Development of Polymer-Based Hemp and Colemanite Composite as a Friction Material

doi:10.21203/rs.3.rs-4116660/v1

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Development of Polymer-Based Hemp and Colemanite Composite as a Friction Material

https://doi.org/10.21203/rs.3.rs-4116660/v1

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published 02 May, 2024

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Natural and organic-based composite materials are widely used in many industrial applications due to their low cost, easy recyclability, economic feasibility, and ready availability. In this study, a polymer-based composite friction material consisting of Hemp-Colemanite composition (HCFCo) has been developed for the automotive sector to exhibit lower cost, environmentally friendly characteristics, and suitable friction-wear behaviors. For this purpose, three different ratios (%4, %8 and %12) of HCFCo composites were produced using a coating technique called impregnation process with a specially designed device. During the production stage, homogeneity of the composites was ensured, and then the final shape was given by the hot pressing method. Properties such as hardness, density, water and oil absorption, friction coefficient, and specific wear of HCFCo samples were examined. In addition, the microstructures of HCFCo composites were investigated to determine the bonding form between hemp fiber and colemanite. The results obtained revealed that the friction coefficient values decreased with an increase in temperature, while no significant change was observed in hardness and density values. Throughout the entire testing process, the friction coefficients varied between 0.14 and 0.29 on average. It was concluded that the developed fiber-reinforced composite can be reliably used in industrial applications and can contribute significantly to innovations in the literature.

Composite materials

Hemp

colemanite

friction and wear

In manufacturing industry, the demand for composite materials is rapidly increasing. Particularly in the automotive industry, the use of natural fiber and filler materials in the production of friction composites is preferred due to their biodegradability, low density, heat resistance, wear resistance, and desired friction coefficient [1–4]. Powder materials such as natural hemp and colemanite, a boron derivative, are used for different purposes in organic-based composites. Hemp, known for its resilient fiber, has low production costs and renewable characteristics [5]. Fu et al. [6] developed a new friction composite using structurally similar flax fiber instead of hemp fiber. In their study, the friction performance of the composite developed with flax fiber was evaluated based on temperature dependence. As a result, a significant improvement in the wear rate was achieved while stabilizing the friction coefficient. Colemanite, on the other hand, is a material that enhances the durability of materials and prolongs their lifespan. Especially, colemanite is preferred as a composite friction material because of its widespread use in the development of heat resistance, wear resistance, high strength properties, and better friction coefficient [7]. Sugözü et al. [8] investigated the friction and wear behavior of untreated boron derivative ulexite and cashew in their studies. It was observed that the composites had a more homogeneous structure with heat treatment, an increase in hardness values, and a decrease in density. From the results, a proportional change in the average friction coefficients of the composites was concluded. Researchers [9, 10, 11] obtained fibers and powders from various chemical processes applied to agricultural wastes (such as palm kernel, palm kernel shell, periwinkle, and coconut shells). By adding these natural-based powders to epoxy resin, graphite, ceramics, and calcium carbonate, they developed new types of composites. Through mechanical, chemical, and tribological tests, they ensured the low-cost and high-performance introduction of waste into industry. In Singh et al.'s [12] research, wollastonite, a non-asbestos fiber filler, was aimed to be used in friction composites and tested and evaluated as a friction composite. They examined the mechanical and tribological properties of friction composites under different parameters, focusing on the ratios of wollastonite in fiber and powder form. It was found that wollastonite in powder form had better friction and wear values than wollastonite fibers. Considering low wear and friction fluctuations, wollastonite fibers yielded better results. In the studies by Öktem et al. and Akıncıoglu et al. [13–15], brake pad samples were developed with powders of natural origin. In their studies, researchers examined the mechanical, chemical, and tribological properties of the samples and evaluated the friction performance with a specially designed test system. The results showed that the measured hot friction coefficient values were higher than the cold friction coefficient values, and there was more stable friction with 1000 braking cycles. Additionally, when the microstructure of brake composites was examined, it was observed from SEM images that the mixture was homogeneous, and wear residues in the friction layer were attributed to steel and brass fibers. Lien et al. [16] conducted a study on asbestos-containing (ABP), non-asbestos-containing (NABP), and commercial samples to obtain and evaluate friction coefficient, temperature, and wear values under sliding speed, nominal contact pressure, and sliding distance. According to their results, the effect of sliding speed was the lowest in three different samples. Due to friction, as the temperature increased, a decrease started in all samples. Glass wool is found in almost all recipes developed for materials against friction. Glass wool is used in thermal and sound insulation and high-temperature applications. However, it is relatively expensive and can cause some health problems due to certain allergies. In this context, in this study, recipes were prepared for hemp fibers, which are organic waste, as an alternative to glass wool. In this study, a new type of friction composite was developed using natural fiber hemp and colemanite, a boron derivative. Hemp fiber was passed through a chemical solution (polymer and colemanite), and their surfaces were coated with colemanite. A specially designed impregnation device was used for this process. The developed composites were subjected to all tests specified in standards, including mechanical, physical, and tribological evaluations.

