Materials

& Design
Materials and Design 27 (2006) 10351045
www.elsevier.com/locate/matdes

Application of response surface method for

predicting electroless nickel plating
B. Oraon a, G. Majumdar a, B. Ghosh
b

b,*

a
Department of Mechanical Engineering, Jadavpur University, Kolkata 700 032, India
Advanced Materials and Solar Photovoltaic Division, School of Energy Studies, Jadavpur University, Kolkata 700 032, India

Received 29 September 2004; accepted 28 January 2005

Available online 21 April 2005

Abstract
Electroless nickel plating process has been studied considering pure copper (99.99%) as a substrate material. Deposition per unit
area has been considered as a response variable and individual as well as combined eects of process parameters on deposited mass
have been studied. Regression analysis and Students t test have been used to identify the signicant inuencing process parameters.
It has been observed that reducing agent (NaBH4), source of metal (NiCl2 6H2O) and temperature signicantly aect the deposition. The interactions among various process parameters have also been observed to be signicant. Mathematical modeling has been
carried out by a second-order response surface model with central composite design (CCD) to take into account the eect of curvature in the predicted response. Equations for response surfaces have been determined for various deposition times using MATLAB software package. Most of the response surfaces show that deposition thickness increases with increased values of process
parameters within the adopted range but with dierent rates. The test for reliability for predicting response surface equations shows
that these equations give an excellent tting to the observed values.
 2005 Elsevier Ltd. All rights reserved.
Keywords: Electroless plating; Regression analysis; Response surface; Central composite design; T test; F test

1. Introduction
Metal deposition by aqueous solutions can broadly
be divided into two categories: electrolytic and electroless. In electroless metal deposition process, no external
current supply is required to deposit material on a substrate. Electroless plating is an autocatalytic process
where the substrate develops a potential when it is
dipped in electroless solution called bath which contains
a source metal of metallic ions, reducing agent, stabilizer
and others. Due to the developed potential, both positive and negative ions are attracted towards the sub-

strate surface and release their energy through charge

transfer process. Each process parameter has its specic
role on the process and inuences the process response
variables. Temperature initiates the reaction mechanism
which controls the ionization process in the solution and
charge transfer process from source to substrate. In
addition to this, the substrate is activated before dipping
into the electroless bath and sensitized to initiate the
charge transfer process. The basic chemical reaction
for electroless nickel plating is given by the following
expression [20]:
Rn ! Rnz ze
Mez ze ! Me

Corresponding author. Tel.: +91 33 2414 6823; fax: +91 33 2414

6853.
E-mail address: bghosh3@vsnl.com (B. Ghosh).
0261-3069/$ - see front matter  2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2005.01.025

where R indicates the reducing agent and Me indicates

the metal to be deposited on a substrate.

1036

B. Oraon et al. / Materials and Design 27 (2006) 10351045

Nomenclature
xi
e
bi
bij
bij
bijk
^
b
i
^
b
ij
^
b
ij
^
b
ijk
^
b
E
m
D
^
D
zi
zmax
i
zmin
i
zoi

ith independent variable

an error component
regression coecient of ith independent variable
regression coecient of interaction between
ith and jth independent variables
regression coecient of self interaction of ith
independent variable
regression coecient of interaction between
ith, jth and kth independent variables
estimated value of bi
estimated value bii
estimated value bij
estimated value of bijk
estimated value of regression coecient (bi,
bii, bij or bijk)
mathematical expectation
deposited mass per unit area (g/cm2)
a variable which is m 104 (observed value
for a particular deposition time)
estimated value (for a particular deposition
time)
actual value of ith process parameter
maximum actual value of the ith parameter
minimum actual value of the jth parameter
center point of the design or the basic level ith
parameter

The chemical reactions for electroless nickel deposition with boron compounds are as follows:
NaBH4 4NiCl2 8NaOH
! NaBOH4 8NaCl 4H2 O 4Ni
In strongly alkaline solution (11 6 pH 6 14), the following reactions take place:


