

=238.9 F

c

<F

tab(p,1,2)

U (x

1

, x

2

, x

3

) p=0.05

1

= N L = 9

2

= N

0

1 = 1 F

c

=

S

2

conc.

S

2

0

= 236.1 F

tab(p,1,2)

=240.5 F

c

<F

tab(p,1,2)

V (x

1

, x

2

, x

3

) p=0.05

1

= N L = 9

2

= N

0

1 = 1 F

c

=

S

2

conc.

S

2

0

= 214.9 F

tab(p,1,2)

=240.5 F

c

<F

tab(p,1,2)

W (x

1

, x

2

, x

3

) p=0.05

1

= N L = 10

2

= N

0

1 = 1 F

c

=

S

2

conc.

S

2

0

= 213.0 F

tab(p,1,2)

=241.9 F

c

<F

tab(p,1,2)

where N is the number of observations (experimental runs), L

is the number of signicant coefcients inthe regressionequa-

tion, y

j

is the response (experimental value) and y

j

denotes the

predicted values of response according to regressionequation.

Note that, the regression model is an adequate t to the exper-

imental data if the F-ratio is smaller than the tabulated value

one F

tab(p,1,2)

(Akhnazarova and Kafarov, 1982; Gavrilescu and

Tudose, 1999):

F =

S

2

res

S

2

0

< F

tab(p,1,2)

(13)

The results of F-ratio test are focused in Table 4 for all

regression models. According to these results, the F-ratio is

lower than tabulated value in all cases revealing the adequacy

of the regression equations fromstatistical standpoint, i.e. the

models can be used for the predictions.

It is of real interest passing from regression equations with

codedvariables to mathematical models withactual variables.

To this end, the nal empirical models were obtained by sub-

stitution technique and are presented in Eqs. (14)(17):

0.8224J pH +0.0964T pH (14)

2

+3.918pH

2

+0.07994J T +0.1499T pH (15)

2

+0.1606J T +2.051J pH (16)

2

+53.49pH

2

+1.119J T (17)

where J, T and pH are the real values of independent variables

related to current density (A/dm

2

), temperature (

C), and pH

value of solution, respectively. The valid region in actual space

is dened by the following set of constraints:

1.33J 5.36 (current density, A/dm

2

);

11.77T48.22 (temperature,

C);

3.78pH6.22 (pH of solution).

Eqs. (14)(17) have been used for simulation (predictions)

and graphical representations of response surfaces as it is

shown in Figs. 310.

Figs. 3 and 4 show the response surface plot of the cathode

efciency Y (%) as a function of design variables. In addi-

tion to main effects, the interaction effects between factors

are considerable. Thus, at lower values of temperature the

increment of current density J (A/dm

2

) conducts to straight

decreasing of cathode efciency, while for higher tempera-

ture levels the growth of current density leads to slightly

increasing of this response. Concerning the inuence of tem-

perature, the cathode efciency goes up with increasing of

temperature, especially at higher levels of current density.

For low levels of current density the increment of temper-

ature conducts to slightly decreasing of cathode efciency.

The inuence of pH is also affected by interaction effects

between variables. As one can see, the increasing of solu-

tion pH leads to descent of cathode efciency, especially

at higher levels current density. For low values of current

density the inuence of pH becomes insignicantly. There

are no quadratic effects of the factors on cathode efciency

response.

Figs. 5 and 6 illustrate the response surface plots and

contour-lines maps in case of the brightness V (%) of nickel

deposition. Owing to strong quadratic effect, an optimal value

of temperature is observed in the range of 3036

C leading

to the maximum level of the brightness. The increment of

solution pH conducts to improving of the brightness. Due to

the main effect, the increasing of current density leads to

enhancement of the brightness. The improving of brightness

withcurrent density is especially conspicuous at higher values

of temperature.

Response surfaces and contour curves illustrated in

Figs. 7 and 8 highlights the effects of design variables on

performance criterion W (Vickers hardness). In this case, the

increasing of solution pH leads to improving of deposit hard-

ness. Because of strong quadratic effect, the optimum range

of temperature is located in the limits of 3036

C where the

Vickers hardness is the highest. The effect of current density

on hardness is the lowest one if compared with the effects of

other two variables. This effect is due to interaction between

temperature and current density. Thus at low values of tem-

perature, the increment of current density leads to a minor

decrease of the response, W (HV). While at high levels of

temperature the increasing of current density cause a slight

improving of hardness.