In this study, a specially designed new type of device, not previously used in the literature, has been developed to coat natural hemp fibers, selected for use in composites subjected to friction, with colemanite and polymer materials prepared in a chemical solution under specific conditions. All the methods and strategies required for this purpose have been detailed in the following sections.

2.1. Impregnation method

Impregnation is defined as a coating process, involving the penetration of a freshly prepared mixture with chemical substances tailored for the desired purpose into another material. It is applied to materials such as wood, brick, stone, fabric, or fibers. Some of these applications are for protective purposes, while others aim to obtain new materials with different characteristics [17]. In this study, the goal is to develop a superior and cost-effective friction material by obtaining Hemp-Colemanite Composite (HCFCo). A composite was obtained by passing hemp fibers through a prepared fresh mixture.

2.1.1. Impregnation device

In this study, a new impregnation device was specially designed and developed. To carry out the impregnation process, a fresh mixture was first prepared. For obtaining this mixture, a mixer named PLANET type was preferred. In these types of mixers, the mixing blade is held at the center and is given a rotating motion by a rotating arm. As the main shaft rotates around its axis, it is circulated around the inner circumference of the mixing bowl to achieve a homogeneous mixture. It is called PLANET because it resembles a planet rotating around the sun. These types of mixers are used for dry mixing, dough mixing, and similar processes. If solid/solid, solid/liquid, or liquid/liquid substances need to be mixed in different proportions and densities, the PLANET mixer can achieve the desired characteristics of the mixture. Technical information about the mixer used is as follows: Volume; 20 liters, speed; 0-360 rpm, mixing time; 30–60 minutes, and motor; 1.5 KW (380 V, 3 Phase). In the scope of this study, the special impregnation machine is shown in Fig. 1. Electronic circuits and sensors were used to ensure the movement of hemp fibers in the desired direction and the realization of process conditions in the impregnation test device. Arduino UNO was used for the control of electronic circuits and sensors. With Arduino, the impregnation test device was programmed to control the movement of hemp fibers using a NEMA 17 stepper motor. The stepper motor provides the rotational movement of the hemp fiber collecting pulley with belt pulley power transmission. In the impregnation test device programmed with Arduino, the control of the liquid pump motor providing raw material replenishment from the pool, and data flow control with the liquid temperature sensor was ensured. The control of the infrared sensor to detect the breakage of hemp fibers on the impregnation path, and the control of the mixer fan DC motor providing continuous homogeneous mixing in the pool, was achieved. The control of the resistance heater fan ensuring the drying of impregnated hemp fibers, and the control of the Bluetooth sensor enabling remote communication, was also provided. The control of the circuit boards was programmed in the Arduino IDE programming language.

2.1.2. Preparation of impregnation mixtures

The preparation of the HCFCo composite was carried out by passing 1400 Tex hemp through an impregnation bath prepared as a fresh mixture. The materials constituting the impregnation bath, as listed in Table 1, were mixed in a fresh mixer until the appropriate density value was achieved. An important aspect here is to maintain the density obtained throughout the impregnation process. This density value is continuously measured and controlled using the BAUME degree [18].

