Materials Research Express

ACCEPTED MANUSCRIPT

Tribological characterization of recycled basalt-aramid fiber reinforced

hybrid friction composites using Grey-based Taguchi approach
To cite this article before publication: S Manoharan et al 2019 Mater. Res. Express in press https://doi.org/10.1088/2053-1591/ab07ce

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Page 1 of 21 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1

1
2
3 Tribological Characterization of recycled basalt-aramid fiber reinforced hybrid friction
4
5 composites using Grey-based Taguchi approach
6
7 S. Manoharan1*, R. Vijay2, D. Lenin Singaravelu2, S. Krishnaraj3, B. Suresha4
8 1
Department of Mechanical Engineering, SSM College of Engineering,

pt
9
10 Komarapalayam, Tamilnadu, India
11
2
12 Department of Production Engineering, National Institute of Technology,
13

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14 Tiruchirappalli, Tamilnadu, India
15 3
Department of Production Engineering, PSG College of Technology, Tamil Nadu, India
16
17 4
Department of Mechanical Engineering, National Institute of Engineering, Mysore,
18
19 Karnataka, India
20

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21 *Corresponding Author Email: ma78sce@gmail.com
22
23
24 ABSTRACT
25
26 Fibers play an imperative role in determining the tribological behavior of
27
28
29
an
reinforced friction composites. The objective of the present study is to develop recycled
basalt and recycled aramid fiber reinforced hybrid friction composites with the addition of
30
31 various fillers and optimize the tribological behaviors of the composites. The pin-on-disc test
32
dM
33 rig was used to conduct dry sliding wear following Taguchi’s L27 orthogonal array with
34
process parameters of the applied load, sliding speed and the weight percentage of fiber
35
36 content. Grey relational analysis was adopted for tribological parameters optimization,
37
38 satisfying multiple performance characteristics. Analysis of variance was used to find the
39
40 contribution of individual factors that affect tribological behavior. Optimal parameter
41 combination for multi-response characteristics of the friction composite under investigation
42
43
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was applied a load of 15 N, sliding speed of 1 m/s and composite with 25 weight percent of
44
45 fiber content. The results showed that addition of fiber content significantly increased wear
46
resistance of the friction composites. Further, from the scanning electron microscopy images
47
48 of friction and wear tested friction composites, plateau formation, fiber-matrix debonding,
49
50 fiber pull out, cracks and damage on the matrix and various wear mechanism were identified.
51
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52 Keywords: Hybrid friction composites, Dry sliding wear, Grey relational analysis (GRA),
53 Weighting and ranking, Analysis of variance (ANOVA).
54
55
56
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57 1. INTRODUCTION
58
59
Fiber reinforced friction composites mainly find applications in automotive and
60 railway brake systems where friction and wear are critical issues. In general, the tribological
 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1 Page 2 of 21

1
2
3 performance of friction materials is based on the friction layer formation on friction surfaces
4
5 and wear debris between the friction couple. The reinforcing fibers in the brake friction
6
7 composites exhibit tribo film developed in the track of tribological stressing by wear debris
8
compaction [1-2]. However, the difficulty and the mechanism of the friction layer formation

pt
9
10 are still not well understood. Sliding speed, normal load, interface temperature and the
11
12 properties of variable composition forms the boundary layers and determines the wear of the
13

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14 friction couple. The purpose of tribology is to eliminate losses due to friction and wear at all
15
levels during sliding in the friction system.
16
17 Basalt fiber in friction composite exhibits the highest µ, and has a tail and a head or
18
19 shot morphology, the "shot" being the harder part of the basalt fiber that enhances
20
tribological performance. Aramid fiber has been effectively used in the non-asbestos organic

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21
22 (NAO) formulations due to its high strength and modulus, high thermal stability, its stable
23
24 and steady coefficient of friction (µ) and low fade behaviors [3]. However, a higher amount
25
26 of fiber in the friction materials enhances thermal stability in maintaining the friction
27
28
29
an
characteristics [4]. Friction composites based on hybrid fiber consisting of the binary/ternary
combination of reinforcement fibers have superior characteristics, which is not possible in
30
31 reinforced composites with single kind of fiber reinforcement [5,6]. Fillers such as copper,
32
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33 molykote, SiC, and alumina play a key role in determining the frictional properties of
34
composites. Among the above, copper plays a major role in determining the tribological
35
36 properties of composites [7-10]. Recycling of fibers is considered as paramount solution to
37
38 lessen junk output and incinerators which are sent to landfills by converting waste and other
39
40 used materials into reusable products and helps to protect the environment by reducing the
41 amount of extraction of natural resources. It increases economic security by tapping a
42
43
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domestic source for materials and prevents pollution by reducing the need to collect new raw
44
45 materials.
46
Most investigations in friction composites detailed the consequence of one
47
48 parameter by maintaining the remaining parameters as an invariable. On the other hand, the
49
50 combined effect of interacting factors which influence the experimentation has not been
51
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52 studied, and the present study addresses this gap in research. Limited literature is available in
53 optimizing the tribological performances of friction materials as they are significant.
54
55 Satapathy et al. [3] applied GRA to find the influence of the fiber combination such as
56
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57 organic fibers and rock fibers as factors, which effect the general performance of composite
58
59
friction material. Taguchi’s orthogonal array and other optimization process were employed
60 by several authors [11-13] in optimizing the friction performances of friction materials.
Page 3 of 21 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1

