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Optimized Characterization of lubricant with with Titanium Oxide


Nor Syahirah Mohamad 1,2, Salmiah Kasolang 1,2, Mimi Azlina Abu Bakar1,2
Faculty of Mechanical Engineering, Universiti Teknologi MARA,
40450 Shah Alam Selangor,Malaysia.
Tribology Group, Faculty of Mechanical Engineering, Universiti Teknologi MARA,
40450 Shah Alam, Selangor Malaysia
Corresponding e-mail:
Keywords: lubricant, nanoparticles, friction, Box-Behnken design, response surface method

ABSTRACT An optimized model is often deployed to environmental-friendly [27]. Lubricants display

reduce trial and error in experimental approach and significant improvement in the tribological properties
obtain the multi-variant correlation. In this study, when added with nanoparticles. The addition of
Response Surface Methodology (RSM) namely Box- nanoparticles in different shapes, sizes and
Behnken design (BBD) approach has been used to concentrations may affect the level of friction and wear
optimizethe characterization of lubricant with additives. reduction [14].
BBD is based on multivariate analysis whereby the This study examined the tribological effect of TiO 2
effects of different parameters are considered nanoparticles using pin-on-disc tribotester. For
simultaneously. It is a non-linear system which is more optimization purposes, RSM using BBD design was
representative of the actual phenomenon. In this study, deployed in this work. This has enabled simultaneous
the effect of three independent variables namely speed, consideration of many variants.
load and concentration of TiO2 on the coefficient of
friction (COF) has been investigated. Using BBD 2. RESPONSE SURFACE METHODOLOGY
approach, the number of testing has reduced from 100 to The main objective of an optimization model is to
15. The result obtained from BBD has shown that the minimize trial and error in experimental work. Response
most influential parameter was speed followed by Surface Methodology (RSM) is one of the most widely
concentration of TiO2 nanoparticles and then normal used technique for optimization in Design of
load. Analysis of variance (ANOVA) indicated that the Experiment (DOE) concept. The basis for DOE is to
proposed experiments from quadratic model has allow analysis of the interactions between input
successfully interpreted the experimental data with a variables and related output variables for identification
coefficient of determination R2 = 0.9931. From the of the optimal response within the experimental region
contour plot of BBD, the optimization zone for [8, 11, 12].
interacting variables have been obtained. The zone
indicates two regions of lower friction values (<0.04): RSM is based on statistical and mathematical
(i) concentration between 0.5 to 1.0 wt% for a speed technique and a useful method to determine optimum
range of 1000 to 2000 rpm and (ii) load between 17 to operating conditions based on several experiments done
20 kg for a speed in the range of 1200 to 1900 rpm. The [810]. RSM is also defined as a statistical method that
optimized condition shows that the minimum value of deployed quantitative data from experimental work to
CoF (0.0191) is at speed of 1782 rpm, load of 20 kg and establish and resolve multi-variable equations. RSM
TiO2 concentration of 1.0 wt%. allows determination of relationships between several
independent variables (factors) and various responses
1. INTRODUCTION (output). A mathematical model can be produced using
In automotive applications, the conventional Box-Behnken design (BBD). The mathematical model
additives used are antioxidants and extreme pressure is to enable statistical analysis of the relationship
agents (EP) additives such as sulfur, chlorine and between input variables and the output variables.
phosphorus[1]. These EP additives prevent excessive namely coefficient of friction (CoF).
wear by metal-to-metal contact under extreme load.
However, these additives specifically sulphur and 3. METHODOLOGY
chlorine have been restricted due to their environmental The response surface methodology (RSM) was applied
impacts. to get the multiplicity of the self-determining input
Due to recent advancement in nanotechnology, the variables and construct mathematical models.
use of nanoparticles as additive in lubricants provide Mathematical models were established in order to
plausible alternative solution to conventional additives predict the CoF and to conduct a statistical analysis of
with environmental limitation. Nanoparticle additives the independent variables interactions on response
have advantages such as promoting smooth performance surface using Minitab 16.0 statistical software. Three
of engine components and are more remarkable and parameters were regulated: speed (X1), load(X2) and
concentration of TiO2 (X3). The output measured was Equation (1)
the coefficient of friction (CoF).
Using Box-Behnken approach, a set of A good model fit should yield an R 2 of at least 0.8
experimental design was produced as shown in Table 1. [12]. The result indicates that the value of R 2 of 0.9931
In the experimental design, the three parameters (speed, at a confidence level of 0.95. Therefore, it examines that
load and concentration of TiO2) were assigned at the response model performed in this study is highly
different configuration for each run. In total, there are significant.
15 experimental runs. As shown in Table 2, the three The results of ANOVA and estimated regression
parameters chosen for this study were designated as X1, coefficient, illustrated in Tables 3 and 4 respectively,
X2 and X3 and prescribed into three levels, coded +1, 0 clearly prove that the fit with an R2(adj) value of 0.9806 is
and -1 for high, intermediate and low value respectively. satisfactorily effective. On the other hand, the analysis
of variance in Table 3 shows that the p- values for the
Table 1 The BBD matrix design. interaction term is low (0.010), indicating that it is
Run Coded variables Real variables significant. For these results to be consistent, the p-
order x1 x2 x3 X1 X2 X3 value must be less than 0.05 [17].
1 +1 -1 0 1100 15 0.5
2 +1 0 -1 1100 10 0.0
Results of the estimated regression coefficients as
3 -1 0 +1 200 15 0.0
given in Table 4 shows that the p-values of squared
4 +1 0 +1 1100 20 1.0 terms for speed are comparatively low whereas load and
5 +1 +1 0 1100 15 0.5 concentration were comparatively high with 0.063 and
6 0 0 0 2000 20 0.5 0.272 respectively. This suggests that only speed has
7 0 0 0 2000 15 1.0 \significant coefficients for the squared terms indicating
8 -1 -1 0 200 10 0.5 a large effect of speed on the friction coefficient. For the
9 0 -1 -1 200 15 1.0 interaction effects, only the interaction between speed
10 0 +1 +1 1100 15 0.5 and concentration of TiO2 is found significant with p-
11 -1 +1 0 200 20 0.5 value of 0.002.
12 0 0 0 2000 15 0.0
13 -1 -1 -1 1100 10 1.0 Table 3 Analysis of variance (ANOVA) results for
14 0 0 -1 2000 10 0.5 acquired model.
15 0 0 +1 1100 20 0.0 F- P-
Source DF Seq SS Adj SS Adj MS
value value

