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1. Introduction

In automotive applications, the conventional The response surface methodology (RSM) was applied to get
additives used are antioxidants and extreme pressure agents the multiplicity of the self-determining input variables and
(EP) additives such as sulfur, chlorine and phosphorus (Alves construct mathematical models. Mathematical models were
et al. 2013). These EP additives prevent excessive wear by established in order to predict the CoF and to conduct a
metal-to-metal contact under extreme load. However, these statistical analysis of the independent variables interactions
additives specifically sulphur and chlorine have been on response surface using Minitab 16.0 statistical software.
restricted due to their environmental impacts. Three parameters were regulated: speed (X1), load(X2) and
Due to recent advancement in nanotechnology, the concentration of TiO2 (X3). The output measured was the
use of nanoparticles as additive in lubricants provide coefficient of friction (CoF).
plausible alternative solution to conventional additives with Using Box-Behnken approach, a set of experimental
environmental limitation. Nanoparticle additives have design was produced as shown in Table 1. In the
advantages such as promoting smooth performance of experimental design, the three parameters (speed, load and
engine components and are more remarkable and concentration of TiO2) were assigned at different
environmental-friendly (Wu et al. 2007; Chang et al. 2014; configuration for each run. In total, there are 15 experimental
Jatti & Singh 2015; Ettefaghi et al. 2013; Pisal & Chavan 2014; runs. As shown in Table 2, the three parameters chosen for
Kasolang et al. 2015). Lubricants display significant this study were designated as X1, X2 and X3 and prescribed
improvement in the tribological properties when added with into three levels, coded +1, 0 and -1 for high, intermediate
nanoparticles. The addition of nanoparticles in different and low value respectively.
shapes, sizes and concentrations may affect the level of
friction and wear reduction (Alves et al. 2013; Wu et al. 2007; Table 1 The BBD matrix design.
Chang et al. 2014; Jatti & Singh 2015). Run
Coded variables Real variables
This study examined the tribological effect of TiO2 order x1 x2 x3 X1 X2 X3
nanoparticles using pin-on-disc tribotester. For optimization
purposes, RSM using BBD design was deployed in this work. 1 +1 -1 0 1100 15 0.5
This has enabled simultaneous consideration of many 2 +1 0 -1 1100 10 0.0
variants. 3 -1 0 +1 200 15 0.0
4 +1 0 +1 1100 20 1.0
2. Response Surface Methodology 5 +1 +1 0 1100 15 0.5
6 0 0 0 2000 20 0.5
The main objective of an optimization model is to minimize 7 0 0 0 2000 15 1.0
trial and error in experimental work. Response Surface
8 -1 -1 0 200 10 0.5
Methodology (RSM) is one of the most widely used
9 0 -1 -1 200 15 1.0
technique for optimization in Design of Experiment (DOE)
concept. The basis for DOE is to allow analysis of the 10 0 +1 +1 1100 15 0.5
interactions between input variables and related output 11 -1 +1 0 200 20 0.5
variables for identification of the optimal response within the 12 0 0 0 2000 15 0.0
experimental region (Ahmed et al. 2013; Wu et al. 2012; Qiu 13 -1 -1 -1 1100 10 1.0
et al. 2013). 14 0 0 -1 2000 10 0.5
RSM is based on statistical and mathematical 15 0 0 +1 1100 20 0.0
technique and a useful method to determine optimum
operating conditions based on several experiments done (Wu Table 2 Experimental level of independent variable selected
et al. 2012; Myers et al. n.d.; Abbasi & Mahlooji 2012). RSM is Variables Symbol Coded levels
also defined as a statistical method that deployed Uncoded Coded -1 0 +1
quantitative data from experimental work to establish and
resolve multi-variable equations. RSM allows determination Speed (rpm) X1 x1 200 1100 2000
of relationships between several independent variables Load (kg) X2 x2 10 15 20
(factors) and various responses (output). A mathematical Concentration X x3 0 0.5 1
(%wt)
model can be produced using Box-Behnken design (BBD).
The mathematical model is to enable statistical analysis of the
relationship between input variables and the output variables. 4. Result and Discussion
namely coefficient of friction (CoF).
The relationship between the response variable (CoF) and
3. Methodology the three independent variables (speed, load and
concentration of TiO2) are shown in Equation (1). The
estimated regression model for CoF with uncoded variables is