1
2
3 Taguchi method examined the influence of each parameter in friction composites and in
4
5 optimizing single performance characteristics. However, it may not be useful for numerous
6
7 responses as it favors a faulty result. To overcome this, the authors combined the Taguchi
8
method with Grey Relational Analysis (GRA) to solve multi-response characteristics and to

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9
10 optimize the tribological parameters. Thus, taking into consideration the above-stated fact,
11
12 the decision to study, dry sliding wear behavior of hybrid fiber reinforced friction composites
13

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14 using design parameters of applied load (L), sliding speed (S) and weight percentage(wt. %)
15
of fiber content (F) was done. The present study is also designed to optimize factors
16
17 influencing the tribological performance of friction composites. A Grey-based Taguchi
18
19 method is used to calculate the optimal tribological behaviors for multi-responses such as
20

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21 coefficient of friction (µ) and the specific wear rate (Ks) of hybrid friction composites.
22 2. MATERIALS AND METHODS
23
24 2.1 Materials
25
26 In general, recycling of waste is done to prevent dumping of solid wastes, the
27
28
29
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basalt and aramid fibers are recycled from the used materials. Other parental ingredients are
procured from the suppliers of the friction material industry.
30
31 2.2. Fabrication of the friction composites
32
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33 The developed hybrid friction composites contain fourteen ingredients as listed in
34
Table 1 and the process of fabrication including mixing in plough shear (lodigee) mixer for
35
36 20 minutes in the sequence of fibers, fillers and friction modifiers and binders, curing was
37
38 done by compressing molding with a pressure of 13 MPa, temperature 145°C for 7 minutes
39
40 and post-curing in a hot oven for 5.5 hours at 160°C. Five intermediate breathings were
41 allowed to remove volatile gas. Condensation polymerization reaction occurs during
42
43
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compression molding. Finally, the friction composite plates of 200 mm × 200 mm × 6 mm

44
45 size were fabricated, and removed from the compression mold, the surfaces of the friction
46
composites were then ground with the belt grinder achieve the required thickness and
47
48 eliminate the resinous skin layer. Thus the developed hybrid friction composites were
49
50 designated as C1, C2, C3 and the pin on disc test specimen of size 27 mm x 6 mm x 6 mm
51
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52 was machined from the developed hybrid friction composite plates. The density of the
53 developed composites was measured as per the Archimedes principle in the density
54
55 measurement apparatus. Hardness was measured using a Rockwell hardness tester possessing
56
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57 K scale with steel indenter of 3.125 mm diameter by application of 1500 N load. Three
58
59
samples were tested with 5% of allowable error for density and hardness measurement as per
60 standard industrial practice. These physical properties tests were done as per IS2742 Part 3.
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1
2
3 Table 1 Formulation and physical properties of the developed hybrid friction
4
5 composites (with ingredients in wt. %)
6
7 Developed Hybrid Friction Composites
8
Broad
Ingredients (Designation)

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9 Classification
10 C1 (in wt%) C2(in wt%) C3(in wt%)
11
12
Recycled Basalt 20 15 10
Fibers
13 Recycled Aramid 5 5 5

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14
15 Phenol formaldehyde powder,
Binder with
16 NBR, Calcium Oxide, Crumb 16 16 16
17 Additives
18 rubber
19
Functional Cashew friction dust, Kaolin
20

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21 Fillers clay, Tin powder, Exfoliated 41 41 41
22
23 vermiculite
24 Inert filler BaSO4 0 5 10
25
26 Friction Modifiers Molykote, Graphite, SiC 18 18 18
27
28
29
Physical
Properties
Density (g/cm )
Hardness (No unit)
3
an 1.76
85
1.82
83
1.83
79
30
31 2.3 Dry sliding wear test
32 Dry sliding wear experiment was conducted according to ASTM G99-05 using a Pin-
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33
34 on-Disc type test rig. A cast iron brake disc (diameter: 160 mm, thickness: 13 mm and
35
36 hardness: 170 BHN) was used as the counter face for the friction composites, and the
37
38
chemical composition of the disc is listed in Table 2. The chemical composition details of the
39 disc were provided by the supplier. Experimental investigations related to the Taguchi’s L27
40
41 (33) orthogonal array were carried out according to controlling parameters shown in Table 3.
42
43 Wear was calculated in terms of weight loss, which was subsequently converted to wear
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44
volume loss using calculated density value. Specific wear rate (KS) was calculated from the
45
46 Equation (1).
47
48 ΔV
49
Ks = m3 /Nm (1)
L D
50
51 ΔV-volumetric wear, L -applied normal load (N) andD-sliding distance (m).
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52
53 Table 2 Chemical Composition of the cast iron disc used for dry sliding wear test
54
Elements Composition (in wt.%)
55
56 C 3.9
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57
58 Si 1.74
59 Mn 0.402
60
Page 5 of 21 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1

1
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3 P 0.089
4
5 S 0.025
6
7
Ni 0.039
8 Cr 0.066

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9
10 Mo 0.015
11 Cu 0.045
12
13 Ti 0.02

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14
15 Fe Balance
16
17
18 Table 3 Control factors and their levels of dry sliding wear
19
20 Factor Description Level I Level II Level III

