Materials 15 06520 v2
Materials 15 06520 v2
Article
Response Surface Methodology Based Optimization of Test
Parameter in Glass Fiber Reinforced Polyamide 66 for Dry
Sliding, Tribological Performance
Narendran Jagadeesan 1, *, Anthoniraj Selvaraj 2 , Santhosh Nagaraja 3 , Mohamed Abbas 4,5 ,
C. Ahamed Saleel 6 , Abdul Aabid 7, * and Muneer Baig 7
Abstract: The tribological performance of a glass fiber reinforced polyamide66 (GFRPA66) composite
with varying fiber weight percentage (wt.%) [30 wt.% and 35 wt.%] is investigated in this study using a
pin-on-disc tribometer. GFRPA66 composite specimens in the form of pins with varying percentages
of fiber viz., 30 wt.% and 35 wt.% are fabricated by an injection molding process. Tribological
Citation: Jagadeesan, N.; Selvaraj, A.;
performances, such as coefficient of friction (COF) and the specific wear rate (SWR), are investigated.
Nagaraja, S.; Abbas, M.; Saleel, C.A.;
The factors affecting the wear of GFRPA66 composites [with 30 wt.% and 35 wt.% reinforcements]
Aabid, A.; Baig, M. Response Surface
are identified based on the process parameters such as load, sliding velocity, and sliding distance.
Methodology Based Optimization of
Test Parameter in Glass Fiber
Design Expert 13.0 software is used for the experimental data analysis, based on the design of
Reinforced Polyamide 66 for Dry experiments planned in accordance with the central composite design (CCD) of the response surface
Sliding, Tribological Performance. methodology (RSM) technique. The significance of the obtained results are analyzed using analysis
Materials 2022, 15, 6520. https:// of variance (ANOVA) techniques. To attain minimum SWR and COF, the wear performance is
doi.org/10.3390/ma15196520 optimized in dry sliding conditions. The analysis of experimental data revealed that SWR and COF
increased with increasing load, sliding velocity, and sliding distance for GFRPA66 [30 wt.%], but
Academic Editor: Andrea Petrella
decreased with increasing polyamide weight percentage. The SWR for a maximum load of 80 N,
Received: 4 August 2022 and for a sliding velocity of 0.22 m/s, and a sliding distance of 3500 m for GFRPA66 composite
Accepted: 14 September 2022 specimens with 30 wt.% reinforcements are found to be 0.0121 m3 /Nm, while the SWR for the same
Published: 20 September 2022
set of parameters for GFRPA66 composite specimens with 35 wt.% reinforcements are found to be
Publisher’s Note: MDPI stays neutral 0.0102 m3 /Nm. The COF for the GFRPA66 composite specimens with 30 wt.% reinforcements for the
with regard to jurisdictional claims in above set of parameters is found to be 0.37, while the GFRPA66 composite specimens with 35 wt.%
published maps and institutional affil- reinforcements showed significant improvement in wear performance with a reduction in COF to
iations. 0.25. Finally, using a scanning electron microscope (SEM), the worn surfaces of the GFRPA66 are
examined and interpreted.
have significant advantages such as a low friction coefficient without external lubrica-
tion, improved abrasion, corrosion, and wear resistance, low density, and suitability for
mass production [1]. Nowadays, many tribological applications are using polyamide and
polyamide composites as a better alternative to metallic parts in the manufacturing of the
mechanical parts. Weight, cost, and ease of manufacturing are also often considered as
additional benefits for using polyamides in composites [2].
Polyamide has a highly ordered (semi-crystalline) molecular structure, a hydrogen
bond, and superior wear and mechanical properties due to its semi-crystalline nature [3,4].
Understanding wear mechanism and behavior under different sliding conditions is critical
when using polyamide and polyamide composites for sliding applications [5]. Moreover,
the adhesion mechanism of friction of polymer occurs due to the breakage of weak bonds
between polymer pin and steel disc. Similarly, dissipation of energy in the contact area
of the deformation mechanism is a major challenge [6–8]. The nylon gears and bearings
possess hydrogen bond and the Van der Waals force present in the molecular chains resist
the wear [9,10]. The transfer layer protects wear loss of material, and this is controlled by
adhesion and cohesion of the transfer film. The wear loss of disc depends on the transfer
layer formation and surface degradation occurs due to the loss of transfer layer [11].
