Materials Research Express

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Investigation of Caryota urens fibers on physical, chemical, mechanical

and tribological properties for brake pad applications
To cite this article before publication: G Sai Krishnan et al 2019 Mater. Res. Express in press https://doi.org/10.1088/2053-1591/ab5d5b

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Page 1 of 15 AUTHOR SUBMITTED MANUSCRIPT - MRX2-103831.R1

1
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3 Investigation of Caryota urens fibers on physical, chemical, mechanical and tribological
4

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5 properties for brake pad applications
6
7 G.Sai Krishnan1*, L.Ganesh Babu2, P.Kumaran3, G.Yoganjaneyulu4, Sudhan Raj Jeganmohan5
8 1
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Department of Mechanical Engineering, Rajalakshmi Institute of Technology, Chennai, Tamil

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10 Nadu, India
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12 Department of Mechatronics Engineering, Tishk International University, Erbil, KRG, Iraq
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14 Department of Automobile Engineering, Saveetha School of Engineering, SIMATS, Chennai,
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Tamil Nadu, India
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17 4
Department of Mechanical Engineering, Vignan’s Institute of Information Technology,
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19 Visakhapatnam, Andhra Pradesh, India
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21 Department of Mechanical Engineering, Karunya Institute of Technology and Sciences,
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Abstract
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Coimbatore, Tamil Nadu, India
*Corresponding Author Email: g.saikrishnan@gmail.com

The idealization of this research work is to extend the utilization of the naturally available fibers
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29 as a key ingredient in the development of a non-asbestos free brake pad. The fibers used in this
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31 work are Caryota urens, which is found all over the Asian regions and abundantly available. The
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33 compression molding machine was used to develop the non-asbestos free brake pad. The fibers
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were added in weight percentages of 5, 10 and 15. The various physical, chemical, and
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36 mechanical properties were evaluated. Chase test rig was used to evaluate the tribological
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38 properties. The combination of Caryota urens fiber with the barytes had a more significant
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40 influence on the tribological properties. The brake pad composites with ten weight percent of
41 Caryota urens fibers based brake pads possessed a good coefficient of friction values with less
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43 fade values and less fluctuations. Increasing the weight percentage of Caryota urens fibers in the
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45 brake pad formulation had a decreasing trend in the wear performance but increased recovery
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properties.
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48 Keywords: Caryota urens Fibers (CUS Fibers), Brake pad Composites, Chase Test
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52 1.Introduction
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53 The purpose of brake is to stop or slow down the vehicle at the required period. The stopping
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55 of vehicles takes place due to the frictional surfaces between two mating services. Frictional and
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3 wear resistance are the important parameters of the brake pad for better operation [1]. The brake
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5 pad generally consists of 13-15 ingredients that are used to satisfy the required frictional
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7 properties [2,3]. They are generally classified as binders, fillers, friction modifiers (abrasives and
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lubricants), and reinforcements. Fillers are used further classified as inert and functional. Initially

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10 the era of brake pad started by using the asbestos as the predominant material. Later it was
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12 identified as carcinogenic, so replacement of asbestos came into existence. Owing to the concern
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14 about eco-friendliness many researchers are showing interest towards the natural fibers which are
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available and present abundantly. Due to its unique advantages as excellent mechanical
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17 properties, lightweight, low cost and high strength it has been selected as the best alternative for
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19 various synthetic fibers. In recent years many natural fibers were used in multiple applications
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21 such as automobile, household appliances, textile industries, aerospace industries, etc. The
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various natural fibers used for various applications are jute, kenaf, bamboo, hemp, flax, cotton,
areca, Tridax procumbens, Cardiospermum Halicababum etc.[4-7]. These natural fibers are
selected based on the ease of availability and its effectiveness in its applications. It is used in
different applications by changing the physical, chemical properties and biocompatibility nature
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29 [8,9]. The different types of fibers were used, such as short fiber, long fiber and chopped short
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31 fiber for its applications. To have better wear resistant the short random fiber is appropriate.
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33 Though natural fibers have many advantages it also has various other disadvantages on the other
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hand such as decreased mechanical property, stiffness and varying strength which is enhanced
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36 using various techniques like chemical treatment [10,11]. Suryarajan et al. [12] investigated the
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38 fade and recovery performance of the silane treated, alkali-treated and untreated Prosopis
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40 juliflora fibers based brake pads using Chase test as per SAE J661a. It was found that silane
41 treated Prosopis juliflora fibers based brake pads with five weight percent performed better
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43 tribological performance. Saikrishnan et al. [13] developed various weight percentages of areca
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45 sheath fiber-based brake pads for automobile applications. It was found that brake pads with five
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weight percent of areca sheath fibers showed excellent tribological properties compared to other
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48 brake pads. Tej Singh et al. [14] investigated the various weight percentages of ramie fibers on
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50 the tribological performance of brake friction composites using Chase test rig. The test results
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52 showed that five weight percent of ramie fibers based brake pads performed better in the
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53 tribological testing compared to other developed composites.