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21
22 L Applied load (N) 15 30 45
23
24 S Sliding speed (m/s) 1 1.5 2
25
26 F Fiber content (wt. %) 15 20 25
27
28
29
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2.4 Design of experiments
30
31 The present experimental work aims to optimize test parameters to obtain maximized
32
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33 µ and minimized Ks for the developed hybrid friction composites as summarised in Table 4.
34
Applied load (L), sliding speed (S) and fiber content wt. % (F) were considered as parameters
35
36 that influence the dry sliding wear process. The main controlling factors and their levels
37
38 along with their experimental results of dry sliding wear are tabulated in Table 4.A standard
39
40 L27(33) orthogonal array was chosen to determine the process interrelationship with four
41 controlling factors. Each influencing parameters was assigned a column and the experiments
42
43
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were ordered randomly to minimize error in the experimental work [14].

44
45 Table 4 Experimental results of dry sliding wear of L27orthogonal array
46
47 Experimental parameters Optimizing parameters
48 Sliding Fiber Specific wear rate Coefficient of
49 Exp. Applied
50 speed content x friction
51 No load (N)
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52 (m/s) (wt.%) 10-5mm3/Nm (μ)

53
54
1 15 1 15 3.3125 0.43
55 2 15 1 20 2.7911 0.48
56
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57 3 15 1 25 1.8845 0.55
58
59 4 15 1.5 15 5.0854 0.40
60
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1
2
3 5 15 1.5 20 3.5449 0.47
4
5 6 15 1.5 25 2.6738 0.54
6
7 7 15 2 15 6.3124 0.38
8
8 15 2 20 5.2721 0.45

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9
10 9 15 2 25 3.5210 0.51
11
12 10 30 1 15 2.9805 0.38
13

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14 11 30 1 20 2.5141 0.47
15
12 30 1 25 1.6345 0.51
16
17 13 30 1.5 15 3.9462 0.35
18
19 14 30 1.5 20 2.9803 0.45
20

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21 15 30 1.5 25 2.2817 0.49
22 16 30 2 15 4.6632 0.30
23
24 17 30 2 20 3.2966 0.41
25
26 18 30 2 25 2.6634 0.47
27
28
29
19 45 1
an 15 2.5925 0.32
20 45 1 20 2.3551 0.34
30
31 21 45 1 25 1.3917 0.39
32
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33 22 45 1.5 15 3.4594 0.25
34
23 45 1.5 20 2.9555 0.27
35
36 24 45 1.5 25 2.1713 0.38
37
38 25 45 2 15 3.8446 0.25
39
40 26 45 2 20 2.9626 0.26
41 27 45 2 25 2.5664 0.36
42
43
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GRA coupled with the Taguchi technique was used to optimize the factors which
44
45 influence dry sliding wear with multiple performance characteristics. To perform GRA, first,
46
47
the experiments results were normalized between zero and one known as data pre-processing
48 (grey relational generation, GRG). As a result of this simplified approach, the optimization of
49
50 problematical multiple responses was converted to single GRG. In the present study
51
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52 experimental data such as specific wear rate and coefficient of friction are the responses to be
53
optimized and were normalized between zero and one. To obtain the optimal wear behavior,
54
55 “lower-the-better” characteristic was used to minimize specific wear rate (Table 5), which is
56
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57 normalized by using the following expression:

58
59
60
Page 7 of 21 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1

1
2
3
4 max xi (k ) − xi (k )
xi* (k ) = (3)
5 max xi (k ) − min xi (k )
6
7 The coefficient of friction of composite should follow the “higher-the-better” criterion
8

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9 (Table 5) which are expressed as
10
11 xi (k ) − min xi (k )
xi* (k ) = (4)
12 max xi (k ) − min xi (k )
13

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14 where xi* (k ) and xi (k ) are sequences after data pre-processing and comparability sequence, k
15
16 = 1 for specific wear rate. i = 1, 2, 3....27 and k = 2 for coefficient of friction. i = 1, 2, 3....27.
17
18 0i (k ) is the deviation of sequence between the reference sequence x0* (k ) and comparability
19
20 sequence xi* (k ) and the difference of the absolute value of x0* (k ) calculated using Eq.(5) as

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21
22 shown in Table 5:
23
24
25
 0i (k ) = x0* (k ) − xi* (k ) (5)
26
27
28
29
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The grey relational coefficient (GRC) stands for the correlation between the desired
and actual normalized experimental results and is given as follows
30  min +  max
31  i (k ) = (6)
32  0i (k ) +  max
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33
34 ξi(k) - grey relational coefficient, 0i (k ) is deviation sequence of the reference sequence x0* (k )
35
36 and comparability sequence xi* (k ) , ζ is the distinguishing and identification coefficient. The
37
38 function of GRC is to develop or to constrict the range of grey relational coefficient. If the
39
40 parameters are defined in identical preference, then ξ is considered as 0.5, which is to turn
41
42 down the effect of ∆max when extremely big and defined in a range of 0 ≤ ζ ≤ 1. Table 6
43
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shows the calculated GRC for every experiment using the Eq. (5). After calculating GRC,
44
45 GRG is calculated by averaging the GRC related to all performance characteristics. GRG
46
47 based multiple performance characteristics of the entire experiments can be evaluated using
48
49
the subsequent equation:
50 1 n
51 i =   i (k )
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(7)
52 n k =1
53
54  i – Grey Relational Grade, ξi (k) - Grey Relational Coefficient, n- Number of experiments
55
56 Table 5 Data pre-processing and deviation sequences of hybrid friction composites
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57
58 Exp. No. Data pre-processing Deviation Sequence (Δ0i )
59 Specific Coefficient Specific wear Coefficient of
60
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1
2
3 rate friction
4
5 wear rate of friction Δ0i (1) Δ0i (2)
6
7 1 0.6100 0.6000 0.3900 0.4000
8

