An Experimental Study on the Effect of Graphite Microparticles on the Mechanical and Tribological Properties of Epoxy Matrix Composites

doi:10.21203/rs.3.rs-2233985/v1

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An Experimental Study on the Effect of Graphite Microparticles on the Mechanical and Tribological Properties of Epoxy Matrix Composites

https://doi.org/10.21203/rs.3.rs-2233985/v1

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In this article, mechanical and tribological properties of epoxy matrix composites filled with graphite particulates of 100µm at loadings between 0-1wt% are comprehensively discussed. The effects of the graphite filler on the wear surface of the specimens was investigated using an optical microscope. Results showed a large decrease in the tensile strength of the composite by more than 50% for 1wt% graphite loading. Flexural strength was seen to increase sharply with 0.1wt% graphite before reducing with higher graphite content. Impact and hardness values are both improved with higher graphite content. Friction coefficient was seen to reduce with the addition of graphite particles, this was attributed to the solid lubrication abilities of graphite. Wear rate was seen to sharply reduce with increase in graphite content as a result of the lubrication layer developed at the contact surface hence reducing the break-off of the specimen.

Graphite

epoxy

composites

mechanical properties

tribological properties

Composite materials have opened doors into research for advanced materials and the opportunity to redesign conventional materials to make them cheaper or more aesthetically pleasing while also combining different properties to design materials with multiple functionalities. Polymeric materials filled strong inorganic materials can possess high stiffness with low weight and excellent wear and corrosion resistance. This is one of the features that makes polymeric composites a promising aspect of industrial application because of its ability to be tailored with functional fillers [1, 2]. It has been found that fibres in polymer matrix can improve strength and stiffness of the composite, particulates when homogenously mixed improve hardness and impact properties. Fillers generally improve the mechanical, thermal and tribological properties of polymer composites [3]. Many materials like glass, carbon and Kevlar have been made into fibres for reinforcing polymers, graphite, graphene and carbon black particles are also employed as fillers. Nano fillers are also widely used like silica, alumina, boron nitride, titanium oxide and carbon all as nano particles [4].

Epoxy is a thermosetting polymer having unique mechanical properties and a high chemical resistance. This makes it a versatile material for application in corrosive environments where metals can easily react and where weaker polymers cannot withstand [5]. Fibre reinforced epoxy matrix composites are one of the most used multi-phase materials mainly because of their outstanding strength-to-weight characteristics. Epoxy-matrix composite provide exceptional mechanical and tribological properties, outstanding dimensional stability and adequate chemical and corrosion resistance [6]. A common method of improving matrix properties involve the incorporation of fillers into the epoxy resin. From literature, it has been shown that fillers like nanoclay [7], silica [8], TiO₂ [9], glass beads [10], fly ash [11] etc. have been used as fillers for epoxy matrix composites and an improvement in stiffness, toughness, hardness, mould shrinkage, heat distortion temperature, wear rate and fracture mechanism were all observed. In some instances a significant reduction in processing cost was reported [12].