Table 1

Formulation of impregnation process
Materials	Quantity (kg)
Phenolic resin	5.20
IPA (Izoprophilealchol)	11
NBR rubber	1.2
Chalk powder	0.6
Friction dust	1.2
Kolemanit (granule)	1.2
Al₂O₃ (Alumina)	0.6
Cr₂O₃ (Chromium oxide)	0.2
Carbon black	1.2
Total	22.4 kg

In the impregnation process with HCFCo, a homogeneous fresh mixture was obtained under the conditions of t = 60 min, T = 20°C, n = 900 rpm, as specified in the recipe. It is crucial to maintain density and viscosity values during the application of the process. The mixture was transferred from the mixer to a basin (with a volume scale of 10 liters), and the environment was prepared for the process. The hemp coil obtained as 1400 Tex was passed through a bath (solution) at a speed of V = 6 ± 0.5 m/min to ensure coating. The amount of mixture absorbed by the hemp rope onto itself was desired to be 2.5 times its unit weight, and this was determined through measurements. The measurement process involved taking the difference between the weight of a 1 m hemp rope and its weight after passing through impregnation (Amount absorbed = 4.9–1.4 = 3.5 g/m > > 3.5 g/1.4 g = 2.5 times).

Throughout the impregnation process, changes in the mixture's density and viscosity were measured using the BAUME degree to ensure that the desired values were maintained with the addition of the mixture. Subsequently, the hemp rope that underwent impregnation was dried by passing it through a unit with hot air blowing (150°C). With this drying process, HCFCo was wound onto a coil, resulting in a new type of friction material with natural additives.

2.2. HCFCo composite mixtures

In this study, three different recipes were created by adding chopped hemp fibers, coated in the developed friction composite, into three different compositions, apart from the commercial recipe (Table 2). In this context, at the initial stage, three substitute friction recipes were created in response to a commercial recipe. By obtaining the Hemp-Colemanite (HCFCo) composite, it will be possible to examine the use of this composite in friction materials through two different applications and observe the results. The application is based on the comparison of the substitute recipe formed by adding chopped HCFCo in different proportions with a commercial recipe through tests. It also involves testing and comparing the results of friction materials obtained by using 100% HCFCo.

Table 2

Samples and mixtures (%)
Materials	Commercial material	ISM-1	ISM-2	ISM-3
Phenolic Resin	8.5	8.5	8.5	8.5
Barite (BaSO₄)	32	32	32	32
Rock wool	22	18	14	10
HCFCo	-	4	8	12
Graphite	9.5	9.5	9.5	9.5
NBR- Rubber	7	7	7	7
Al₂O₃	3	3	3	3
Vermiculite	10	10	10	10
Iron Powder	6	10	10	10
MgO	2	6	6	6

2.2.1. Mixture process of composites

The modified commercial vehicle friction material recipe (Table 2) and the target friction material recipes were mixed in a mixer (Lodige mixer in Fig. 2,) until 95% homogeneity was achieved. The homogeneity of this mixture was ensured by first ensuring that equal volumetric proportions of dust samples taken from fixed amounts in different regions in a beaker were obtained. The mentioned criteria were applied to ensure precision in homogeneity. For this, 150 ± 2 g of dust samples were taken with a 500 ml beaker, and volumetric values of 100 ± 1 ml were obtained. Throughout this mixing process, five samples were taken from different regions. Additionally, mixing homogeneity was ensured through numerous trial and error attempts. Chandradass et al. [19] used a similar method for mixing sugarcane ash, an agricultural waste, in a composite.

2.3. Production of friction composites

The production of brake pads involved mixing, pre-forming, hot molding, and post-curing. Mixing was conducted in two batches to preserve the original shapes of the delicate raw materials and prevent potential thermal degradation during mixing. Pre-forming took place at room temperature under 35 MPa pressure, and hot molding occurred at 155 ºC under 35 MPa pressure for 10 minutes. The initial volume of the mixture was three times greater than that of the hot-pressed products. Post-curing, or heat treatment, was performed in a mechanical convection oven at 180 ºC for 7.5 hours. Following post-curing, the brake pads were finished using a polisher-grinder with grinding paper of various grit sizes to achieve the final products.