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9 2 0.7160 0.7670 0.2840 0.2330
10 3 0.9000 1.0000 0.1000 0.0000
11
12 4 0.2490 0.5000 0.7510 0.5000
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14 5 0.5620 0.7330 0.4380 0.2670
15
16
6 0.7390 0.9670 0.2610 0.0330
17 7 0.0000 0.4330 1.0000 0.5670
18
19 8 0.2110 0.6670 0.7890 0.3330
20

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21 9 0.5670 0.8670 0.4330 0.1330
22
10 0.6770 0.4330 0.3230 0.5670
23
24 11 0.7720 0.7330 0.2280 0.2670
25
26 12 0.9510 0.8670 0.0490 0.1330
27
28
29
13 0.4810
an
0.3330 0.5190 0.6670
14 0.6770 0.6670 0.3230 0.3330
30
31 15 0.8190 0.8000 0.1810 0.2000
32
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33 16 0.3350 0.1670 0.6650 0.8330
34
35
17 0.6130 0.5330 0.3870 0.4670
36 18 0.7420 0.7330 0.2580 0.2670
37
38 19 0.7560 0.2330 0.2440 0.7670
39
40 20 0.8040 0.3000 0.1960 0.7000
41 21 1.0000 0.4670 0.0000 0.5330
42
43
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22 0.5800 0.0000 0.4200 1.0000

44
45 23 0.6820 0.0670 0.3180 0.9330
46
47
24 0.8420 0.4330 0.1580 0.5670
48 25 0.5020 0.0000 0.4990 1.0000
49
50 26 0.6810 0.0330 0.3190 0.9670
51
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52 27 0.7610 0.3670 0.2390 0.6330

53
54
Worn surface characteristics were analyzed using a scanning electron microscopy(SEM).
55 3. RESULTS AND DISCUSSIONS
56
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57 A higher GRG is considered the strongest relational degree between both

58
59 reference and comparability sequences, corresponds to the optimal parameter combination. If
60
Page 9 of 21 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1

1
2
3 GRG is higher, the quality of the product will be nearest to an ideal value which is considered
4
5 for optimum tribological performance. It is clear that lesser wear of friction composite is
6
7 offered by the comparability sequence with a higher value of GRG. From the combination of
8
factors result, higher GRG is allocated for the highest order, while the minimum GRG is

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9
10 allocated for the lowest order. Ranking of the GRG values as shown in Table 6.
11
12 Table 6 Grey Relational Coefficient and Grey Relational Grade of hybrid friction
13

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14 composites
15
Exp. No Grey relational coefficient GRG Rank
16
17 Specific wear rate Coefficient of friction
18
19 1 0.5620 0.5560 0.5586 15
20

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21 2 0.6370 0.6820 0.6596 8
22
3 0.8330 1.0000 0.9166 1
23
24 4 0.4000 0.5000 0.4499 23
25
26 5 0.5330 0.6520 0.5927 12
27
28
29
6 0.6570
an 0.9380 0.7975 3
7 0.3330 0.4690 0.4010 26
30
31 8 0.3880 0.6000 0.4940 19
32
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33 9 0.5360 0.7900 0.6628 7
34
35
10 0.6080 0.4690 0.5382 17
36 11 0.6870 0.6520 0.6694 6
37
38 12 0.9100 0.7900 0.8498 2
39
40 13 0.4910 0.4290 0.4596 22
41
14 0.6080 0.6000 0.6038 11
42
43
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15 0.7340 0.7140 0.7243 5

44
45 16 0.4290 0.3750 0.4021 27
46
47 17 0.5640 0.5170 0.5404 16
48 18 0.6590 0.6520 0.6557 9
49
50 19 0.6720 0.3950 0.5334 18
51
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52 20 0.7190 0.4170 0.5676 13

53
54
21 1.0000 0.4840 0.7419 4
55 22 0.5430 0.3330 0.4383 24
56
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57 23 0.6110 0.3490 0.4801 20

58
59 24 0.7590 0.4690 0.6141 10
60
 AUTHOR SUBMITTED MANUSCRIPT - MRX2-101880.R1 Page 10 of 21

1
2
3 25 0.5010 0.3330 0.4170 25
4
5 26 0.6100 0.3410 0.4756 21
6
7 27 0.6770 0.4410 0.5590 14
8
The optimal parameter setting for multiple performances of maximum µ and

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9
10 minimum Ks is obtained for experiment number 3, which has the highest grey relational
11
12 grade (0.9166). This implies that the factor setting of experiment number 3 provides the
13

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14 nearest optimal setting from the point of dry sliding wear. Since the factorial design is
15
orthogonal, the consequence of every parameter over the GRG value at various levels is
16
17 separated. For example, the mean GRG for factor A at three levels is estimated by calculating
18
19 the average value of GRG for experiments 1 to 9, 10 to 18 and 18 to 27. Similarly, the mean
20