4Ni2 BH
4 8OH ! 4Ni BO2 6H2 O

4Ni2 2BH
4 6OH ! 2Ni2 B 6H2 O H2

and also
8NaBH4 10NiCl2 17NaOH 3H2 O ! Ni10 B3
3Ni3 B Ni 5NaBOH4 20NaCl 17:5H2 O
Surface properties, like strength and wear resistance
of pure copper can be improved by internal oxidation
[1], chemical vapor deposition [2,3], electroplating [4]
and many other means [57]. Electroless deposition
has the advantages of simplicity and feasibility over
other processes. The amorphous boron content is intro-

Dzi
ta,t
rb
N
m
Moi
Mesti
Moci
Mavgci
nc
r2res
r2
Fa;t 0 ,t00

l
k
nf

unit or interval of variation on the zi axis for

the ith parameter
value of Students t distribution for a level of
signicance and v degrees of freedom
standard deviation of variabily in regression
coecients
total number of observations = 2k + 2k + nc
number of coecients in the regression equations
observed value of deposited mass per unit
area for ith observation
estimated value of deposited mass per unit
area for ith observation
observed value of deposited mass per unit
area for ith central point
average value of deposited mass per unit area
for the central points
number of central points
residual variance
estimate of error (replication variance)
value of Fishers F-ratio for a level of signicance and t 0 degrees of freedom v00 degrees of
freedom
number of levels
number of factors
number of points used in factorial positions

duced to improve the adherence between coating and

the substrate besides improving properties, like wear
resistance, hardness, corrosion resistance, surface
roughness, etc. [8].
The applications of electroless nickel have been reported in many industries, like petroleum, chemical,
plastics, optics, aerospace, nuclear, electronic, computer, and printing [9] because of its excellent corrosion
and wear resistance properties. There are few exceptions
in the properties of deposits between NiB and NiP.
Deposit characteristics of NiB deposits change with
boron content similar to NiP deposits [10]. The boron
content in NiB electroless nickel coating with borohydride as reducing agent varies between 1% and 10% in
weight [11]. The microstructure of NiB deposits is a
mixture of microcrystalline nickel and amorphous Ni
B phases in the as-deposited condition. The quantity
of amorphous phase increases with boron content [12
15]. The electrical resistivity of these coatings is similar
to that of NiP coatings ranging from 89 lX cm before
heat treatment to 43 lX cm after heat treatment at 1100
C [16].

B. Oraon et al. / Materials and Design 27 (2006) 10351045

The main advantage of electroless NiB coatings is

that these coatings have high hardness and superior
mechanical wear resistance. In the as-deposited condition, microhardness values for borohydride reduced
coatings range from 650 to 750 HV100. After 1 h heat
treatment between 350 and 400 C, hardness values of
about 1200 HV100 can be produced [16]. Long-term heat
treatment for about 3040 weeks between 200 and 300
C can produce hardness between 1700 and 2000
HV100 [15,17]. The study on corrosion rate of NiB
coating has been seen to be greater than that of NiP
coating for as deposited condition [18].
However, the above studies, despite their excellent
contributions, were limited to a discussion about the effect of one particular process parameter at a time on a
particular response. A limited number of literatures
are available which discuss about how the process is affected by individual as well as many combined process
parameters. In order to have better understanding on
the role of individual as well as combined process
parameters, a statistical analysis is essential which relates the response variable with independent process
parameters.
In this study, a boron based reducing agent (NaBH4)
has been used to deposit nickel on a substrate of pure
copper. The nickel boron (NiB) composites are deposited on the basic substrate at various compositions of
nickel salt, reducing agent and temperatures. Other
parameters, like pH of the bath, activation temperature,
bath loading, etc. have been kept constant. In a preliminary study, the eects of individual parameter have
been studied to observe their eects on deposition per
unit area. A statistically designed experiment known
as full factorial design with six additional central points
has been used to collect data for tting a rst-order response surface and test of signicance has been carried
out by t test. Central composite design (CCD) has been
used to collect data for tting the second-order response surface. The computations has been carried
out by using MATLAB software. The predictability
of established response surface equations have been
determined by using Fishers F test, which shows that
the predicting equations are in good agreement with observed data.

2. Response surface method

Response surface method (RSM) adopts both mathematical and statistical techniques which are useful for
the modeling and analysis of problems in which a response of interest is inuenced by several variables.
RSM attempts to analyze the inuence of the independent variables on a specic dependent variable (response). The independent variables denoted by x1,
x2, . . . xk are presumed to be continuous and can be con-

1037

trolled with negligible error. The response (D) is postulated to be a random variable. For two independent
variables x1 and x2, the response D can be represented
as a function of x1 and x2 as follows [19]:
D f x1 ; x2 e;

where e represents an error component.