2.4. Friction testing procedure

A series of tests were conducted to determine the tribological performance of the Hemp-Colemanite combination composite friction material. The composite samples named ISM-1, ISM-2, and ISM-3 were subjected to measurements of friction coefficient and wear rate using a specially designed friction test apparatus (Fig. 3). The measurements were carried out according to the SAE-J661 (SAE, 2000) standard. The wear amount resulting from the friction was calculated using the weight loss or mass loss method [13, 20, 21].

To measure the densities of the friction composites, a RADWAG PS300 precision balance, operating on the Archimedes principle and compliant with ASTM D792 standards, was used. In addition to hardness and density tests, water and oil absorption tests were conducted on the developed samples to observe changes in swelling in water and oil environments. These tests were performed according to the ASTM D570-98 standard. Composite samples with dimensions of 25x25x10 mm³ were used for the oil and water absorption test. The hardness of the friction composites produced from recipes ISM-1, ISM-2, and ISM-3 was measured using a Shore D (ASTM D2240) method on a MACRON-brand device. Three measurements were taken from each of the six surfaces of each composite, and the average values were recorded.

3.1. Mechanical and physical properties

To determine the mechanical, chemical, and physical properties of the friction composites developed according to the recipes (ISM-1, ISM-2 and ISM-3), hardness, density, and water-oil absorption tests were conducted. The hardness results for the composites with dimensions of 25x25x10 mm³ are provided in Table 3. Upon reviewing Table 3, it can be observed that the values obtained in 12 hardness measurements for each recipe are very close to each other. Hardness values ranged from 62 to 69 Shore D. The hardness values of all samples were very close to each other, and the chemical composition change did not affect the hardness values. These results are consistent with findings from previous studies in the literature [9–11, 19, 22].

Table 3

Hardness of tested samples (Shore D)
Test numbers	Samples
Test numbers	ISM-1	ISM-2	ISM-3
1.	68	67	66
2.	67	64	63
3.	68	64	68
4.	65	66	65
5.	65	63	66
6.	63	64	64
7.	65	65	66
8.	68	65	63
9.	69	66	64
10.	64	65	66
11.	63	65	64
12.	68	65	62
Average	66.08	64.92	64.75

Density measurements were conducted for three types of recipes: ISM-1, ISM-2, and ISM-3. The averages of the results are presented in Table 4. Upon examining Table 4, it is observed that the density of the ISM-1 recipe is the highest. This is attributed to ISM-1 having the least HCFCo in its recipe. Since glass wool has smaller dimensions and higher density compared to hemp fiber, it affects the density of the composite material. Similar to hardness values, the three different samples exhibit similar densities. The densest sample corresponds to the highest hardness value. Similar results for different materials can be found in studies in the literature [23–25].

Table 4

Density of samples
Composite Code	ISM-1	ISM-2	ISM-3
Average density (gr/cm³)	2.5680	2.5667	2.5463

After soaking the samples in water and oil for 48 hours, total hardness and weight changes were measured (Fig. 4). In water and oil immersion, it was determined that the ISM-3 recipe samples underwent the greatest weight changes (Table 5). The least swelling occurred in the ISM-1 sample, with 0.16 g, while the highest water absorption appeared in the ISM-3 sample, which had the lowest density and hardness. Although the rate of weight increase was not as high in oil as in water, the same trend was observed in the oil-containing samples. Depending on density and hardness, the ISM-1 sample showed a weight increase of 6.25% in both water and oil, while the lightest and softest ISM-3 sample exhibited a weight increase of nearly 90%. Additionally, when looking at the difference in weight change between ISM-1 and ISM-3 samples in water, this ratio is around 33%, while in oil, it is approximately 17%. Table 5 gives the variations in hardness values of the samples. No significant changes were observed in Shore D hardness values for all three samples, and a slight increase in hardness was observed in the oil-containing samples. Overall, microstructure, density, and hardness changes directly affect many mechanical properties of the material [9]. Despite the limited number of studies in the literature, some researchers have emphasized the significant effect of water and oil absorption on reinforced composites [10, 11]. Chandradass et al. conducted similar water and oil absorption tests, and the results are close to those obtained in this study [19].