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21 of GRG for every level of remaining parameters can be calculated and listed in Table 7. The
22 total mean of GRG of this orthogonal array can be obtained by dividing the sum of GRG with
23
24 the total number of experiments, is summarised in Table 7. The delta (max-min) value is the
25
26 differences between the highest and lowest values among values in each row and based on
27
28
29
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this; the response table assigns a rank for optimum parameter setting.
Table 7 Response table for grey relational grade
30
31 Grey Relational Grade Delta
32 Symbol Parameter Rank
dM
33 Level 1 Level 2 Level 3 (max-min)
34
35 L Applied load (N) 0.6147 0.6048 0.5363 0.0784 3
36 S Sliding speed (m/s) 0.6706 0.5734 0.512 0.1586 2
37
38 F Fiber content (wt. %) 0.4665 0.5648 0.7246 0.2582 1
39
40 Total mean of grey relational grade = 0.5853
41
42
43
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In general, large variation of GRG values from setting one factor on further implies
44
45 that the specific design parameter is an important factor to reach the performance
46
47 characteristic. It is clear from Table 7 that the delta values of GRG of sliding wear parameters
48
are as follows: 0.0784 for applied load, 0.1586 for sliding speed and 0.2582 for wt. % of fiber
49
50 content. The maximum value for fiber content viz., 0.2582 shows that among the other two
51
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52 parameters, fiber content (factor F) has the strongest effect over multi-response
53
54 characteristics in controlling the sliding wear behavior of the reinforced friction composites
55 under investigation. This indicates that sliding wear performance is determined by the
56
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57 addition of wt. % of fiber content (F) followed by sliding speed (S) and applied load (L) in
58
59
60
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1
2
3 that order. The optimal combination of design parameter for specific wear rate and coefficient
4
5 of friction are estimated from the GRG values as shown in Figure 1.
6
7
8

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9
10
11
12
13

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14
15
16
17
18
19
20

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21
22
23
24
25 Figure 1 Graphical representation of the grey relational grade
26
27
28
29
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In the current experimental investigation, it is L1S1F3, i.e., applied load of 15 N (L1), sliding
speed of 1 m/s (S1) and composite with 25 wt. % fiber content (F3) is confirmed in Figure 2.
30 Figure 2 also illustrates the signal-to-noise (S/N) ratio of GRG for all parameters and
31
32 confirms the order of priority to control parameters that determine the friction wear
dM
33
34 performances.
35
36 Main Effects Plot for SN ratios
37 Data Means
38
Applied Load Sliding Speed
39
-3
40
41 -4
42
-5
43
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Mean of SN ratios

44 -6
45
-7
46 15 30 45 1.0 1.5 2.0
47 Fiber Content
48 -3
49
50 -4
51
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-5
52
-6
53
54 -7
55 15 20 25
56 Signal-to-noise: Larger is better
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57
58 Figure 2 Effect of dry sliding wear parameters levels in terms of GRG
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3 In general, the tribological behavior of friction composites is associated with various
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5 parameters such as sliding speed, applied load and wt. % of reinforcement fiber and interface
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7 temperature. Tribological characteristics are evaluated by the degree of interactions between
8
the friction composite and cast iron surface that are in contact. This is because during sliding;

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10 formation of the frictional film determines the µ and Ks of the friction composites. The
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12 formations of frictional film and friction characteristics are mainly dependent on the interface
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14 temperature and reinforcement material. A higher amount of fiber content in the friction
15
composites with better thermal stability resists the thermal degradation of the phenol-
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17 formaldehyde matrix and enhances fiber-matrix bonding. Öztürk et al. [4] evaluated the
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19 tribological properties of basalt and ceramic fiber-based friction materials and stated that
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21 inclusion of basalt fiber in the friction composites increases specific wear rate and coefficient
22 of friction considerably. The findings of this study agree with the above-stated literature.
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24 3.1 Analysis of Variance
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26 Analysis of variance (ANOVA) is a statistical tool which exhibits significant
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conclusions and reveals the altitude of the significance of the main factor and its interactions
on a particular response by comparing the mean square against errors at specific confidence
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31 levels [16]. The results of the sliding wear experiments have been analyzed using ANOVA to
32
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33 identify the parameters exerting a major influence on the wear of friction composites. Table 8
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shows the ANOVA values for GRG carried out using MINITAB R15. The percentage of
35
36 contribution of fiber content (63.01 %) was found to be a most effective parameter that
37
38 affects the sliding behavior of hybrid friction composites. Sliding speed (23.74%) was found
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40 to be next influencing factor, followed by applied load (6.76 %) as shown in Figure 3,
41 revealing various the levels of the factors considered.
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Table 8 ANOVA results for combined response of specific wear rate and coefficient of
44
45 friction of hybrid friction composites
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47 Source of F- P- % of
DOF Seq SS Adj SS Adj MS
48 variation Ratio Value contribution
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50 Applied load 2 0.03280 0.03280 0.01640 10.41 0.001 6.76
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52 Sliding
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54 speed 2 0.11512 0.11512 0.05756 36.55 0 23.74
55 Fiber
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57 content 2 0.30558 0.30558 0.15279 97.02 0 63.01