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3 The CUS fibers are commonly called solitary fishtail palm, toddy palm, wine palm, or
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5 jaggery palm. It belongs to Arecaceae family and found in regions of South India and South Asia
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7 countries. It can grow up to a medium-sized of 20 m tall like palm which has branched and
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having an extension at internodes. The study on mechanical properties of the CUS fibers in the

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10 polyester composites was already explored. The current study is to investigate the CUS fiber as
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12 reinforcement in brake pad applications. The percentage of fibers were chosen based on the
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14 previous literature [15]. The brake pads were developed as per standard practice. The developed
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brake pads were analyzed for physical, chemical, mechanical and tribological properties as per
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17 industrial standards.
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19 2. Materials and Methods
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21 2.1. CUS fiber extraction and brake pad development
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The CUS fiber used in this work was sourced locally from Chennai, Tamilnadu, India. The
extraction of fibers was done using water retting process. After extraction, the fibers which were
at the inner side were again separated from the outer sheath manually. The CUS fibers were
again thoroughly washed, and the moisture content was removed by heating in a hot air oven at
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29 50°C for 5 hours. Then the brake pads were developed using a friction material formulation
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31 possessed 15 parental ingredients namely fibers with additives (11 weight%): acrylic fiber, rock
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33 wool fiber, steel fiber, hydrated lime, binders with additives (16 weight%): phenolic resin, NBR,
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crumb rubber, CaCO3, frictional modifiers (18 weight%) graphite, silicon carbide, and fillers of
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36 (15 weight%) mica, friction dust, tin powder. The barytes, CUS Fibers are the varying
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38 ingredients and its formulation weight percentage are given in Table 1.The conventional method
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40 was used to develop the brake pad, and its details are given in Table 2 [16-20]. The developed
41 brake pad is shown in figure 1.
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43 Table 1 Designation of brake pads and its weight percentage
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45 Sl.No Ingredients of the Composites Designation of developed brake pads
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CUB1 CUB2 CUB3
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48 1 Varying CUS fibers 5 10 15
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50 2 Ingredients Barytes 35 30 25
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52 3 Parental ingredients 60 60 60
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55 Table 2 Sequential Procedure Followed in developing composites [16-20]
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4 Procedure Conditions

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6 Sequential mixing in Total duration 20 minutes, shovel and chopper speed: 140 and 2800
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plough shear rpm. 1kg mix was prepared. Mixing sequence is fibers (10 minutes),
9 (lodigee) mixer friction modifiers & fillers (6 minutes), binders (4 minutes).

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11 Compression Moulding machine with six mold cavities was used, Die
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13 temperature was set to 145ºC; Compression Pressure 13 MPa; Each
14 Curing in hydraulic
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cavity filled with 80 grams of mixture; Curing Time: 7 minutes; Five
cure press
16 intermittent breathings for removing volatile gases evolved during

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18 curing
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20 Post curing 5.5 hours at 160 °C in a hot air oven
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22 Finishing Grinding of the baked pad in the belt grinder
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Figure 1 Developed Brake Pads
38 2.2. Characterization of the developed brake pads
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40 2.2.1 Physical, chemical and mechanical characterization of the developed brake pads
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42 The physical and mechanical properties of the developed brake pad composites were assessed by
43
using industrial standards and the details are given in Table 3 [21-25].
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45 Table 3 Measurement procedure of various Physical, Chemical And Mechanical properties [21-
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47 25]
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49 Composite Property Procedure/ Standard
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CUS Density (Machine: Digital
51 The test was performed as per IS 2742 Part 3
52 Brake Pad density measurement
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53 based on Archimedes principle

54 (CUB) apparatus)
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3 Acetone extraction
4 The test was performed as per IS 2742 Part 3

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5 (Machine: Soxhlet
6 was the uncured resins percentage was found
7 extraction apparatus)
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9 The test was performed as per IS 2742 Part 3

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10 Ash content( Machine: where the brake pads samples of 10 grams
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12 Muffle furnace) were placed in a muffle furnace for 2 hours at
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14 800°C
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The test was performed as per IS 2742 Part 3.