The need to withstand the environmental degradations and higher stress are also the
major concerns for plastic parts in current scenario [12–14]. To overcome the above chal-
lenges, mechanical and tribological properties such as tensile strengths, Young’s modulus
of polyamide and bending strength needs to be improved by using fillers such as glass
fiber, MoS2 (Molybdenum disulfide), and carbon fiber in a polymer matrix [15–18]. On the
other hand, while improving mechanical and tribological properties, several properties
tend to decrease, owing to the improper distribution of reinforcements in the matrix phase.
Hence, there is a need for filler material. The filler may be affected by fiber reinforcement.
The filler material used depends on the matrix, size, shape and type of the reinforcement.
The tribological characteristics of such composites mainly depends on wear conditions.
Polyamide 66 (PA66) is preferred due to its economy, maximum wear resistance,
better strength, thermal properties, and capability to absorb energy and plastically deform
without fracturing [19,20]. For ultimate properties, PA66 is used in food and chemical
industry, at the same time it is used for betterment of tribological properties facilitating their
use in components such as gears, bearings etc. [21–24], and also polyamide has inherent
lubrication property as added advantage [25]. Many researchers have explained the effect
of adding glass fiber as a reinforcement material to PA66 for enhancing its wear behavior
The reinforcement material, such as glass fiber, increases wear resistance and generates a
transfer film between the polyamide pin and steel disc during surface contact, as well as it
acts as a self-lubricant [26].The wear behavior of polyamide 66 and polyamide composites
with 10, 20, and 30 wt.% glass fiber addition have been studied. The results show an increase
in wear resistance with an increase in weight percentage [27]. The ultimate strength, flexural
strength, and elastic modulus all increase as the weight fraction of glass fiber increases [28].
As a result, the deformation mechanism of polymer should be considered while using
fiber reinforced material. The deformation mechanism mainly depends on tribological
properties. At low load and low sliding speeds, the coefficient of friction and wear becomes
high, but as the load increases within the elastic limit, the friction coefficient decreases. With
a further increase in the load beyond the elastic limit, the friction coefficient may increase
due to the increase in the plastic deformation [29]. However, the tribological properties are
found to be lower while using a glass fiber reinforced polymer composite with 30 weight %
glass fiber and 6 wt.% nylon (30 wt.% GFR and 6 wt.% nylon) [30].
Also, several studies have focused on the optimization of the reinforcement percentage
using statistical methods. The best statistical method such as design of experiments (DoE)
for determining a specific quality characteristic of a result by using a large number of
variables is an important technique for optimization studies. DoE consists of arrangement
of variables, experiments, performance, evaluation, experiments controlled by a set of
data facilitating the reduction in the number of experimental trials [31]. This supports the
Materials 2022, 15, 6520 3 of 16
primary goal of the current study, which is to investigate the effect of process parameters
and condition optimization using RSM for optimizing the tribological performance of
polyamide. This fosters the objective of the optimization of process parameters such as
load, temperature, weight percentage of reinforcement, sliding velocity, sliding distance,
and etc., especially using the response surface methodology (RSM) [32]. To optimize the
process variables for tribological performance, the central composite design (CCD) is used,
and the results of the experiments are scientifically tabulated. The influence of process
parameters of polyamide with varying weight percentages are identified and also the
number of trials is reduced via RSM to improve the tribological performance [33–37]. Also,
several related studies on the optimization of process variables using the RSM approach
for improving the tribological performance in polyamide has been studied and adopted for
the present work [38–51].