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59 Error 20 0.03150 0.03150 0.00158 6.49
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3 Total 26 0.48500 100.00
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5 DOF- Degrees of Freedom, SS - Sum of Squares, MS - Mean Square
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21 Figure 3 Contribution (%) of factors on grey relational grade
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23 3.2 Confirmation Experiment
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25 In general, verification study is needed to confirm the accuracy of analysis
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after optimal of test parameters levels are identified. Once the optimum level is selected, the
improvement in multiple response characteristics affecting (Table 3) dry sliding wear is
30 predicted and verified subsequently. The predicted optimum value is found with the aid of
31
32
additive law as given by:
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33 q
34 ˆ =  m +  (ˆi −  m ) (8)
35 i =1
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37  m -Total mean of GRG, ˆi -mean of GRG at an optimum level, q -the number of main
38
39 control parameters affecting multiple response characteristics. ANOVA indicates that the
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41 sliding speed (S) and wt. % of fiber content (F) are significant factors, and applied load (L) is
42 the least significant factor. The predicted GRG value is 0.8393, and the experimental GRG
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44 value using optimized test parameters is 0.9166 as listed in Table 9. The improvement of the
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46 grey relational grade is 0.0773. Thus, the present works statistics by GRG shows evidence for
47
48
improvement in sliding wear behavior of the friction composites.
49 Table 9 Comparison of predicted and experimental value of Grey Relational Grade
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Results for confirmation of experiment

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53 Experimental value Predicted value
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55 Combination of testing parameters L1S1F3 L1S1F3
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57 Grey relational grade 0.9166 0.8393

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59 Improvement in GRG 0.0773
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5 3.3 Correlation of Optimum Results with Worn Surface Morphology
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7 The process of optimization identifies the minimum number of experiments to be
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carried out based on the Design of Experiments (DOE) under dry sliding conditions. The

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10 experimental results were analyzed using ANOVA to identify the parameters exerting major
11
12 influence over the wear of friction composites. The optimum conditions were identified, and
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14 confirmatory experiments were carried out to validate the results of the GRA.
15
3.3.1 Effect of reinforcement
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17 The coefficient of friction for friction composites increases with the addition of
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19 fiber content i.e., composite C3 (15 wt. % of fiber content) and exhibits a lower value of μ
20
(0.25). The value of μ increases to (0.55) with increase in wt. % of fiber content to 25 wt. %

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22 (C1). This is because the higher the fiber content the higher will be the friction and thermal
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24 stability. During braking, friction composites slide against the metallic counter surface;
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26 frictional heat is developed at the friction interface. Frictional heat thus developed affects the
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tribological behavior of the friction composites by thermal degradation and softening of the
phenol-formaldehyde resin. According to Herring [17], at high interface temperatures,
30
31 constituents in the friction composites release gas leading to thermal degradation. The
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33 softening of phenol formaldehyde resin causes debonding in fiber-matrix, detachment in the
34
phenol-formaldehyde matrix and cracking in the composite surface layers of the composites
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36 [18]. Composite with a higher content of recycled basalt fiber (C1, 20 wt. %) resists thermal
37
38 degradation due to higher thermal stability which was challenging to fiber-matrix debonding
39
40 as it maintains the matrix integrity of composite at high temperatures. At a high braking
41 temperature, wear rate of the friction composites may increase exponentially due to the
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degradation of organic resin binders.

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45 Further, it also depends on various ingredients of the friction composites and their interaction.
46
While braking, the developed heat at the friction interface affects the friction surface of the
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48 composites forming a frictional film on the surface. With an increase in temperature,
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50 formation of a frictional film on the surface is reduced considerably, and wear rate increases
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52 exponentially. A drop in interface temperature augments transfer film formation which covers
53 the worn surface with a related change in the corresponding wear rate and friction coefficient.
54
55 Hence, a higher fiber content in friction composites leads to higher thermal stability and a
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57 reduction in interface temperature which reduces the wear rate with enhanced friction
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performances in the friction composites [4].
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3 A higher content of recycled basalt fiber in friction composites has a higher
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5 degree of hardness as it has increased the amount of shot or harder part in the composites.
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7 The higher amount of recycled basalt fiber in composite C1 with a superior harder part
8
further resists wear rate of the friction composites. Hence, composite C1 with a higher degree