^
If the expected response is denoted by ED  e D,
^
then the surface represented by D f x1 ; x2 is termed
as the response surface. A second- or higher-order
RSM model is necessary to approximate the surface
around a curvature. In most cases, a second-order
RSM model is adequate which can be represented by
the following equation:
D b0

k
X

bi xi

i1

k
X

bi x2i

k X
k
X
i

i1

bij i < jxi xj e;

2
and the tted equation is represented by
^ ED  e
D
^
b
0

X
i1

^ xi
b
i

k
X

^ x2
b
i i

k X
k
X

i1

^
b
iji<j xi xj :

In this study, 0.1 mm thick copper (99.99% pure) sheets

have been used as the substrate material and deposited
mass per unit area (g/cm2) has been considered as a response variable. From the literature [20], it appears that
metal source, temperature, reducing agent, pH of the
bath, bath loading, etc. aect the deposition. Metal
source (NiCl2 6H2O), reducing agent (NaBH4) and
temperature have been considered as three independent
parameters keeping other parameters as constant. The
bath pH, bath loading and activation temperature have
been kept constant at 12.5, 0.09 and 55 C, respectively.
Depositions have been carried out for dierent time
periods.

3. Experimental procedure and design

3.1. Measurement of deposition
An analytical balance with 0.0001 g resolution has
been used to measure the weight of the specimen before
and after electroless deposition. The deposited mass
(deposition per unit area) has been calculated by the following equation:
m

Md  M0
D  104 g=cm2 ;
A

where M0 and Md represent the weight of the specimen

before and after electroless deposition, respectively, and
A represents the area of deposition. For example, if
M0, Md and A are 0.36 g, 0.3892 g and 4.124 cm2,

1038

B. Oraon et al. / Materials and Design 27 (2006) 10351045

respectively, then m = 70.805 104 g/cm2. Hence, D =

70.805 and in all the subsequent tables, the values of D
have been tabulated. Figs. 1 and 2 show the microstructure and cross sectional views of NiB deposits (taken in
SEM).
3.2. Eect of process parameters on deposition
The bath for electroless nickel plating has been prepared by mixing nickel chloride (NiCl2 6H2O), sodium
borohydride (NaBH4), sodium hydroxide (NaOH), sodium potassium tartrate and distilled water in appropriate sequence. The pH of the bath has been maintained
around 12.5 by adding required amount of NH3 solution (25% solution). In order to reduce the eect of bath
loading, the bath volume has been xed at 50 cm3 and
area of immersion of substrate surface is xed at 4.5
cm2. Hence, bath loading has been kept at 0.09 cm1
(A/V = 4.5/50 = 0.09). The activation temperature has
been kept xed at 55 C. Before placing into the bath
the copper sheets have been cut into appropriate sizes
cleaned by dilute HCl and distilled water. The cleaned
copper sheets have been activated at 55 C temperature
and placed in the bath for deposition.
A series of experiments on electroless nickel plating
have been conducted and it has been observed that
reducing agent, source of metal and temperature are
the important parameters which aect the deposition
signicantly. In some cases, the interactions between
two factors also signicantly aect the deposition. Figs.

Fig. 3. Eect of NaBH4 on deposition.

36 show how the deposition varies with individual process parameters.

From Fig. 3, it can be seen that deposition increases
with time and becomes constant after sometime. It can
also be seen that increase in the concentration of
NaBH4 increases the deposition up to a certain value
(Fig. 4). Further increase in the concentration of
NaBH4 decreases deposition. Fig. 5 indicates that increase in temperature increases deposition and deposition becomes maximum around 7 C. Fig. 6 shows
how bath loading aects the deposition thickness. At
lower bath loading deposition increases rapidly, while

Fig. 1. Microstructure of NiB coated copper (magnication: 3500).

Fig. 2. Cross sectional view of NiB coated copper (magnication: 1000).