In Figs. 9 and 10 are shown the response surfaces related to

the thickness of electroplated layer, U (m). One can observe

that in this case, pH of solution has the greatest inuence on

the response. More precisely, the increment of pH in the range

studied contributes to the evident growth of the thickness U

(m). Due to quadratic effect associated with temperature fac-

tor, there is a ridge-type surface with a maximum visible in

the range of 2040

inated by the effect of interaction. Thus, for low temperature

(<25

of thickness. By contrast, at high levels of temperature (>30

C)

142 chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147

Fig. 3

Y response surface plot and contour-lines map depending on T (

C) and J (A/dm

2

) variables, holding the third

variable at xed level, pH 5.0.

Fig. 4

Y response surface plot and contour-lines map depending on pH and J (A/dm

2

) variables, holding the third variable

at xed level, T=30

C.

the increasing in current density conducts to growth of the

thickness.

3.2. Optimization of electroplating process

The optimization of a process described by two or more

responses, it is helpful to carry out by using the concept

of desirability function. According to this methodology, each

response y

i

must be converted into the individual desirabil-

ity function d

i

that ranges from 0 (very undesirable) to 1 (very

desirable). Such transformation may be presented as follows

(Akhnazarova and Kafarov, 1982):

d

i

( y

i

(x)) = exp[exp((a

i1

+a

i2

y

i

(x)))] i = 1, s (18)

where s is the number of responses involved (in our spe-

cic case s =4); the coefcients a

i1

and a

i2

were calculated by

assigning for two values of y

i

the corresponding two values

of d

i

, preferably in the range 0.2<d

i

<0.8 (Akhnazarova and

Kafarov, 1982).

Afterwards, the individual desirability values are combined

into the overall desirability function, D, which is computed as

Fig. 5

V response surface plot and contour-lines map depending on pH and T (

xed level, J =3.33A/dm

2

.

chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147 143

Fig. 6

V response surface plot and contour-lines map depending on J (A/dm

2

) and T (

variable at xed level, pH 5.0.

Fig. 7

W response surface plot and contour-lines map depending on pH and T (

xed level, J =3.33A/dm

2

.

geometric mean (Derringer and Suich, 1980; Akhnazarova and

Kafarov, 1982; Khayet et al., 2008):

D(x) = [d

1

( y

1

(x)) d

2

( y

2

(x)) d

s

( y

s

(x))]

1/s

(19)

If an individual desirability function is completely unde-

sirable, i.e. d

i

=0 then the value of overall desirability is

nullied. In case of nickel electroplating process discussed in

the present paper, the overall desirability function approach

combines four responses, namely, the cathode efciency,

thickness, brightness and hardness of nickel deposition and

may be written in extended form as follows:

D(x

1

, x

2

, x

3

) = exp{(1/4) [exp((6.731 +0.075

Y(x

1

, x

2

, x

3

)))

+exp((1.495 +0.039

U(x

1

, x

2

, x

3

)))

+exp((0.387 +0.031

V(x

1

, x

2

, x

3

)))

+exp((1.111 +3.71 10

3

W(x

1

, x

2

, x

3

)))]}

(20)

The formulation of multi-response optimization problem

in this case is related to maximization of desirability function

Fig. 8

W response surface plot and contour-lines map depending on J (A/dm

2

) and T (

variable at xed level, pH 5.0.