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given by: speed* -0.000025 0.000004 -5.988 0.002 significant

concentration

load* -0.000305 0.000759 -0.402 0.704 not significant

concentration

CoF = 0.082438 0.000093 x1 + 0.004997 x2 + 0.029238

Likewise, the experimental and predicted friction
x3 0.000188 2 2 0.009755 3 2 0.000025 1 3
coefficient (COF) values are observed to display a very high
0.000305 2 3 Equation (1)
concurrence among them as shown in Table 5.
A good model fit should yield an R2 of at least 0.8 (Qiu et Table 5 The BBD Matrix with Observed and Predicted Values of
al. 2013). The result indicates that the value of R2 of 0.9931 at CoF
a confidence level of 0.95. Therefore, it examines that the Coded variables Response Error
Run
response model performed in this study is highly significant. order x1 x2 x3 Experimental Predicted (%)
The results of ANOVA and estimated regression 1 0 0 0 0.05147 0.05101 0.89
coefficient, illustrated in Tables 3 and 4 respectively, clearly 2 0 -1 -1 0.04969 0.05216 4.98
prove that the fit with an R2(adj) value of 0.9806 is satisfactorily
3 -1 0 -1 0.09794 0.09847 0.55
effective. On the other hand, the analysis of variance in Table
3 shows that the p- values for the interaction term is low
4 0 +1 +1 0.03654 0.03406 6.78

(0.010), indicating that it is significant. For these results to be 5 0 0 0 0.04689 0.05101 8.79

consistent, the p-value must be less than 0.05 (Prakash Maran 6 +1 +1 0 0.03849 0.04150 7.83

et al. 2013). 7 +1 0 +1 0.02806 0.02752 1.92

Results of the estimated regression coefficients as given in 8 -1 -1 0 0.10787 0.10485 2.80
Table 4 shows that the p-values of squared terms for speed 9 -1 0 +1 0.10650 0.10833 1.73
are comparatively low whereas load and concentration were 10 0 0 0 0.05467 0.05101 6.69
comparatively high with 0.063 and 0.272 respectively. This 11 -1 +1 0 0.09681 0.09745 0.66
suggests that only speed has \significant coefficients for the 12 +1 0 -1 0.06493 0.06309 2.83
squared terms indicating a large effect of speed on the
13 0 -1 +1 0.03966 0.04083 2.97
friction coefficient. For the interaction effects, only the
14 +1 -1 0 0.04524 0.04460 1.41
interaction between speed and concentration of TiO2 is found
significant with p- value of 0.002. 15 0 +1 -1 0.04962 0.04844 2.37

Table 3 Analysis of variance (ANOVA) results for acquired model.

Source DF Seq SS Adj SS Adj MS

F- P- 5. Model Accuracy Check
value value

Regression 9 0.010339 0.010339 0.001149 79.82 0.000

In order to determine the validity of ANOVA, it is important
to check accuracy in ANOVA analysis to obtain an adequate
Linear 3 0.007137 0.001991 0.000664 46.10 0.000 model. The accuracy of model was checked by comparing
the predicted and experimental of CoF. Figure 1
Square 3 0.002679 0.002679 0.000893 62.04 0.000
demonstrates the linear relationship between the predicted
Interaction 3 0.000523 0.000523 0.000174 12.11 0.010 and experimental CoF values using Equation (1). The results
indicated that the CoF was distributed relatively near to
Lack-of-fit 3 0.000041 0.000041 0.000014 0.90 straight line, and sufficient correlation between these values.
Pure Error 2 0.000031 0.000031 0.000015 Furthermore, a normal probability plot of residuals to
evaluate the assumptions of populations being sampled are
normally distributed or not. Figure 2 shows the relationship
between normal probability and residuals. From the graph,
Table 4 Estimated Regression Coefficients for CoF of synthetic oil they likely clustered around blue line indication, which
with TiO2 nanoparticles. supports claim that the residual are normally distributed.
Source
Coef
SE Coef
T-
value
p-
value
Characteristics Thus, our assumption of normality is valid.
Constant 0.0824438 0.019979 4.126 0.009 significant
speed -0.000093 0.000009 -10.744 0.000 significant Figure 1 Comparison of predicted and experimental CoF of
load 0.004997 0.002458 2.032 0.098 slightly synthetic oil
significant
concentration 0.029238 0.014852 1.969 0.106 not significant
speed*speed 0.000000 0.000000 13.061 0.000 significant
load*load -0.000188 0.000079 -2.377 0.063 slighty
significant
concentration.* 0.009755 0.007897 -1.235 0.272 not significant
concentration.