B. Oraon et al. / Materials and Design 27 (2006) 10351045

1039

higher value of bath loading decreases deposition

thickness.
3.3. Statistical analysis of process parameters
In order to determine the degree of signicance of
individual process parameters as well as their interactions, an equation which can be considered is given by
the following equation [21]:
D b0 b1 x1 b2 x2 b3 x3 b12 x1 x2 b13 x1 x3
b23 x2 x3 b123 x1 x2 x3 e;

and the corresponding tted equation can be expressed

as follows:
^ ED  e
D
Fig. 4. Eect of NaBH4 concentration on deposition.

^ x1 b
^ x2 b
^ x3 b
^ x1 x2 b
^ x1 x3
^ b
b
0
1
2
3
12
13
^ x2 x3 b
^ x1 x2 x3 :
b
23
123

Table 1 shows the parameter settings for performing

the statistical test on degree of signicance of process
parameters and their interactions. For any factor zi,
the transformation from actual to coded values has been
performed by considering the following equations:
zoi

zmax
zmin
i
i
;
2

Dzoi
Xi

Fig. 5. Eect of temperature on deposition.

zmax
 zmin
i
i
;
2

zi  zoi
:
Dzoi

7
8
9

A full factorial experimental design with six additional central points has been considered for performing the statistical analysis. The six additional central
points give an estimate of experimental error. Table 2
gives the observed data at dierent settings of process
parameters. The data have been collected by conducting
the experiments in a random order of run numbers and
depositions have been carried out for 10, 20 and 30
min.
The observed deposited mass for 10, 20 and 30 min
are denoted by D1, D2 and D3, respectively. The tted
equations for D1, D2 and D3 are as follows:
^ 1 9:5463 1:5063x1 4:3938x2 3:6913x3
D
1:2988x1 x2 0:5163x1 x3 1:4238x2 x3
0:7237x1 x2 x3 ;

10

^ 2 17:4063 2:3513x1 7:0137x2 3:3812x3

D
1:7738x1 x2 0:7012x1 x3 2:2288x2 x3
Fig. 6. Eect of bath loading on deposition.

0:4538x1 x2 x3 ;

11

1040

B. Oraon et al. / Materials and Design 27 (2006) 10351045

Table 1
Symbols, levels and values of process parameters
Process parameters

Symbols

Levels

Actual

Coded

Actual

NiCl2 6H2O (g/100 cm3 distilled water)

NaBH4 (g/100 cm3 distilled water)
Temperature (C)

z1
z2
z3

x1
x2
x3

1.5
0.03
55

Coded
2.0
0.05
60

1
1
1

2.5
0.07
65

0
0
0

+1
+1
+1

Table 2
Observed D-values for dierent settings of process parameters
Coded values of parameters

Deposited mass per unit area (g/cm2) (D 104)

z3

x1

x2

x3

D1 (10 min)

D2 (20 min)

D3 (30 min)

55
55
55
55
65
65
65
65
60
60
60
60
60
60

1
1
1
1
1
1
1
1
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
0
0
0
0

2.47
3.30
7.26
10.39
7.42
7.42
15.01
23.10
10.39
10.89
11.22
11.38
10.39
11.71

8.91
9.57
15.84
21.78
10.72
12.37
24.75
35.31
18.81
20.62
18.15
17.32
17.49
18.64

12.04
14.35
18.31
31.51
13.53
15.18
34.32
55.60
22.60
25.24
24.42
26.23
23.92
26.23

Run No.

Actual values of parameters

z1

z2

1
2
3
4
5
6
7
8
9
10
11
12
13
14

1.5
2.5
1.5
2.5
1.5
2.5
1.5
2.5
2.0
2.0
2.0
2.0
2.0
2.0

0.03
0.03
0.07
0.07
0.03
0.03
0.07
0.07
0.05
0.05
0.05
0.05
0.05
0.05

^ 3 24:355 4:805x1 10:58x2 5:3025x3

D
3:815x1 x2 0:9275x1 x3 4:7225x2 x3
1:0925x1 x2 x3 :

12

The estimated t-values for particular process parameter

can be obtained from the following equation:
testimated

^
jCoefficient of a process parameterj jbj

;
rb
rb
13

been observed that the standard t-values for 1% and 5%

level of signicance and ve degrees of freedom
(v = n  1 = 5) are t0.01;5 = 3.365 and t0.05;5 = 2.015.
From Table 3, it is clear that all the individual eects
are signicant at 1% level of signicance level. The interactions x1 x2 and x2 x3 are also signicant at 1% level of signicance. The interactions x1 x3 and
x1 x2 x3 are also signicant at 5% and 1% level (for
deposition time of 10 min). The interaction x1 x2 x3
is also signicant at 5% level (for deposition time of 30
min).