144 chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147

Fig. 9

U response surface plot and contour-lines map depending on pH and T (

xed level, J =3.33A/dm

2

.

and may be written as:

max

x

D(x)

= max

_

_

d

1

(

Y(x)) d

2

(

U(x)) d

3

(

V(x)) d

4

(

W(x))

1/4

, x

_

(21)

Note, that, the solving of multi-response optimization

problem dened by Eq. (21) involves guring out of a solu-

tion in the design space that satises several specications

(objectives) in the performance space of responses. Usually,

such specications are conicting and there is no simulta-

neous optimal solution for all of them. In this respect, the

solution is not unique; instead there is a set of possible solu-

tions where none is best for all responses. Such set of possible

optimal solutions in the design space is called Pareto optimal

set (Blasco et al., 2008). The Pareto optimality is a condition

when a single response cannot be improved without damag-

ing the qualities of other responses. The region dened by the

responses for all Pareto set points is called the Pareto optimal

front. In fact, the Pareto front supplies a set of solutions where

the designer (decision-maker, experimentalist) has to look for

the best choice according to his preferences. In order to g-

ure out Pareto optimal set, a genetic algorithm (GA) has been

employed for mathematical optimization.

Genetic algorithms (GAs) are a special class of evolutionary

algorithms (EA) that make use of random search techniques

inspired from evolutionary processes in nature (e.g. natural

selection and genetics) (Pasandideh and Niaki, 2006; Hibbert,

1993; Leardi, 2007).

GA involves a series of successive steps (Renner and Ekrt,

2003; Yuan and Qian, 2010; Preechakul and Kheawhom, 2009;

Shopova and Vaklieva-Bancheva, 2006) that are given in the

owchart shown in Fig. 11. The algorithm starts with initial-

ization of the rst population. Thus, it creates a rst current

population {x

(k)

c1

, x

(k)

c2

, . . . , x

(k)

cg

} with g number of individuals

(population size) where k denotes the iteration number also

known as generation. Each individual x

(k)

cj

in the population is

called a chromosome and represents a solution to the prob-

lem. Traditionally, solutions are represented in encoded form

as binary strings of 0s and 1s, but other encodings are also

possible including real code. Each individual in the current

population is evaluated in terms of tness value. Note that,

according to GA terminology the tness function is identical

with the objective function or desirability function in our case.

The tness evaluation of the current population may be noted

as

_

D

_

x

(k)

c1

_

, D

_

x

(k)

c2

_

, . . . , D

_

x

(k)

cg

__

. Afterwards, the termi-

nation criterion is veried. If it is met, the best solution is

then returned. As usually, the termination criterion allows at

most a predened number of iterations and veries whether

an acceptable solution was found (Renner and Ekrt, 2003).

If the termination criterion is not satised, then, some indi-

viduals are selected from the current population based on

the tness values. Such selected individuals are named par-

ent chromosomes

__

x

(k)

p1

_

,

_

x

(k)

p2

_

, . . . ,

_

x

(k)

p(gm)

__

and are used

Fig. 10

U response surface plot and contour-lines map depending on J (A/dm

2

) and T (

variable at xed level, pH 5.0.

chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147 145

Fig. 11 The owchart of the genetic algorithm.

for generation of new chromosomes (offspring) that make

a new population

__

x

(k+1)

c1

_

,

_

x

(k+1)

c2

_

, . . . ,

_

x

(k+1)

cg

__

. To this

end, the genetic operators like reproduction, crossover and muta-

tion are used to generate a new population (Pasandideh and

Niaki, 2006; Hibbert, 1993; Leardi, 2007; Renner and Ekrt,

2003; Yuan and Qian, 2010; Preechakul and Kheawhom, 2009;

Shopova and Vaklieva-Bancheva, 2006). Generally, implemen-

tations of genetic algorithms differ in the mode of constructed

new population. In this work, the population size used in GA

optimizationwas of g =20. Inorder to developnewgenerations

the genetic operators were used in the following proportion:

reproduction (10%), mutation (20%) and crossover (70%).

The results of optimization (Pareto optimal set) given by

GA are displayed in Table 5. The set of optimal solutions

determined by mathematical calculation contains 5 points

(solutions) that are localized on Pareto front. The desirabil-

ity function scores in these points (tness values) are ranged

from 0.509 to 0.529 pointing out that all these points are of

interest. However, selecting a single solution as the optimal

point for process is a matter of decision that depends on spe-

cialist preferences. In this acceptation, the sensitivity analysis

and experimental conrmation plays an essential role.