Integration of various functional fillers is an important route in the design of load bearing and wear resistant polymer composites. Baptista et al. [13] studied the mechanical properties of epoxy-matrix composite containing graphite filler. Graphite fractions between 5-30wt% were added in the epoxy matrix and the tensile strength was observed to greatly decrease while tensile modulus increase. This is associated to the high graphite particle content which lead to agglomeration and formation of both micro and macro pores. Kulkarni et al. [14] tried to enhance the mechanical properties of epoxy by adding graphite particles of about 75µm with weight fractions between 3 and 12%. They recorded an increase in the impact, flexural and fracture toughness of the composite by 100%, 59% and 19% respectively for a graphite content of 12wt%. El-Melegy et al. [15] investigated the synergistic effect of different nanoparticles hybridization on mechanical properties of epoxy composite where nanoparticles like graphite, silicon carbide and alumina were dispersed in an epoxy matrix. Results showed a 37% and 195% increase in the tensile and elastic modulus of 2wt% SiC/epoxy composite, 132% and 200% for 3wt% Alumina and 85% and 32% for a 2wt% graphite/epoxy composite. Alajmi et al. [16] investigated the tribological characteristics of graphite epoxy composites under adhesive wear experiments. Composites with graphite content between 0-7wt% were prepared and tested, it was found that wear and friction were best at graphite contents between 3-4wt% making it the optimum amount, anything less than that results in high friction and wear and anything more than that resulted in higher friction and wear rates. Sakka et al. [17] studied the correlation between friction coefficient and temperature for epoxy matrix composites filled with either carbon nanotubes, graphite or a hybrid of both, they concluded that there is a strong correlation between friction and temperature because the flash temperature measured at the beginning of the experiment was higher than the degradation temperature of the composite hence affecting the friction coefficient of the whole system. Considerable attention has been given on the incorporation of particles and fibres into polymer matrix to get better mechanical properties so as to be able to compete with metals and other high-strength structural members. This lead to the more than 30 years of investigation by researchers. Such works are presented in articles by Shalwan [18], Kaushik [19], Yasmin [20], Novak [21], Suherman [22], Yao [23] among others.

In this study, epoxy matrix composite filled with different fractions of graphite particulates having approximately 100µm were fabricated. Composites with layered structure are also developed after which mechanical and tribological properties of both composites were investigated. The adhesion of the layered specimen is also considered. This is also an attempt to find cheaper alternatives to fillers in polymers employed in a friction intensive system.

2.1 Materials used

Epoxy resin (KEMAPOXY 150) gotten from Chemicals for Modern Building (CMB), Cairo, Egypt with hardener with the ratio 2:1 was used in this study. Graphite particles sourced from EGYCARBON, Cairo was sieved and graded to the particle size of 100µm. Physical and mechanical properties of the constituents used in this study are given in Table 1.

2.2 Mixing and preparation

Two separate type of composite structures were developed in this study, the homogenously mixed (where the composite resin and the filler are mixed together) and the layered structure (where a layer is first poured of neat epoxy before a layer of graphite/epoxy composite). For the homogenously mixed composite, epoxy and hardener are mixed in a container according to the ratio and direction of the manufacturer (2:1), it was mechanically stirred for two minutes with a drilling machine using a coupled metal stirrer head. Graphite particles are added slowly into the mixture according to the graphite content while stirring so as to get a homogenous mixture and avoid agglomeration. Liquid composite is poured in a mould after 5 minutes of stirring. Specimen cured for 24 hours in room temperature are removed from the mould and allowed to continue curing for 5 days to reach its maximum strength. For the layered composite, the first layer of neat epoxy is poured into the mould and allowed to cure for 1 hour before another layer of either 0.1wt% graphite/epoxy or 1wt% graphite/epoxy composite is poured and allowed to cure together. Sample are then cut according to the dimension of the test to be carried out. Figures 1 and 2 shows the homogenous and the layered specimen. Tensile and flexural specimen were in a rectangular dimension of 25mm×8mm×270mm. Tribological specimen were cut into rectangular cubes of 10mm×10mm×30mm. Table 2 shows the designation of each specimen.

2.3 Mechanical properties

The tensile and flexural measurement were carried out using a universal tensile testing machine (iBERTEST, Spain model TESTCOM-100) according to ASTM D638 and D790 respectively. The tensile and flexural tests were both performed with a crosshead speed of 1mm/min. Three specimens were tested for each specimen range (Neat, 0.1, 0.5, 1wt%) and an average was taken. Hardness value was determined using a Shore D hardness tester where five points where randomly tested on the specimen to get the average hardness value. Impact tests were carried out using a Charpy impact testing machine according to ASTM D256.

2.4 Friction and wear test

A Block-on-Ring (BOR) test setup as shown in Fig. 3 was used for friction and wear testing in this study. The block specimen was 10mm×10mm×30mm in dimension and the ring was the stainless steel counterface (AISI 304, hardness 1250HB). Adhesive wear tests were carried out according to the G-77 ASTM standard at ambient conditions (temperature 25°C, humidity = 50 ± 5%) and a sliding speed of 200-400rpm and normal loads of 10,20 and 40N were applied.