speed*load 0.000000 0.000000 0.568 0.595 not significant

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Figure 2 Normal plot residuals showing the relationship between
normal probability and residuals.
6. Response Surface Analysis
The relationships between the CoF and these three
independent variables are shown in Figure 3 to 4 . The
response can be represented graphically, either in the three-
dimensional space or as a contour plots that help visualize
the shape of response surface. A contour plot is designed by
a succession of vertical and horizontal lines. Each contour
represents a specific response surfaces height. The shape of
the surface is illustrated with the help of contour plots.
Applying Equation (1) of the established empirical model,
the response surface and contour plots of CoF are apparent
in Figures 3 - Figure 4, as a function of the independent
variables.
Figure 3 Effect of speed and concentration of TiO2 on COF at the
zero level: (a) response surface and (b) contour plot
(a)
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(b)
As shown in Figure 3, the CoF decreases as speed increases.
The region with the lowest friction is indicated by dark blue
between 1000 rpm to 2000 rpm and beyond 0.5 by weight
percentage of of TiO2 concentration. Generally, high sliding
speed may result in high interface temperatures that can
significantly reduce the strength of most materials
(Chowdhury et al. 2011). There is always an optimal speed
beyond where the properties and performance of materials
start to reduce. Beyond the optimal speed, the temperature
may reach the melting point causing high adhesion between
contact surfaces and eventually an increase in friction
(Chowdhury & Nuruzzaman 2013). The region with the
highest friction is beyond 0.4 wt% of concentration of TiO 2
at speed below 250 rpm with 0.10 as shown in Figure 3. This
is similar to what has been reported in Ettefaghi et. al
(Ettefaghi et al. 2013). They found that the concentration of
nanoparticles has a great effect on the functionality of nano-
lubricants. A range of 0.1 to 0.5 wt% of concentration was
reported as the optimum values in many studies (Sunqing et
al. 1999; Schirru & Dwyer-joyce 2014).
Figure 4 Effect of speed and load on COF at the zero level:
(a) response surface and (b) contour plot.
(a)
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Figure 5 Response Optimization values of COF.

Optimal speed (r load (kg concentr

D High 2000.0 20.0 1.0
Cur [1781.8182] [20.0] [1.0]
1.0000 Low 200.0 10.0 0.0

Composite
Desirability
1.0000

SAE10W40
Minimum
y = 0.0191
d = 1.0000
(b)

With respect to the load, it is clear that the CoF increases with
increasing load from 10 kg to 18 kg. However, beyond this
load, the CoF begins to reduce. It can be explained that the Table 6 Optimum conditions, predicted and experimental value of
lubricant film might not effectively separate the contact COF.
surfaces. Besides that, at lower normal load, the contact
asperities is smaller hence increasing the CoF (Rabinowics
1995). As the normal load increases, an oxide layer may have
formed on the surface due to the elevation of surface contact
temperature and hence provide lubricating action to reduce
the friction (Kathiresan & Sornakumar 2010). From
observation in Figure 4, it can be seen that as speed increases
at low normal load, the COF tend to reduce. The dark blue
zone represents a large region of lower friction values (<0.04)
at load between 17 to 20 kg and a speed range of 1200 to
The corresponding COF from experimental value is 0.0191.
1900 rpm. At these optimal conditions, the contribution of
The experimental and predicted results agree well and this
separation is believed due to the higher speeds causing the
verifies the validity of the model with the percentage error of
distance between interfacial surfaces become far apart as the
5.24%.
duration of asperities compressing each others is reduced. .

7. Optimization Plot Of CoF 8. Conclusion

The optimization function in the Minitab software was Preliminary work has been carried out on the effect of
used to obtain the optimal conditions for the CoF. The vertical
TiO2 nanoparticles on lubricating oil towards friction
red lines in the graph refer to the current factor settings. The
coefficient. RSM has been deployed to optimize the
numbers displayed on the top of column represent the
characterization. Based on the results, the following are
current factor level settings. Besides that, the horizontal blue
observed:
lines and number represent the responses for the current
factor level. The results show that the minimum value of CoF
i) Of the three variables, ANOVA analysis reveals that speed
was given at the speed, load, and concentration of TiO2 of
is the main parameter, which has the greatest influence
1782 rpm, 20 kg, and 1.0 wt% respectively. This corresponds
compared to load and additive concentration. The interaction
to a CoF value of 0.0191 as shown in Figure 5.
of input variables indicates that nanoparticles had influenced
friction values to some extent. Nanoparticles promote a
protective film formation and hence reduce contact between
interfacial surfaces during extreme speed and load
conditions.

ii) The optimization zone for low friction was observed at a

region of optimum concentration of more than 0.5 wt% with
speed in the range of 1000 rpm to 2000 rpm with respect to
the concentration.

iii) The optimization zone for low friction was observed at a

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large region for load between 17 to 20 kg and a speed range
of 1200 to 1900 rpm with respect to load.
iv) The optimal conditions for the CoF reveals that that the
minimum value of CoF (0.0191)was given at the speed, load,
and concentration of TiO2 of 1782 rpm, 20 kg and 1.0 wt%
respectively
In general, it has been shown that RSM is an effective and
powerful tool in experimental optimization of multi-variants.
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Corresponding Author
Salmiah Kasolang can be contacted at:
salmiahk@salam.uitm.edu.my