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17 K scale was considered in which the ball
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19 Hardness (Machine: indenter was made of steel having dia 3.125
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21 Rockwell hardness tester) mm, the load applied was 1500 N at ten
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andifferent
reported
portions. Average values

This test was performed as per JIS D 4418.

The samples were dipped in SAE 90 oil heated
were
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29 for 24 hours and the weight was noted. Then it
30 Porosity
31 was wiped out with filter paper to remove the
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33 oil. Then the weight was noted. The difference
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35 was noted.
36 Test carried out based on ISO-6312 at room
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38 temperature conditions. In this test, the
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40 developed brake pad with the backplate was
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placed in the shear testing fixture. A side load
Shear strength
43 was applied to the brake pad surface while
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45 another load was applied in a perpendicular
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direction using a rammer. The load was
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applied gradually until failure.
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50 2.2.2 Estimation of the tribological performance by using Chase test rig
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52 The Chase test rig was used to determine the tribological properties of the developed brake pads.
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54 The IS2742 part 4 was followed for evaluating the tribological performances. Initially, the
55 burnishing was carried out. In order to make good contact between the samples and drum
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3 burnishing was done. It was done at the standard 308 rpm for 20 minutes time until the saturation
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5 temperature reaches 93°C. After completing burnishing process the baseline cycle was initiated.
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7 A temperature between 82 to 104°C was maintained. It was done as per the procedure at 411 rpm
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and a load of 660 N. After that the speed and the load were kept constant, fade, and recovery

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10 were measured. The detailed procedure is presented in Table 4 [25-27]. Finally the wear loss was
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12 calculated as per the change in weight observed in the digital weighing balance.
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14 Table 4 Experimental procedure of the Chase test as per IS2742-Part-4
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16 Temperature Off

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17 Speed Load On time No. of
18 Cycles (°C) time Heater Blower
19 (rpm) (N) Applications
20 min max min sec sec
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22 Burnish 308 - 93 440 20 - - 1 Off Off
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Initial
Baseline
Fade-I
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411
82

82
104

289
660

660
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-

10
10

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-

-
20

1
Off

On
Off

Off
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29 Recovery-I 411 261 93 660 - 10 - 1 Off On
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31 Wear 411 193 204 660 - 20 10 100 Off Off
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33
Fade-II 411 82 345 660 10 - - 1 On Off
34 Recovery-
35 411 317 93 660 - 10 - 1 Off On
36 II
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38 Final
411 82 104 660 - 10 20 20 Off Off
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40
Baseline
41 3. Results and Discussions
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43 3.1. Physical, Chemical and Mechanical properties of CUS fibers based brake pads
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45 The physical, chemical and mechanical properties of the CUS fibers based brake pads are
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evaluated and given in Table 5. The CUB1 has the highest density of 2.39 g/cc which is higher
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48 compared to the other two composites. This is mainly due to the higher density of the barytes
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50 which is 4.1 g/cc that is higher than the natural fibers. This is in tandem with the literature
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52 findings of Lenin Singaravelu et al., 2019[28] where crab shell powders were replaced by
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53 synthetic barytes in the brake friction formulation. The increase in CUS fibers decreased the
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55 hardness which is due to the presence of barytes in less weight percentage that doesn’t fill the
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3 pores that are essential for effective braking. Similar results were seen in the literature findings
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5 of Lenin Singaravelu et al., 2019 [18]. The better curing is seen in the CUB3 composite due to
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7 the less hardness that enables effective heat penetration during curing. This effect can be seen
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from the lower acetone extraction value. Ash content shows the decreasing trend value with

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10 increase in the fiber content. This is attributed due to the thermal stability of the barytes
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12 compared to the natural fibers [29]. It is a postulate that higher the density, hardness then there
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14 will be lower porosity [30,31]. Similar behavior is seen in the current study, where the baryes
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being smaller in size fill the space thereby reducing the porosity in the case of CUB1, while the
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17 natural fibers which increase the volume show higher porosity as in the case of CUB3. The shear
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19 strength for CUB3 is higher compared to other two composites which are mainly due to the
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21 better adhesion of friction materials layer with the backplate caused by effective curing of the
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Babu, 2019 [19, 33].