Table 1

Physical and Mechanical properties of matrix and filler.
Polymer/filler	Density (g/cm³ )	Colour	Hardness	Modulus (GPa)	Temperature resistance (°C)
Epoxy resin	1.11 ± 0.02	Transparent	64.1 (Shore D)	3.42	150
Graphite	2.09–2.23	Dark gray-black	5 (Brinell Hardness)	8–15	2500

Table 2

Specimen designation
Designation	Epoxy (wt%)	Graphite (wt%)
Neat	100	-
0.1% G	99.9	0.1
0.5% G	99.5	0.5
1% G	99	1

3.1 Tensile behaviour

Tensile tests were performed on three specimens of each graphite/epoxy composite as well as the neat polymer. Typical engineering stress-strain curves are shown in Fig. 4. These curves illustrate evidence of brittle behaviour of all the specimens with and without graphite filler. It is clear that the mechanical properties of a composite are dependent on the characteristics of the filler used. In the present work, all composites exhibited lower tensile strength than the neat epoxy, the higher the graphite filler content, the lower the tensile strength measured. Tensile properties derived from the curves are given in Table 3. Results show that an addition of 0.1wt% graphite reduced the tensile properties of the neat epoxy by 32.7% (from 52.11MPa to 35.05MPa). This reduction is expected as graphite is a brittle material and its incorporation into the epoxy matrix makes the epoxy more brittle. A 43.5% reduction is also observed with the addition of 0.5wt% graphite particles. A final reduction of 56.03% was concluded with the specimen having 1wt% graphite particles. A similar trend was observed by Suresha et. al [3] in their study on the role of micro/nano particles on the mechanical and tribological properties of polymer composites. The strain at break for each specimen as given in Table 3 shows a drastic reduction in elongation with addition of graphite particles. This higher brittleness can be attributed to the increase in stress concentration areas as well as the reduced bonding between the matrix and the filler because with higher graphite content, agglomerates are generated which in turn help in developing micro cracks as well as air bubbles from where there is larger interfacial distance between matrix and filler as presented in Fig. 5. Additionally, the graphite micro particles may provide obstacles to cracks formed in the composite which results in a less convenient crack path which makes the fracture brittle.

Table 3

Tensile properties of graphite/epoxy composite
Specimen	Tensile strength (MPa)	Tensile Modulus (GPa)	Strain at break
Neat	52.11	2.96	0.0190
0.1% Graphite	35.05	3.0	0.0119
0.5% Graphite	29.41	3.08	0.0104
1% Graphite	22.91	3.26	0.0072

3.2 Flexural behaviour

3.2.1 Homogenously mixed composite

Flexural properties are of great importance for any structural element. Composite materials used in structures are prone to fail by bending and therefore the development of new composites with improved flexural characteristics as essential. Figure 6 shows the flexural strength of the homogenously mixed graphite/epoxy composites compared to neat epoxy. It is observed that all graphite epoxy composites exhibited higher flexural properties than the neat epoxy. This is as a result of the mechanism of load transfer from the matrix to the high-strength graphite particles in bending. This is not the case in tension because the stresses are in the opposite direction. The best improvement in the flexural properties of graphite/epoxy composite is with the addition of 0.1wt% graphite micro particles which increased the flexural strength of neat epoxy from 46.8MPa to 80.08MPa, this is a 71.1% increase. With a graphite content of 1wt%, increase in flexural strength compared to neat epoxy was 59.79MPa which was a reduction from the 0.1wt% and 0.5wt% graphite content but still an increase of 27%.

A comparison between tensile strength and flexural strength is shown in Fig. 7. Is can be clearly seen that the advantages of graphite as a filler are more prominent in bending than they are in tension. This was confirmed in literature were different inorganic fillers are added in a polymer matrix composite [24, 25].