where
r2b

Estimate of error r2
:
N
N

14

Table 3 gives the t-values for various coecients

and the estimate of errors for dierent deposition
times.
The tests of signicance have been carried out at different levels of signicance using Students t test. It has

4. Mathematical modeling by response surface method

A second-order response surface can be adequately
represented by Eq. (4). In order to t a second-order model,
the experimental design must have at least three levels of
each factor. An experimental design which is rotatable
should be selected. A rotatable experimental design

Table 3
Estimated t-values for process parameters and their interactions
Deposition times (min)

Estimate error

rb

t0

t1

t2

t3

t12

t13

t23

t123

10
20
30

0.29063
1.42898
2.00760

0.19060
0.42264
0.50095

50.1
41.3
48.6

7.9
5.6
9.6

23.0
16.6
21.1

19.4
7.9
10.6

6.8
4.1
7.6

2.71
1.71
1.85

7.47
5.32
9.43

3.78
1.02
2.18

B. Oraon et al. / Materials and Design 27 (2006) 10351045

1041

Table 4
Symbols, levels and values of process parameters for second-order RSM model
Process parameters

Symbols

Levels

Actual

Coded

Actual

NiCl2 6H2O (g/100 cm3 distilled water)

NaBH4 (g/100 cm3 distilled water)
Temperature (C)

z1
z2
z3

x1
x2
x3

2.2
0.06
60

Coded
2.5
0.07
65

1
1
1

2.8
0.08
70

0
0
0

+1
+1
+1

Table 5
Observed data for second-order RSM
Run No.

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Deposited mass per unit area (g/cm2) (D 104)

Actual values of parameters

Coded values of parameters

z1

z2

z3

x1

x2

x3

D1 (10 min)

D2 (20 min)

D3 (30 min)

2.2
2.2
2.2
2.2
2.8
2.8
2.8
2.8
1.995
3.005
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5

0.06
0.06
0.08
0.08
0.06
0.06
0.08
0.08
0.07
0.07
0.053
0.087
0.07
0.07
0.07
0.07
0.07
0.07
0.07
0.07

60
70
60
70
60
70
60
70
65
65
65
65
56.6
73.4
65
65
65
65
65
65

1
1
1
1
+1
+1
+1
+1
1.682
+1.682
0
0
0
0
0
0
0
0
0
0

1
1
+1
+1
1
1
+1
+1
0
0
1.682
+1.682
0
0
0
0
0
0
0
0

1
+1
1
+1
1
+1
1
+1
0
0
0
0
1.682
+1.682
0
0
0
0
0
0

13.03
17.98
13.53
21.12
11.22
17.65
14.19
26.23
19.63
18.97
13.36
19.47
8.91
27.06
16.34
18.81
13.20
14.19
19.63
19.30

23.10
28.21
25.21
36.79
24.91
23.92
25.90
41.25
34.98
34.65
26.07
35.64
22.60
47.19
26.07
25.24
19.80
31.35
32.83
32.67

26.56
46.03
38.28
45.87
36.30
26.23
40.42
50.00
35.47
39.76
29.04
45.04
27.06
52.80
36.79
34.65
31.04
41.25
38.61
43.56

^ at
means that the variance of the predicted response D
some point X is a function only of the distance of the
point from the design center and is not a function of direction. [19]. Any rst-order orthogonal design is rotatable.
The CCD is the most widely used experimental design for
modeling a second-order response surface, A CCD consists of lk factorial or fractional factorial points (usually
coded 1 rotation), augmented by 2k axial points
[(a, 0, 0, . . ., 0), (0, a, 0, . . ., 0), (0, 0, a, . . ., 0), . . ., (0, 0,
. . ., a)] and nc center points [(0, 0, 0,. . ., 0)]. A CCD can
be made rotatable by selecting the appropriate value of
a and for a rotatable CCD, a = (nf)1/4. With proper
choice of nc, the CCD can be made orthogonal or it can
be made uniform precision design. The uniform precision
^ at origin is equal to
design means that the variance of D
^ at a unit distance from the origin. A unithe variance of D
form precision design ensures more protection against
bias in the eoecients than an orthogonal design. Hence,
a CCD with uniform precision has been selected in this
study.
The experiments have been carried out for a bath
loading of 0.09 cm1 (A/V). The pH of the bath
and activation temperature have been kept constant
at 12.5 and 55 C, respectively. The sequence of per-