Properties Unit
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composite. These can be inferred from the literature findings of Vijay et al., 2019 and Ganesh

Table 5 Physical, Chemical and Mechanical characteristics of the developed friction composites
Standard CUB1 CUB2 CUB3
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29 Density g/cc 2.39 2.32 2.28
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31 Hardness No Unit 105 97 91
32 IS 2742 Part-3
33 Acetone Extraction % 1.204 1.195 1.183
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35 Ash Content % 83.26 81.79 79.21
36 Porosity % JIS D 4418 4.3 5.24 5.57
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38 Shear Strength N/mm2 ISO 6312 442.3 451.2 456.2
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42 3.2. Tribological properties of the developed CUS fibers based brake pads
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44 The tribological properties of the developed brake pad composites are done with the help of the
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Chase test rig and the output graphs of fade and recovery are given in figure 2. Among the tested
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47 brake pads, CUB1 showed the constant frictional values till 177°C and later got decreased. After
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49 this a gradual reduced is observed, and then it went down at the end of the test without much
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51 difference for the CUB2 composites. Thus there is the marginal difference among the
52 composites. CUB3 showed increased frictional value till 149°C and later it decreased down
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54 marginally. During the first fade rate the all the developed brake pads showed drastically µ
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56 decrease, whereas during the second fade rate all the brake pad composites had a high frictional
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3 value at the temperature above 250°C and decreased slowly. Further, a slight decrease in the
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5 frictional values is observed above the 280°C for all the three composites. In the second
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7 recovery, frictional values are higher till a temperature of 289°C. CUB1 showed a marginal
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decrease in the frictional value above 260°C, whereas the composites with CUB3 decreased

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10 vigorously. All the frictional values are within the industrial range (0.3 to 0.55) as per the
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12 literature [29]. The fade and recovery showed similar trends. Out of all the three composites the
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14 CUB1 and CUB2 had a slight decrease in the values above 260°C whereas CUB3 showed a
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phenomenal reduction in the frictional values above 205°C. This is mainly due to increase in µ
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17 during fade cycles is due to the least thermally stable natural fibers compared to more thermally
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19 stable barytes in the frictional formulation. But the trend got reversed in the recovery cycles
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21 since the porosity of the brake pads helped to regain the friction value drastically by removing
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the heat at the interface thereby sustaining the brake pads from transfer film formation by
pyrolysis and other abrasive mechanisms. This is tandem with the literature findings of
Manoharan et al., 2019 and Vijay et al., 2019 [23, 29].
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56 Figure 2 Response in friction during (a,b) fade 1&2 ; (c,d) recovery 1&2 cycles.
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3 3.2.1. Frictional performance parameters
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5 The frictional behavior of all the developed composites is observed and given in figure 3. All the
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7 developed composites µ are well within the industrial range as specified in the literature [23].
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The µ hot values will be lesser than µ normal values as per the literature [22] similar trend is also

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10 seen in the current study. µ Performance was measured by taking the average of both fade and
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12 recovery test runs. The minimum coefficient of friction was taken from both the fade cycles and
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14 highest coefficient of friction was obtained recovery cycles. The µ performance and μ Fade are
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between 0.33–0.370 and 0.345–0.365 respectively and it showed decreasing trend on increasing
16

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17 the CUS fiber, and it is presented in the figure below. This is mainly due to degradation of least
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19 stable ingredients at higher temperatures. From figure 3, it is witnessed that the performance
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21 coefficient of friction and fade possessed increasing values for CUB1 and CUB2; later on it
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decreased by increasing the fiber content and reduction in thermally stable barytes [29]. This
thermally stable barytes also plays a vital role in film formation that protects the braking
interface prone to further degradation of least stable ingredients and contact plateaus from further
disintegration. The µ recovery showed an increasing trend due to the better porosity which
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29 helped to prevent degradation causing pyrolysis [30-32].
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55 Figure 3 Friction performance parameters of the developed brake pads
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3 3.3 Wear performance and worn surface morphology of the brake pads
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5 The wear performance is a combination of different mechanisms that are thermally activated. In
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7 this work increasing the content of the CUS fibers increased the wear rate. The wear for all the
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composites remains in the range between 1.29 for CUB1 and 1.39 for CUB2 and 1.57 for CUB3.