Table 5

Water and oil absorption of composites
Samples	Weight Gain (g)
Samples	Water	Oil	Change (%)
ISM-1	0.16	0.17	6.25
ISM-2	0.46	0.26	65
ISM-3	0.53	0.28	89.2
Change (%)	33.1	16.5	-

3.2. Tribological properties

As seen in Fig. 5, the friction coefficient value, dependent on temperature at a constant speed, has steadily decreased. The results in Table 5 were found to be close to literature values. While the ISM-1 sample had the highest friction coefficient at 160°C in the tests, at 260°C and 360°C, all three samples reached similar friction coefficients. However, looking at the wear values in Fig. 6, no difference was observed in tests at 160°C and 360°C for all three samples, while at 260°C, the ISM-3 sample exhibited the highest wear. This may be attributed to differences in hardness and density values. In some studies in the literature, an increase in temperature has been observed to partially increase the friction coefficient, which then rapidly decreases afterward [19].

Additionally, in some studies, similar changes have been attributed to the surface vitrification effect with an increase in the number of revolutions [26–32]. However, in tests at 850 rpm, as observed in Fig. 7, a regular decrease in the friction coefficient with increasing temperature was observed for all three samples. Under the specified test conditions, the best friction coefficient was again observed in the ISM-1 test sample. The highest friction coefficient at all temperature values was observed in the ISM-2 sample.

Figure 8 presents the wear rates for the same tests and samples. Similar to previous tests, wear increased with the rising test temperature for each sample. The highest wear was observed in the ISM-3 sample, while the least wear occurred in the ISM-1 sample, with the ISM-2 sample falling between these two values. Once again, density and hardness were major factors for this test and these samples. When compared with literature values, the test results were found to be within the desired ranges [13, 33–37]. The impact of temperature on the friction coefficient and friction rates of brake pad materials is also evident in the study by, where they studied the effects of brake pressure, initial braking velocity, and braking frequency on the average friction coefficient, stability coefficient of friction coefficient, wear rate, and average surface temperature [38]. It is highlighted that excessive heat exposure can lead to a decrease in friction coefficients within brake linings, consequently diminishing the stopping ability of brakes [39]. Furthermore, emphasized the variability of the pad friction-coefficient with humidity, the number of brake applications, and temperature changes [40]. These findings collectively underscore the significant influence of temperature on the friction characteristics of brake pad materials.

3.2. Microstructural evaluation of HCFCo composite

Figure 9 (a, b, c, d) shows typical SEM pictures of raw hemp fibers (a = 50 X, b = 100 X, c = 50, d = 125 X). Figure 10 (a, b, c, d) presents electron microscope images and an EDX analysis graph for raw hemp fibers. The main difference between both graphs is that Fig. 9 shows multiple hemp fibers, while Fig. 10 shows a 1000X magnification of a single hemp fiber.The results of the EDX analysis are shown in Table 6. Hemp, a natural cellulose fiber, contains hemicellulose, lignin, and pectin, which play a crucial role in determining the structural properties of the fiber, including water retention and strength. In untreated samples, fiber bundles displaying some splitting due to mechanical separation during carding are clearly visible. The average diameter of all fiber bundles was determined from the cross-section obtained from SEM pictures. The average diameter of raw fibers (20 µm) is significantly lower than the value reported by Sauvageon et al. [41] (41 µm). The average fiber lengths are in the range of 15–20 mm. Continuous and main fibers containing fine spiral fibers with a diameter of 2 microns can be observed in these images. Hemp fibers, composed of the basic elements C, N, and O, exhibit properties that can provide high tensile and abrasion resistance. Hemp is a bast fiber grown in temperate climates, contributing to various important products such as textiles, seeds (oil), and pulp and paper.