forming the experiments has been appropriately ramdomized to avoid any bias and to minimize trend
error. For each experiment, six samples, each of size
2 cm 1.5 cm, have been selected for deposition
and each sample has been taken out in every 10
min interval. Table 4 gives the symbols, levels and
values of process parameters for second-order RSM
model. The actual values of the process parameters
have been changed into coded values by using Eqs.
(12)(14).
Table 5 gives the observed data at dierent settings of
process parameters. The data have been collected by
conducting the experiments in a random order of run
numbers and depositions have been carried out for 10,
20 and 30 min.

5. Results and discussion

5.1. Response surfaces and interpretations
The second-order response surface can be given
by Eq. (2) and the tted equation can be written
as Eq. (3). The second-order response surface equa-

1042

B. Oraon et al. / Materials and Design 27 (2006) 10351045

tions have been tted by using MATLAB software

(version 6.1). The coecients of the tted equations
can be obtained from Eq. (15). For example, the Dvalue for 20 min deposition time is denoted by D2.
Hence
1

B XT X XT D2 ;

15

where
h
iT
^ b
^ b
^ b
^ b
^ b
^ b
^ b
^ b
^ b
^
B b
;
0
1
2
3
11
22
33
12
13
23
X x0 x1 x2 x3 x11 x22 x33 x12 x13 x23 ;
x0 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1T ;
x1 1  1  1  1 1 1 1 1
T

 1:682 1:682 0 0 0 0 0 0 0 0 0 0 ;
x2 1  1 1 1  1  1 1 1 0 0

Figs. 79 show the three-dimensional surface as well

^ 2 f x1 ; x2
^ 1 f x1 ; x2 ; D
as contour plots for D
^
and D3 f x1 ; x2 , respectively. All the three gures
indicate that for a constant value of x1, the deposition
increases with increase in the value of x2 and for lower
constant value of x2, deposition decreases with increase in the value of x1 but for higher constant values
of x2 deposition increases with increase in the value of
x 1.
Figs. 1012 show the surface and contour plots for
^ 1 f x1 ; x3 ; D
^ 2 f x1 ; x3 and D
^ 3 f x1 ; x3 , respecD
tively. Here, for a constant value of x1, deposition increases more rapidly with x3 but for 30 min deposition
time and for higher value of x1, deposition decreases
with increase in x3. For constant values of x3, change
in deposition is moderate for 10 and 20 min deposition
times. For higher constant values of x3, deposition
decreases signicantly with increase in x1.
Figs. 1315 give the surface and contour plots for
^ 1 f x2 ; x3 ; D
^ 2 f x2 ; x3 and D
^ 3 f x2 ; x3 , respeD
ctively. These gures show that at lower constant values

 1:682 1:682 0 0 0 0 0 0 0 0 ;
x3 1 1  1 1  1 1  1 1 0 0 0 0
 1:862 1:682 0 0 0 0 0 0T ;
xij Scalar product of column vectors of xi and xj ;
D2 23:10 28:21 25:21 36:79 24:91 23:92 25:90
41:25 34:98 34:65 26:07 35:64 22:60 47:19
26:07 25:24 19:80 31:35 32:83 32:67T :
The experimental results given in Table 5 have
been fed into MATLAB software to establish a set
of second-order response surfaces. The predicted
deposited mass per unit area (D-values) for 10, 20
^ 1; D
^ 2 and D
^ 3,
and 30 min have been denoted by D
respectively, and given by the following response surface equations:

^ 1 f x1 ; x2 .
Fig. 7. Surface and contour plots for D

^ 1 16:9468 0:1845x1 1:8646x2 4:5056x3

D
0:6141x21  0:4057x22 0:1493x23
0:9887x1 x2 0:7412x1 x3 1:0313x2 x3 ;