This study focuses on coefficient of friction (COF) and the specific wear rate (SWR) of
PA66 composite with 30 wt.% and 35 wt.% glass fiber against a very high strength alloy
steel (EN31) disc. The glass fiber reinforced polyamide 66 composite with 30 and 35 wt.%
reinforcement has been preferred due to superior mechanical properties such as increased
strength, rigidity, creep strength, and dimensional stability [52–56]. When compared to
unreinforced PA66, the properties of the glass filled composites make it suitable for use
in parts subjected to high static loads for extended periods of time in high temperature
conditions [57–61]. The following assumptions are considered for investigation: (1) while
increasing the weight percentage of glass fiber, the COF and SWR decreases; (2) if the load,
sliding velocity and sliding distance is increased, the transfer film in the specimen is not
affected by contact surface temperature; (3) if the weight of glass fiber increases it may
increase elastic modulus and ultimate strength of glass fiber. Finally, a study was conducted
to analyze the optimized conditions in order to determine the tribological performance of
polyamide and also results are validated by RSM.
Figure 1. (a) GFRPA66 30 wt.% pin, (b) GFRPA66 35 wt.% pin, and (c) EN31 steel disc.
Materials 2022, 15, 6520 4 of 16
3. Experimental Design
3.1. Friction and Wear Analysis
The COF and SWR of GFRPA66 with 30 wt.% and 35 wt.% reinforcements are studied
under dry conditions by using pin-on-disc tribometer (DUCOM make) which is as shown
in Figure 2. The input parameters for tribological tests are load (60, 70, and 80 N), sliding
velocity (0.16, 0.19, and 0.22 m/s) and sliding distance (2500, 3000, and 3500 m). The
experiments are conducted with constant room temperature under dry sliding conditions.
Before conducting the test, the disc was cleaned by acetone and surface of the pins were
polished using emery paper (320 and 600 grit sizes) [48]. Subsequently, the friction force
was measured, and the data were recorded during the experiment by using transducer. The
mass losses of the pin were measured by using micro weighing balance with an accuracy
of 0.0001 mg. The mass loss was determined by measuring the mass of the specimen before
and after the experiment.
β = f (A, B, C) (1)
factor is further divided into three levels: low, medium, and high. Experiments are car-
ried out for at least three levels of each factor, with the levels being equally spaced, in
order to develop a quadratic model. Table 1 displays the actual values of the factors
as well as their coded levels. The optimization of process variables in RSM consists of
seven distinct steps. The steps are as follows: (1) response selection (COF/SWR mini-
mize), (2) variable selection and assignment of codes, (3) development of experimental
design for minimizing the tribological properties, i.e., COF/SWR, (4) analysis of regression,
(5) response development i.e., quadratic polynomial formation, (6) development of a 2D
contour plot or 3D surface of the observed response surface, and finally (7) analysis of the
optimum operating conditions. The experimentations on given optimal standard settings
is used to validate the mathematical model generated by the RSM approach. The various
statistical parameters are validated by statistical t-test such as R2 (coefficient of determina-
tion), R2 adj (adjusted R2 ) and R2 pred (predicted R2 ). Table 1 gives the process parameters
and their levels, adopted in the present investigation.
Factor Levels
Parameters
−1 0 +1
Load (N) 60 70 80
Sliding Velocity (m/s) 0.16 0.19 0.22
Sliding Distance (m) 2500 3000 3500
Figure 3. Effect of glass fiber content on COF at varying loads, sliding velocities, and sliding distances.
Materials 2022, 15, 6520 6 of 16
In the case of GFRPA66 with 35 wt.% reinforcement, the COF decreases under all
load and sliding velocity conditions attributed to the transition in material’s behavior from
ductile to fragile [29,46,47]. As the glass fiber weight increases in the matrix, the glass
fiber carries all of the friction load and the transfer film available on specimen surface
maintains relatively lesser temperature between pin and steel disc surface. From the result
it is revealed that the COF of GFRPA66 with 35 wt.% is low as compared with GFRPA66
with 30 wt.% reinforcements, since it has better transfer layer formation, increased adhesion
of PA66, and low abrasion by glass fiber with less temperature between the contact surfaces.
Also the elastic modulus and ultimate strength of glass fiber improve as the weight of glass
fiber increases [70–73].