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10 of hardness reduces the specific wear rate along with hard fillers such as silicon carbide, iron,
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12 and alumina particles. Along with basalt fiber, aramid fiber also enhances the wear resistance
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14 of friction composite due to its combined properties of fibrillation, ductility, and elongation.
15
In hybrid friction material composites, addition of hard basalt fiber along with ceramic fiber
16
17 effectively increases the friction coefficient and decreases the specific wear rate of the
18
19 friction materials [4]. Similarly, Kato & Magario [19] assessed the role of aramid fiber in the
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21 wear of friction materials and confirmed that the adding of aramid fiber considerably
22 enhances wear resistance and friction stability. Also, molykote and graphite are dispersed in a
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24 soft phase. The phenol formaldehyde matrix acts as a lubricant and enhances the frictional
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26 film formation on the surface of the composites which effectively prevents the wear rate of
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the composite C1.
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Poor adhesion between fiber-matrix interface results in fiber-matrix debonding,
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31 fiber pull out, cracks and damage on the matrix surface (marked as C) which are more in
32
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33 lesser fiber (15 wt. %) reinforcement composite (C3), is evident from Figure 4 (a). However,
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good adhesion between the fiber-matrix interfaces in increased fiber reinforcement composite
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36 (C1, 25 wt. %) shows smooth and better surface integrity (marked as S) as confirmed by
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38 Figure 4 (b). Fibers in the composites enhance the tribological performances by maintaining
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40 the true contact area (marked as A) between friction surfaces. This is because, composite C1
41 associated with more fibers which increase the area of contact and form plateaus. Thus, the
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rough surface of the composite specimen is worn, and the real contact surface area between
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45 the specimen and counterface disc is increased in composite C1, unlike composites C2 and
46
C3. Further, good adhesion between the fiber- matrix interfaces protects the low modulus
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48 phenol formaldehyde matrix from damage during sliding. This is because the degree of
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50 debonding is not adequate to cause fiber pullout in the friction composite C1.
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19 Figure 4 Worn surface morphology of (a) 15 wt. % of fiber content composite (C3)
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21 and (b) 25 wt. % of fiber content composite (C1)
22
23 3.3.2 Effect of sliding speed
24 In general, the µ of the friction composites seem to decrease with an increase in
25
26 sliding speed due to rise in the interface temperature. Detailed SEM investigations on sliding
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wear behavior of hybrid fiber reinforced friction composites on the effect of varying the sliding

30
speed from 1 m/s to 2 m/s are shown in Figures 5 (a & b). This rise in temperature causes the soft
31 phenol formaldehyde matrix to melt, forming more patches on the matrix surface which peels
32
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33 off while friction composites slide against the counterface surface. Further, the melting of the
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35 phenol-formaldehyde matrix reduces the fiber-matrix adhesion and causes fiber to pull out
36
(marked as E) from the matrix. Hence, at a higher sliding speed the friction coefficient is
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38 reduced. Table 4 confirms that, at a lower speed, the higher values of friction coefficient are
39
40 experienced. However, the value of μ decreases with an increase in sliding speed. Also, the
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42 worn surface of friction composites appeared to be smooth with limited formation of a
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primary plateau with lesser wear track at lower sliding speed, as shown in Figure 5 (a).
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45 However a rough and damaged surface is observed when it slides at a higher speed, as shown
46
47 in Figure 5 (b). The primary plateaus are formed by adhering fibers which play a key role in
48
49
arresting fine wear particles from movement at the interface forming loose granular films.
50 These loose fine wear particles a mainly constituent of polymeric ingredients, aramid, etc.
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52 stick together with an increase in pressure and temperature during braking thus forming
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54 secondary plateaus and leading to dense film formations. As stated in literature, that primary
55
plateaus have load bearing capacity as well as boost friction, while the secondary plateaus
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57 deteriorate the same[20,21].

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3 Wear mainly depends on the applied load and sliding speed of the composites.
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5 The developed heat at the friction interface results in plastic deformation and thermal
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7 softening in the frictional surfaces and of the various ingredients. It also changes the rate of
8
oxidation in the friction surface affecting wear rate of the composites. The change in speed

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10 causes frictional heating resulting in severe wear in the composites. At a higher sliding speed,
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12 a high degree of fiber pull out (marked as E) from the composites causes an increased amount
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14 of hard wear debris or asperities (marked as D) formation at the friction interface, which
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directs severe wear and crack (marked as C ) in the friction composite as shown in Figure 5
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17 (b). The wear asperities consist of small broken fibers from the sheared-deformed phenol
18
19 formaldehyde matrix and wear particles of the cast iron friction counterface. Also, at a higher
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21 sliding speed, the debris particles present in the counter face increase the degree of the impact
22 type based on the repeated loading on friction surface. Hence, this impact load causes some
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24 frictional thrust and constrained vibration and chatter at the friction interface resulting in
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26 more debonding and cracking of hybrid fibers [22]. These hybrid fibers have an abrasive
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effect on the sliding interface and increase the wear rate of the friction composites by
damaging the counter face friction film as sliding speed increases. Also, the surface of
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31 tribofilm formed at low speed is smooth; while that formed at a higher sliding speed is rough.
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33 Hence, a lower wear rate is observed at a lower sliding speed as confirmed in Figure5 (a).
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50 Figure 5 Worn surface morphology of friction composites sliding at (a) lower sliding
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52 speed (1 m/s) (b) higher sliding speed (2 m/s)

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3.3.3 Effect of applied load
55 The coefficient of friction of the friction composites, as a rule, decreases as the
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57 applied load is increased. At a lower load (15 N), a higher friction coefficient (0.55) is
58
59 experienced, however, it decreases to (0.25) as the load is increased to 45 N. This is because
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3 as the load increases, space between the friction composite specimen and cast iron disc is
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5 reduced considerably causing more wear debris to lodge between the disc and composite
6
7 specimen as confirmed from Figure 6(b). In general, a film or agglomerates causes
8
lubrication on the friction composites [2]. The molykote and graphite present in the friction