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10 The increase in the wear is attributed due to the increasing content of the CUS fibers with the
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12 reduction in thermally stable barytes [29]. Thus optimal percentage of CUS fibers has beneficial
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14 effects on the wear performance. It can also be due to the more amount of CUS fibers that were
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added in CUB3, caused fibers agglomerated and peeled off, thereby increasing the wear rate.
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17 Higher the hardness increases the wear resistance in certain cases for brake pads; similar
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19 behavior is also seen in this study [33].
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21 The worn surface analysis of the Chase tested brake pads are analyzed and discussed below in
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figures 4(a-c). The wear debris and small pits, groves are observed in all the tested brake pads. It
is formed due to the scattered particles. The formation of contact plateaus and transfer patches
are mainly due to the fibers, thermally stable, and least stable ingredients which in turn control
the tribological properties of the brake pads. The wear debris also depends on these fibers. The
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29 transfer patches are seen in all the composites but more in CUB3. This is due to the reduced wear
30
31 resistance of CUB 3 when compared to CUB1. Thus CUB3 SEM images 4(c) shows a lot of
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33 wear debris and severe damages on the tested surface. While in the case of CUB1 as shown in
34
figure 4(a), there exist transfer patches and film formation which helps to prevent the pyrolysis
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36 and further degradation of ingredients leading to good wear resistance. CUB2 as shown in figure
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38 4(b) performed slightly lower than CUB1.
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32 Figure 4 SEM images of Chase tested brake pads (a) CUB 1; (b) CUB 2; (c) CUB 3
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34 4. Conclusions
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36 Caryota urens fibers based brake pads were fabricated by compression molding technique and
37 physical, chemical mechanical and tribological properties were evaluated. The following
38
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39 conclusions were drawn.

40
41 • The density, hardness, ash content got decreased with an increase in Caryota urens fibers in
42
43
the brake pads while the shear strength, porosity got increased.
44 • The brake pads with 10 weight percent of Caryota urens fibers showed better frictional
45
46 performance especially in the fade, performance, and normal µ, while the 15 weight percent
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Caryota urens fibers showed better recovery µ.
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49 • The wear performance was better in the case of 5 weight percent Caryota urens fibers
50
51 based brake pads compared to the other two developed brake pads. This behavior can be seen
52
from worn surface images that shows film and transfer patches.
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54 Thus Caryota urens fibers can be optimally used in the brake friction materials formulation as a
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56 reinforcement.
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1
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3 References
4

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5 [1]Chan, D., & Stachowiak, G. W. (2004), “Review of automotive brake friction materials”,
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7 Proceedings of the Institution of Mechanical Engineers, Part D: Journal of Automobile
8
9
Engineering, Vol.218 No.9, pp.953-966.

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10 [2]V Vineeth Kumar, S Senthil Kumaran Friction material composite: types of brake friction
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12 material formulations and effects of various ingredients on brake performance–a review Mater.
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14 Res. Express 6 (2019) 082005
15
[3]Aranganathan, N., & Bijwe, J. (2016), “Development of copper-free eco-friendly brake-friction
16

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17 material using novel ingredients”, Wear, Vol.352, pp.79-91.
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19 [4]Vijay, R., Lenin Singaravelu, D., Vinod, A., Sanjay, M. R., Siengchin, S., Jawaid, M., Anish
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21 Khan & Parameswaranpillai, J. (2019). Characterization of raw and alkali treated new natural
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26
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cellulosic fibers from
macromolecules, 125, 99-108.
Tridax

an
procumbens. International journal of biological

[5]Jafrey Daniel D, G Sai Krishnan and P Velmurugan Investigation on the characteristics of

bamboo/jute reinforced hybrid epoxy polymer composites Materials Research Express Vol.
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29 6,No.6(2019).105346
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31 [6]Jothibasu, S., Mohanamurugan, S., Vijay, R., Lenin Singaravelu, D., Vinod, A., & Sanjay, M. R.
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33 (2018). Investigation on the mechanical behavior of areca sheath fibers/jute fibers/glass fabrics
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reinforced hybrid composite for light weight applications. Journal of Industrial Textiles, 00, 1-
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36 25.
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38 [7]Vinod, A., Vijay, R., Lenin Singaravelu, D., Sanjay, M. R., & Siengchin, S. (2019). Extraction
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40 and Characterization of Natural Fiber from Stem of Cardiospermum Halicababum. Journal of
41 Natural Fibers, 00, 1-11.
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(2019). Characterization of raw and benzoyl chloride treated Impomea pes-caprae fibers and its
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Polyester composites. Journal of Engineering and Applied Sciences, 13(12), 3920-3928.
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performance of copper-free brake pads. Industrial Lubrication and Tribology, 71(3), 398-405.
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