In our case, the emphasis was placed on the experimental

conrmation of Pareto solutions. After experimental verica-

tion, the best experimental runis the point O3 being denedby

the following values of factors: J* =5.35 (A/dm

2

), T* =33.44 (

C)

and pH* =6.22. In such conditions the quality of nickel electro-

plating deposit (layer) was the best one being superior over the

other points fromPareto optimal set. Note that, for other solu-

tions fromPareto set (i.e. O1, O2, O4 and O5) the electroplating

layers obtained experimentally are of lower quality. More pre-

Table 5 Pareto optimal solutions.

No. Design variables (factors) Responses (performance criteria) Desirable function

Current density Temperature pH

Y

U

V

W D

O1 x

1

=1.211J =5.35A/dm

2

x

2

=0.104T=31.56

C x

3

=1.215pH=6.22 93.537 49.194 27.961 431.96 0.514

O2 x

1

=1.202J =5.34A/dm

2

x

2

=0.806T=42.09

C x

3

=1.215pH=6.22 97.357 50.843 25.174 408.95 0.529

O3 x

1

=1.211J =5.35A/dm

2

x

2

=0.229T=33.44

C x

3

=1.215pH=6.22 94.215 49.712 27.879 433.17 0.520

O4 x

1

=1.211J =5.35A/dm

2

x

2

=0.104T=31.56

C x

3

=1.215pH=6.22 93.537 49.194 27.961 431.96 0.514

O5 x

1

=0.601J =4.34A/dm

2

x

2

=0.408T=36.12

C x

3

=1.169pH=6.17 96.515 49.143 20.979 416.10 0.509

146 chemical engineering research and design 8 9 ( 2 0 1 1 ) 136147

Table 6 Experimental conrmation of optimal solution

O3, J =5.35A/dm

2

, T=33.44

C, pH=6.22.

Y (%) U (m) V (%) W (HV)

Run 1 79.09 52.71 26.10 370.0

Run 2 79.31 52.33 26.57 371.3

Run 3 78.95 53.28 25.68 373.5

Mean value 79.12 52.77 26.12 371.6

S.D. 0.18 0.48 0.45 1.77

cisely, suchlayers were non-uniformand had a week adhesion

to the substrate.

Table 6 shows the experimental values of responses deter-

mined under the conditions given by point O3, i.e. J =5.35

(A/dm

2

), T=33.44 (

were performed in these conditions and the mean values of

responses as well as their standard deviations (S.D.) are also

reported in Table 6. Thus, the optimal solution O3 is described

by the following mean values of responses conrmed exper-

imentally (Table 6): Y=79.120.18 (%), U=52.770.48 (m),

V=26.120.45 (%) and W=371.61.77 (HV). As one can

deduce, the optimal condition conrmed experimentally rep-

resents a compromise between involved responses and have

conducted to a high quality properties of metallic deposition.

All computations were performed using Matlab software as

a tool for scientic programming and technical calculations.

4. Conclusions

In the present work it was demonstrated the applicabil-

ity of experimental design, response surface methodology

and desirability function approach for modeling and multi-

response optimization of nickel electroplating process.

Based on the experimental design results, the second-

order polynomial models were developed for predicting the

electroplating responses (i.e. cathode efciency Y (%), coating

thickness U (m), brightness V (%) and Vickers hardness W

(HV)) as a functional combination of design variables, namely

current density J (A/dm

2

), temperature T (

C) and pH of the

solution. The polynomial models were statistically validated

using F-ratio test. The graphical response surfaces analy-

sis was employed for identication and discussion of main,

quadratic and interaction effects of factors on responses.

A global objective function (desirability function) was

constructed for multi-response optimization. In order to

solve the multi-response problem a genetic algorithm was

employed. The results of optimization offered a set of solu-

tions known as Pareto optimal front. The mathematical

solutions were veried via experimentation and the best

experimental conditions were established. The optimal solu-

tion conrmed by experiment involves the following levels

of factors: J* =5.35 (A/dm

2

), T* =33.44 (

desirable values of responses in these conditions are as fol-

lows: Y=79.120.18 (%), U=52.770.48 (m), V=26.120.45

(%) and W=371.61.77 (HV). As one may conclude, the opti-

mal combination of factors conducted to desirable levels of

responses, and nally to the best characteristics of the elec-

troplated cover.

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