16

^ 2 28:1596 0:1402x1 3:3172x2 5:2869x3

D
1:3208x21  0:0789x22 1:3491x23
0:9287x1 x2  0:2662x1 x3 2:8262x2 x3 ;

17

^ 3 37:6311 0:2508x1 4:8587x2 5:1152x3

D
0:0907x21  0:1125x22 0:909x23
2:0413x1 x2  3:4437x1 x3 0:9712x2 x3 :

18

^ 2 f x1 ; x2 .
Fig. 8. Surface and contour plots for D

B. Oraon et al. / Materials and Design 27 (2006) 10351045

^ 3 f x1 ; x2 .
Fig. 9. Surface and contour plots for D

^ 1 f x1 ; x3 .
Fig. 10. Surface and contour plots for D

1043

^ 3 f x1 ; x3 .
Fig. 12. Surface and contour plots for D

^ 1 f x2 ; x3 .
Fig. 13. Surface and contour plots for D

^ 2 f x2 ; x2 .
Fig. 14. Surface and contour plots for D
^ 2 f x1 ; x3 .
Fig. 11. Surface and contour plots for D

5.2. The test of reliability for predicting equations

of x2, change in deposition is less when x3 varies. But
with higher constant values of x2, deposition increases
rapidly with increased value in x3 for all 10, 20 and 30
min deposition times.

The test of reliability for the predicting response surface equations has been carried out by Fishers variance
ratio test known as F test. The F-ratio is given by the following equation:

1044

B. Oraon et al. / Materials and Design 27 (2006) 10351045

like dierent mechanical, electrical and electronic properties. Studies on the composition of the deposited material can also be carried out. RSM can also be used for
the characterization of microstructure, grain sizes, surface roughness, etc. may also be interesting area of future study.
7. Conclusion

^ 3 f x2 ; x3 .
Fig. 15. Surface and contour plots for D

Table 6
F test for response surface equations
Predicting
equations

Residual
variance r2res

Replication
variance (r2)

Estimated
F-values

^ 1 f x1 ; x2 ; x3
D
^ 2 f x1 ; x2 ; x3
D
^ 3 f x1 ; x2 ; x3
D

5.2183
27.5218
29.9907

7.6416
26.9880
20.5012

0.6829
1.0198
1.4628

F r2res =r2 ;

19

where
r2res

N
X
2
M oi  M esti =N  m;

20

i1

and
r2

nc
X
2
M oci  M avgci =nc  1:

21

i1

Table 6 gives the values of r2res , r2 and F for the three

predicting equations
^ 1 f x1 ; x2 ; x3 ; D
^ 2 f x1 ; x2 ; x3 and D
^ 3 f x1 ; x2 ; x3 :
D
The upper degrees of freedom (v1 = N  m) and lower
degrees of freedom (v2 = nc  1) are 10 and 5, respectively. The F-values for 1% level of signicance (for
v1 = 10, v2 = 5) are F0.01;10,5 = 10.05. The estimated Fvalues for all the three predicting equations are much
less than 10.05. Hence, it can be concluded that the
established predicting equations give an excellent tting
to observed data.

6. Future scope of the study

RSM is a tool used for optimizing a process response.
Hence, it can be used for optimizing deposition, which
the authors have been carrying out presently. Similar
studies can be carried out for other response variables

Inuence of various process parameters, like source

of metal, reducing agent and temperature on deposited
mass per unit area has been studied for electroless
nickel plating process. Initial studies have been carried
out to observe the inuence of individual process
parameters on deposited mass. It has been observed
that increase in the concentration of reducing agent increases deposition up to a certain value and further increase in concentration of reducing agent decreases the
deposition. Temperature also aects the deposition signicantly and it has been seen that deposition is maximum around 70 C. For lower bath, loading
deposition is signicantly high. A statistical analysis
has been carried out to study individual as well as
combined eects of process parameters on deposited
mass and has been found that all the individual eects
are highly signicant. The interactions x1 x2, x2 x3
and x1 x2 x3 are also highly signicant. Response
surface equations have been determined and threedimensional surface and contour plots for various
deposition times give pictorial views of how deposition
varies with dierent process parameters. The reliability
for predicting equations has been tested by F test,
which indicates that the established response surface
equations are in good agreement with the observed
data.
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