Regression 9 0.010339 0.010339 0.001149 79.82 0.000

Linear 3 0.007137 0.001991 0.000664 46.10 0.000
Table 2 Experimental level of independent variable
Square 3 0.002679 0.002679 0.000893 62.04 0.000
selected. Interaction 3 0.000523 0.000523 0.000174 12.11 0.010
Variables Symbol Coded levels Lack-of-fit 3 0.000041 0.000041 0.000014 0.90
Uncoded Coded -1 0 +1
Pure Error 2 0.000031 0.000031 0.000015

Speed (rpm) X1 x1 200 1100 2000

Load (kg) X2 x2 10 15 20
Concentration X x3 0 0.5 1
(%wt) Table 4 Estimated Regression Coefficients for CoF of
synthetic oil with TiO2 nanoparticles.
4. RESULT AND DISCUSSION Source Coef SE Coef T-value
The relationship between the response variable
Constant 0.0824438 0.019979 4.126
(CoF) and the three independent variables (speed, load
speed -0.000093 0.000009 -10.744
and concentration of TiO2) are shown in Equation (1). load 0.004997 2.032
The estimated regression model for CoF with uncoded
variables is given by: concentration 0.029238 0.014852 1.969

speed*speed 0.000000 0.000000 13.061

CoF = 0.082438 0.000093 x1 + 0.004997 x2 + load*load -0.000188 0.000079 -2.377

2 2
0.029238 x3 0.000188 x 2 0.009755 x 3 concent.*concent. 0.009755 0.007897 -1.235

speed*load 0.000000 0.000000 0.568

x 1 x 3 0.000305
x2 x3 speed*concentration -0.000025 0.000004 -5.988

load*concentration -0.000305 0.000759

Likewise, the experimental and predicted

friction coefficient (COF) values are observed to display
a very high concurrence among them as shown in Table

Table 5 The BBD Matrix with Observed and

Predicted Values of CoF
Coded variables Response Error
Figure 1 Comparison of predicted and experimental
x1 x2 x3 Experimental Predicted CoF of synthetic oil
1 0 0 0 0.05147 0.05101 0.89
2 0 -1 -1 0.04969 0.05216 4.98
3 -1 0 -1 0.09794 0.09847 0.55
4 0 +1 +1 0.03654 0.03406 6.78
5 0 0 0 0.04689 0.05101 8.79
6 +1 +1 0 0.03849 0.04150 7.83
7 +1 0 +1 0.02806 0.02752 1.92
8 -1 -1 0 0.10787 0.10485 2.80