4.2. Effect of Applied Load, Sliding Velocity and Sliding Distance with Constant Glass Fiber
Content 30% and 35% Weight on SWR
Figure 4 shows the SWR variation with glass fiber content such as 30 wt.% and
35 wt.% reinforcements at different loads, sliding velocities, and sliding distances. From
the graph, the SWR of GFRPA66 with 30 wt.% reinforcement range from 0.0120 m3 /Nm to
0.0164 m3 /Nm. Similarly, the SWR of GFRPA66 with 35 wt.% range from 0.0101 m3 /Nm
to 0.0161 m3 /Nm. In the case of GFRPA66 with 35 wt.%, the SWR has decreased due to the
increase in glass fiber content. The SWR also increased due to the increase in load, sliding
velocity and sliding distance in the case of GFRPA 66 with 30 wt.% reinforcement due to
stronger contact between the surfaces (such as between the pin and rotating disc) [74–78].
From this contact, more heat was developed between the surfaces by visco-elastic property
and SWR also increased. T Trzepiecinski et al., have also iterated the significance of
studying the basic concepts related to the material losses in polymer based composite
materials and have reported that the heating effect is also an important factor in analyzing
the material removal process, especially for the aerospace applications [79,80].
Figure 4. Effect of glass fiber content on SWR at varying loads, sliding velocity, and sliding distance.
Also, when the fiber peels out by removal of transfer layer in GFRPA66 30 wt.%
after an increase in the load, sliding velocity, and sliding distance, greater contact occurs
between the two relatively hard surfaces (EN31 steel and peeled glass fiber) resulting in
severe abrasive friction. In case of GFRPA66 35 wt.%, the fiber reinforcement does not
peel out as the transfer film is retained even at increased load, sliding velocity and sliding
distance, thereby resulting in contact between a hard surface (EN31 steel) and another
relatively soft (polymer) material, which corresponds to a soft abrasive friction mechanism,
and a lesser SWR.
Materials 2022, 15, 6520 7 of 16
Table 2. ANOVA table of COF for GFRPA66 30 wt.% and GFRPA66 35 wt.%.
Table 3. ANOVA table of SWR for GFRPA66 30 wt.% and GFRPA66 35 wt.%.
Large F values can occur due to noise, with a 0.01% chance. The “Prob > F” values
are less than 0.0500, indicating that both model terms are significant. Model terms for
GFRPA66 30 wt.%—A, B, C, AC, A2 , B2 , C2 and GFRPA66 35 wt.%—A, B, C, AC, B2 , C2
are found to be significant for COF, respectively. In the case of SWR also, model term
for GFRPA66 30 wt.%—A, B, C, AB, C2 and GFRPA66 35 wt.%—B, C, AB, AC, BC, B2 ,
respectively, are found to be significant. “p values” for all of the models were remarked
to be <0.001, representing the significance level of developed models. The model terms
are insignificant if the p-values are greater than 0.10. In addition to p value, the ability of
developed models is evaluated using other statistical parameters such as R2 (coefficient of
determination), R2 adj (adjusted R2 ), R2 pred (predicted R2 ), CV (coefficient of variation), etc.
The R2 analysis for COF for GFRPA66 30 wt.% (R2 values-0.9886 and R2 adj −0.9783) and
COF—GFRPA66 35 wt.% (R2 values—0.9757 and R2 adj −0.9538) are greater than 0.9 which
ascertains its validity. In the case of SWR, R2 values for GFRPA66 30 wt.% (R2 = 0.9999 and
R2 adj. = 0.9999) and GFRPA66 35 wt.% (R2 = 0.9778 and R2 adj. = 0.9578) are having a value
closer to 1. Both the models’ standard deviations (SD) are found to be small (i.e., the SD
for GFRPA66 30 wt.% (COF-0.0048. and SWR-0.0001) and GFRPA66 35 wt.% (COF-0.0252
and SWR-0.0069)) are very minimal. The adjusted R2 value is very close to the predicted R2
value and models are statistically accurate.
To fit the experimental outcomes attained from the design, several iterative are runs
performed in connection with the arranged CCD, the response designs are subsequently
modified. This resulted in a coded equation. Where, A, B, and C represent load, sliding
velocity and sliding distance. Consequently, the response (i.e., minimum COF and SWR
for GFRPA66 30 wt.% and GFRPA66 35 wt.% was calculated using Equations (3)–(6),
respectively) [33–37,50].