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10 composites enhance the lubrication behavior of the composites due to its better lubrication
11
12 property. Hence, the lubrication thus developed in the friction composites reduces the
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14 coefficient of friction, as the load is increased.
15
Further, the specific wear rate of the composites decreases with an increase in the applied
16
17 load. This can be explained by the fact that hard particles such as fibers and fillers in the
18
19 phenol-formaldehyde matrix support the load and reduce plastic deformation at higher loads.
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21 Also, the formation of friction film (primary plateau) decreases the specific wear rate at
22 higher loads. This is confirmed from the Figure 6(a) where at a lower load formation of tribo
23
24 film (primary plateau) is been reduced considerably. Thus, the composite displays a higher
25
26 wear rate under a load of 15 N.
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SEM analysis of the worn surfaces of the composite experienced at an applied load of
15 and 45 N are shown in Figures 6 (a & b) respectively. The hard wear debris particles
30
31 (marked as D) and patches (marked as H) consist of sheared-deformed phenol formaldehyde
32
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33 matrix which contains small broken fibers and wear particles of the counterface. During the
34
wear, more iron particles from the metallic counter face accommodate with small broken
35
36 fiber elements on the friction surface, resulting in tribofilm formation. The formation
37
38 tribofilm on the friction surface covers the worn surface of composite and protects it from
39
40 severe wear conditions reducing wear rate at higher loads [23,24]. Hence, with increases in
41 load, the enhancement of plastic deformation under wear causes surface damage mechanism
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(fracture in fiber and fiber-matrix interface). In a similar study [23,25], the inclusion of fiber
44
45 content in friction materials decreases the specific wear rate with increased applied load.
46
Hence, this conclusion concurs with the above studies.
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Figure 6 Worn surface morphology of friction composites for the applied load of (a) 15

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21 N (b) 45 N
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23 4. CONCLUSIONS
24
25 The influence of control parameters on the tribological performance of hybrid friction
26
27
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29
➢
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composites was studied, and the following conclusions drawn:
The experimental study of the dry sliding test indicates that the addition of fiber content
30 improves the coefficient of friction and reduces the specific wear rate of the composites. The
31
32 tribological performance of friction composite C1 (25 wt. % fiber content) was better than
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33 all other formulations.
34
35 ➢ A Grey-Taguchi technique was used to optimize multiple responses of dry sliding wear
36
37 behavior of hybrid friction composites. The experimentation of optimal parameter setting
38
39
confirms the decrease in specific wear rate and improvement in coefficient of friction of the
40 friction composites. The optimum parameter combination from the Grey –based Taguchi
41
42 method for the present experimental study is as follows: L1S1F3, i.e., applied load of 15 N
43
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44 (L1), sliding speed of 1 m/s (S1) and composite with 25 wt. % fiber content (F3).
45
➢ From the ANOVA test, the wt. % of fiber content (63.01 %) was found to be the major
46
47 influencing factor, determining the tribological behavior of the friction composites; sliding
48
49 speed (23.74%) was found to be the next influencing factor, followed by applied load (6.76
50
51 %).
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52 ➢ Worn surface features show plateau formation, fiber-matrix debonding, fiber pull out,
53
54 cracks and damage on the matrix and various wear mechanisms. These were largely due to
55
56 design parameters such as wt.% of fiber content, sliding speed and applied load.
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Thus from the results, it is clear that higher fiber content in the hybrid friction composite
59 helps to sustain the coefficient of friction and wear resistance.
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1
2
3 References
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5 [1] Tej Singh, and Amar Patnaik (2015) Archives of Civil and Mechanical Engineering
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7 15.1: 151-161.
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[2] Eriksson Mand Jacobson S (2002) Tribology International 33, 817-827.

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10 [3] Satapathy BK and Bijwe J (2005) Journal of Reinforced Plastics and Composites 24,
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14 [4] Öztürk B, Arslan F and Öztürk S (2007), Tribology International 40(1), 37-48.
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[5] Sreekala M, George J, Kumaran MG and Thomas, S (2002) Composite Science and
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17 Technology 62, 339-353.
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19 [6] Manoharan S, Vijay R, Lenin Singaravelu D, Mohamed Kchaou (2018) Industrial
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21 Lubrication and Tribology, 1-8.
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24 Institute of Metals 71(8), 2025–2033.
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26 [8] Thankachan T Soorya Prakash K (2017) Materials Science and Engineering: A 688,
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[9] Harikishor Kumar, Khan MZ, Vashista M (2018) Materials Research Express, 5(8)
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33 [10] Harikishor Kumar, Prasad R, Srivastava A, Khan MZ, Vashista M (2018) Journal of
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Cleaner Production 196, 460-468
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36 [11] Ferit Ficici, Mesut Durat and Murat Kapsiz (2014) Journal of the Brazilian Society of
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48 [15] Kuo Y. Yang T and Haung GW (2008)Engineering Optimizations 4(6), 517-528.
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50 [16] Ramesh BN and Suresh B(2014)Materials and Design 59, 38-49.
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52 [17] Herring JM (1967) Society of Automotive Engineers, 670146.

53 [18] Tanaka K, Ueda S and Noguchi N (1973) Wear23(3), 349-365.
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57 [20] Vijay R, Lenin Singaravelu D, Jayaganthan R (2019) Friction, 1-45.

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3 [22] Vishwanath B, Verma A, Pand Rao, CVSK (1990) Composites 21(6), 531-536.
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5 [23] Gomes JR, Silva OM, Silva CM, Pardini LC and Silva RF (2001) Wear249, 240–5.
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