9 -1 0 +1 0.10650 0.10833 1.73

10 0 0 0 0.05467 0.05101 6.69
11 -1 +1 0 0.09681 0.09745 0.66
12 +1 0 -1 0.06493 0.06309 2.83
13 0 -1 +1 0.03966 0.04083 2.97 Figure 2 Normal plot residuals showing the relationship
between normal probability and residuals.
14 +1 -1 0 0.04524 0.04460 1.41
15 0 +1 -1 0.04962 0.04844 2.37


The relationships between the CoF and these three
independent variables are shown in Figure 3 to 4 . The
5. MODEL ACCURACY CHECK response can be represented graphically, either in the
In order to determine the validity of ANOVA, it is three-dimensional space or as a contour plots that help
important to check accuracy in ANOVA analysis to visualize the shape of response surface. A contour plot
obtain an adequate model. The accuracy of model was is designed by a succession of vertical and horizontal
checked by comparing the predicted and experimental lines. Each contour represents a specific response
of CoF. Figure 1 demonstrates the linear relationship surfaces height. The shape of the surface is illustrated
between the predicted and experimental CoF values with the help of contour plots. Applying Equation (1)
using Equation (1). The results indicated that the CoF of the established empirical model, the response
was distributed relatively near to straight line, and surface and contour plots of CoF are apparent in
sufficient correlation between these values. Figures 3 - Figure 4, as a function of the independent
Furthermore, a normal probability plot of residuals variables.
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, they likely clustered around
blue line indication, which supports claim that the
residual are normally distributed. Thus, our assumption
of normality is valid.


(b) (b)
Figure 3 Effect of speed and concentration of TiO2 on Figure 4 Effect of speed and load on COF at the zero
COF at the zero level: level:
(a) response surface and (b) contour plot (a) response surface and (b) contour plot.

As shown in Figure 3, the CoF decreases as With respect to the load, it is clear that the CoF
speed increases. The region with the lowest friction is increases with increasing load from 10 kg to 18 kg.
indicated by dark blue between 1000 rpm to 2000 rpm However, beyond this load, the CoF begins to reduce. It
and beyond 0.5 by weight percentage of of TiO 2 can be explained that the lubricant film might not
concentration. Generally, high sliding speed may result effectively separate the contact surfaces. Besides that, at
in high interface temperatures that can significantly lower normal load, the contact asperities is smaller
reduce the strength of most materials [18]. There is hence increasing the CoF [22]. As the normal load
always an optimal speed beyond where the properties increases, an oxide layer may have formed on the
and performance of materials start to reduce. Beyond surface due to the elevation of surface contact
the optimal speed, the temperature may reach the temperature and hence provide lubricating action to
melting point causing high adhesion between contact reduce the friction [23]. From observation in Figure 4, it
surfaces and eventually an increase in friction [19]. The can be seen that as speed increases at low normal load,
region with the highest friction is beyond 0.4 wt% of the COF tend to reduce. The dark blue zone represents a
concentration of TiO2 at speed below 250 rpm with 0.10 large region of lower friction values (<0.04) at load
as shown in Figure 3. This is similar to what has been between 17 to 20 kg and a speed range of 1200 to 1900
reported in Ettefaghi et. al [5]. They found that the rpm. At these optimal conditions, the contribution of
concentration of nanoparticles has a great effect on the separation is believed due to the higher speeds causing
functionality of nano-lubricants. A range of 0.1 to 0.5 the distance between interfacial surfaces become far
wt% of concentration was reported as the optimum apart as the duration of asperities compressing each
values in many studies [20, 21]. others is reduced. .


The optimization function in the Minitab software
was used to obtain the optimal conditions for the CoF.
The vertical red lines in the graph refer to the current
factor settings. The numbers displayed on the top of
column represent the current factor level settings.
Besides that, the horizontal blue lines and number
represent the responses for the current factor level. The
results show that the minimum value of CoF was given
at the speed, load, and concentration of TiO 2 of 1782
rpm, 20 kg, and 1.0 wt% respectively. This corresponds
to a CoF value of 0.0191 as shown in Figure 5.


Optimal speed (r load (kg concentr
D High
1.0000 Low 200.0 10.0 0.0 In general, it has been shown that RSM is an effective
and powerful tool in experimental optimization of

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