(COF)GFRPA66 30 wt.% = +0.2866 + 0.0127 A+0.0196 B + 0.0130 C + 0.0238 AC + 0.0105 A2 + 0.0105 B2 − 0.0124 C2 (3)
(COF)GFRPA66 35 wt.% = +0.2646 + 0.0613 A + 0.0524 B+0.0916 C + 0.0687AC + 0.0639B2 − 0.0249 C2 (4)
(SWR)GFRPA6635 wt.% = +0.0186 − 0.0049B − 0.0056C + 0.0216 AB − 0.0205 AC − 0.0152BC + 0.0252 B2 (6)
Materials 2022, 15, 6520 9 of 16
The relationship between actual values of COF for GFRPA66 30 wt.% and GFRPA66
35 wt.% and SWR for GFRPA66 30 wt.% and GFRPA66 35 wt.% and the measured responses
depicted by CCD, are as shown in Figure 5a–d, and by using the estimated function values
for model assessment, the differences between the actual and predicted responses are found
to be close to each other.
Figure 5. (a) Relationship between actual and predicted values of GFRPA66 30 wt.% COF;
(b) relationship between actual and predicted values of GFRPA66 35 wt.% COF; (c) relationship
between actual and predicted values of GFRPA66 30 wt.% SWR; (d) relationship between actual and
predicted values of GFRPA66 35 wt.% SWR.
To examine the combined effect of the factors on the COF of GFRPA66 30 wt.% and
GFRPA66 35 wt.%, 3-D surface plots of the regression equation were used and are presented
in Figure 6a–f. The contour 3D-plot shows the plot in three different colors: the lowest
value—blue; the average value—green and cyan; and the highest value—red. The highest
COF was obtained due to more interaction between polyamide and the steel surface, such
as frictional heating and bulk erosion. Similarly, the lowest COF was obtained due to strong
control of molecular position during the run. The moderate COF was obtained due to a
lower surface degradation effect.
Materials 2022, 15, 6520 10 of 16
Figure 6. 3D surface of COF model GFRPA66 30 wt.% and GFRPA66 35 wt.%; (a) GFRPA66 30 wt.%
effects of sliding velocity and load, (b) GFRPA66 30 wt.% effects of sliding distance and load,
(c) GFRPA66 30 wt.% effects of sliding distance and sliding velocity, (d) GFRPA66 35 wt.% effects of
sliding velocity and load, (e) GFRPA66 35 wt.% effects of sliding distance and load, and (f) GFRPA66
35 wt.% effects of sliding distance and sliding velocity.
To study the combined effect of the factors on SWR of GFRPA66 30 wt.% and GFRPA66,
3-D surface plots of the regression equation were used in Figure 7a–f. The contour 3D-plot
shows the plot in three different colors: the lowest value—blue; the average value—green
and cyan; and the highest value—red. The highest SWR was obtained due to the volume of
the material decreased. Similarly, the lowest SWR was obtained due to strong control of
molecular position during run and less frictional heating (e.g., less temperature developed
between contacting surfaces). The moderate SWR was obtained due to less degradation of
polyamide occurs throughout the whole material evenly.
Materials 2022, 15, 6520 11 of 16
Figure 7. 3D surface of SWR model GFRPA66 30 wt.% and GFRPA66 35 wt.%; (a) GFRPA66 30 wt.%
effects of sliding velocity and load, (b) GFRPA66 30 wt.% effects of sliding distance and load,
(c) GFRPA66 30 wt.% effects of sliding distance and sliding velocity, (d) GFRPA66 35 wt.% effects of
sliding velocity and load, (e) GFRPA66 35 wt.% effects of sliding distance and load, and (f) GFRPA66
35 wt.% effects of sliding distance and sliding velocity.
Experimental Validation
In order to evaluate the numerical model, validating experiments are conducted at
optimized parameters of 70 N load, sliding velocity of 0.19 m/s, sliding distance of 3000 m,
and weight percentage of 35%. The results of the predictions and experiments for COF and
SWR can be seen in Table 4. It is herewith reported that the experimental outcomes and
predicted results are in close agreement.