Table 6

EDX results of raw hemp fibers
Element	Weight %	Atomic %	Net Int.	Net Int. Error
C K	28.54	53.9	164.65	0.01
N K	4.04	6.55	8.76	0.14
O K	24.4	34.6	159.24	0.02
AuM	43.02	4.95	432.08	0.01

Figure 11 displays the microstructures of the HCFCo composite at four different magnifications (50X, 125X, 500X, and 1000X) and presents the corresponding EDX results. The EDX analysis for hemp fiber impregnated with colemanite is provided in Table 7. In contrast to Table 6, elements B, Na, Mg, Al, Si, Ca, and Fe are observed densely on the coating surface. Figure 12 shows the high magnification of hemp fiber and colemanite with EDX graph. From Fig. 12, it can be seen that hemp fiber and colemanite display a very good distribution in general matrix. Also from this here, good bonding has occurred between hemp fiber fiber and colemanite. In addition to this, EDX graph has associated with Table 7.

Wear surface images are shown in Fig. 13a. ISM-1, with the least wear and deformation, has been identified as the most dense and hardest material. In ISM-1, which contains only 4% hemp fibers uniformly distributed within the microstructure, ISM-3 with 12% hemp fibers has become the composite material subjected to the most abrasive wear, exhibiting the least hardness and toughness. Figure 13b shows some friction materials in sample. These materials were marked with help of their shapes and studies in litetature [3, 28, 29, 37, 41].

In this study, the aim is to develop a new type of composite with a polymer base using natural materials, specifically hemp-colemanite combination, and produce a composite that can be used in industrial applications according to internationally specified conditions. Throughout the study, the following results and achievements have been obtained:

• A special design impregnation device has been developed for coating hemp fibers. The distinctive feature of this system, despite various models in the literature, is its ability to pass the hemp fiber through a washing bath and then through the impregnation solution, facilitating the drying process. This allows for the production of a composite fiber with a more homogeneous and higher interfacial quality.
• HCFCo composites were produced by changing the weight ratios of rock wool while keeping other powders constant.
• As a result of hardness and density tests of the composites, there was no significant change in density values for ISM-1, ISM-2, and ISM-3 recipes. However, a better density value compared to the commercial vehicle friction material was achieved. On the other hand, when examining hardness values, a 2% change was observed in all three recipes.
• By measuring the density of ISM-1, ISM-2, and ISM-3 recipes, it was determined that the density of the ISM-1 recipe is the highest. The reason for this is that the ISM-1 recipe has the least amount of HCFCo (4%).
• As a result of friction tests of the composites, the coefficient of friction decreased with increasing temperature during all three tests. The coefficient of friction varied between 0.29 and 0.14 on average throughout the test process. It was observed that the decrease in the coefficient of friction during all three experiments was related to the increase in temperature.
• Abrasive and adhesive wear mechanisms were observed in the slip traces examined under an optical microscope on the worn sample surfaces.
• With the increase in temperatures to 160 ºC, 260 ºC, and 360 ºC while the speed was 850 rpm, it was observed that the coefficient of friction gradually decreased. The main reason for this is believed to be the formation of a glassy effect on the surface with the increase in speed.
• This developed friction composite can be used in industrial applications as a clutch lining, weaving lining in eccentric presses, and brake lining in marine vessels with high performance and reliability.

Acknowledgements

The authors express their gratitude to Engineer Mustafa Serdar at Apetech Automotive Trade in Gebze/Kocaeli.

Conflict interest

Authors declare no conflict of interest for this work/manuscript.

Author contribitions:

1. Hamdi Karakas: He made all experiments. (% 50 )

2. Hasan ÖKTEM: Writing and arraging. (% 25 )

3. İlyas UYGUR: Writing, arranging and discussion. (% 25 )

Funding:

There is no funding

Data avability:

All datas can be supplied by e-mails.

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No competing interests reported.

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published 02 May, 2024

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Development of Polymer-Based Hemp and Colemanite Composite as a Friction Material

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Abstract

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1. Introduction

2. Material and methods

2.1. Impregnation method

2.1.1. Impregnation device

2.1.2. Preparation of impregnation mixtures

2.2. HCFCo composite mixtures

2.2.1. Mixture process of composites

2.3. Production of friction composites

2.4. Friction testing procedure

3. Results and Discussion

3.1. Mechanical and physical properties

3.2. Tribological properties

3.2. Microstructural evaluation of HCFCo composite

4. Conclusions

Declarations

References

Additional Declarations

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