4.4. Worn Surface Morphology for Variations in Sliding Velocity and Sliding Distance at 80N Load
Figure 8a,b shows the worn out surfaces of GFRPA66 30 wt.%, for a sliding velocity
0.16, and 0.22 m/s, sliding distance of 2500 m, and 3500 m and applied load of 80 N. It
is observed that the glass fiber comes out of the surface due to surface degradation and
increase the SWR. Similarly Figure 8c,d shows the worn out surface of GFRPA66 35 wt.%,
for the same set of parameters. It is observed that the glass fiber does not come out of the
surface and is less due to less surface erosion. Subsequently, it decreases the SWR.
Figure 8. SEM image of worn surfaces of the GFRPA66 30 wt.% and GFRPA66 35 wt.%, at a load
of 80 N: (a) GFRPA66 30 wt.%, 0.16 m/s; (b) GFRPA66 30 wt.%, 0.22 m/s; (c) GFRPA66 35 wt.%,
0.16 m/s; (d) GFRPA66 35 wt.%, 0.22 m/s.
5. Conclusions
The tribological properties of polyamide GFRPA66 30 wt.% and GFRPA66 35 wt.%
composites are analyzed, and the following inferences are drawn:
• The friction coefficient and SWR decreases with increase in weight percentage of glass
fiber content and lowest values are achieved for 35 wt.% of glass fiber.
• The SWR of GFRPA66 30 wt.% ranges from 0.0120 m3 /Nm to 0.0164 m3 /Nm for
different set of process parameters. Similarly, the SWR of GFRPA6635 wt.% range from
0.0101 m3 /Nm to 0.0161 m3 /Nm. However, as the load, sliding velocity and sliding
distance increases, the SWR decreases.
• The coefficient of friction values ranges from 0.22 to 0.37 for GFRPA66 30 wt.%, while
the coefficient of friction values ranges from 0.15 to 0.31 for GFRPA 66 35 wt.% for
different set of process parameters, which are carefully observed and optimized.
• The ANOVA revealed that the significant and insignificant terms used for the model
(i.e., the “F-value” of GFRPA66 30 wt.% and GFRPA66 35 wt.% for the developed
model) was found to be 96.25 and 44.54 for COF and 17411.57 and 48.87 for SWR,
respectively, indicating that both models are statistically significant.
• The R2 values for COF for GFRPA66 30 wt.% (R2 values-0.9886 and R2 adj -0.9783) and
COF for GFRPA66 35 wt.% (R2 values- 0.9757 and R2 adj -0.9538) are close to a unity.
In the case of SWR, GFRPA66 30 wt.% (R2 = 0.9999 and R2 adj. = 0.9999) and SWR-
GFRPA66 35 wt.% (R2 = 0.9778 and R2 adj. = 0.9578) are also close to unity.
Materials 2022, 15, 6520 13 of 16
• Based on the significant terms, the polynomial equations are formed and using this
equation, optimized COF and SWR are estimated.
• The experimental validations signified that the predicted values are in good conformity
with the actual data and the developed models are adequate.
• The SEM image showed the wear mechanism of the worn out surface of composites
and glass fibers which have come out of the polyamide surface for GFRPA66 30 wt.%
and is more than the GFRPA66 35 wt.% composites.
Author Contributions: Conceptualization, N.J. and C.A.S.; Data curation, A.S. and A.A.; Formal
analysis, N.J., S.N. and M.B.; Methodology, A.S., S.N., M.A., A.A. and M.B.; Resources, A.S., M.A. and
C.A.S.; Software, S.N. and M.A.; Validation, C.A.S.; Writing—original draft, N.J.; Writing—review &
editing, A.A. and M.B. All authors have read and agreed to the published version of the manuscript.
Funding: This research is supported by the Structures and Materials (S&M) Research Lab of Prince
Sultan University. Furthermore, the authors acknowledge the support of Prince Sultan University for
paying the article processing charges (APC) of this publication.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Acknowledgments: The authors extend their appreciation to the Deanship of Scientific Research at
King Khalid University, Saudi Arabia for funding this work through Research Group Program under
Grant No: R.G.P.1/256/43.
Conflicts of Interest: The authors declare no conflict of interest.
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