3.2.2 Layered composite

The development of layered composites in this study is to determine the possibility of successfully bonding together different layers of epoxy and graphite/epoxy composites to have a new material that has different internal and external flexural properties. This investigation is so stiffer materials can be combined with a weaker material to reduce the general stiffness of the bulk material and to combine cheaper and expensive materials to reduce cost among other benefits. Figure 8 presents the flexural strength of the graphite/epoxy layered composites with regards to the neat epoxy. It is concluded that the best layered specimen in terms of flexural strength is the composite with a layer of neat epoxy and 0.1wt% graphite/epoxy composite which had a 64.8% increase compared to the plain neat epoxy. This is close to the improvement noticed with the homogenously mixed graphite/epoxy composite. The layered composite with neat + 1wt% graphite had the least flexural strength compared to the other layered specimens which was 49.9MPa. This is still an improvement compared to the neat epoxy by 6.6%. The specimen with a triple-layer of Neat + 0.1 + 1wt% graphite had a flexural strength of 61.28MPa. This is an encouraging output in the layered composites which means flexural properties can be improved with the layering of a composite with another composite that has better flexural properties. Failure of layered specimen were noticed to be a delamintion failure because of the clear interlayer debonding and the change of direction of crack path when propagating between layers as seen in Fig. 9.

3.3 Hardness and impact values

The hardness and impact values of all graphite/epoxy composites were improved with the addition of higher graphite content. This is expected as the graphite particles have a higher density, surface hardness and mechanical strength compared to the neat epoxy. Table 4 shows the hardness and impact values of the composites. It can be seen that the Shore D hardness value of neat epoxy was 50.36SHD, with the final addition of 1wt% graphite, hardness values increased to 64.6SHD, this is a 28% increase in the hardness value. For the impact strength of the composite, a 1wt% graphite content increased the impact value by 29%. These improvements can be attributed to the load transfer mechanism in a homogenously dispersed composite where the surface of the graphite particles become load bearing during compression (Shore D hardness testing) and hence prove to be hard. For the impact strength, the change in direction created by graphite particles as a crack propagated during failure reduces the ease of fracture and hence increases the toughness of the material. It has been reported in [26, 27, 28] that addition of high density and high strength inorganic particles enhance the surface hardness and the impact strength of a composite.

Table 4

Hardness and impact results
Specimen	Hardness value (SHD)	Impact value (J)
Neat	50.36	6.75
0.1% G	57.16	7.25
0.5% G	61.04	7.65
1% G	64.6	8.75

3.4 Friction and Sliding wear results

3.4.1 Friction

The friction coefficient of neat and graphite/epoxy composites are obtained under different conditions of operation. A sliding speed of 200 and 600rpm, applied loads of 10,20 and 40N and a constant time of 300sec. The coefficient of friction was obtained by dividing the frictional force by the applied load. In this study, it was observed that as applied load increases, the coefficient of friction increases for all composites and neat epoxy, this is to be expected as higher normal loads means the pressure exerted on the specimen and counterface increases and this increases the frictional force generated in the system. The lowest coefficient of friction was observed in the specimens with 1wt% graphite content for all applied loads and sliding speeds. For specimens tested at 10N applied load and 200rpm sliding speed, a reduction in the coefficient of friction of 14% was observed from the neat epoxy to the 1wt% graphite/epoxy composite as shown in Fig. 10. For specimen tested at 20N applied load and 600rpm sliding speed, it can be seen from Fig. 11 that the composite with the higher graphite content stared with a lower friction coefficient, a decrease of 12% was observed between the neat epoxy and the specimen with 1wt% graphite content, this is as a result of the ease with which the graphite particles come off with higher graphite content and form the lubricating film as discussed earlier [23]. This is also comparable to results recorded in experiments by [29, 30]. Similar trends are noticed in all other operational conditions as shown in Fig. 12. The reduction of coefficient of friction is most noticeable when applied load is changed, despite the effect of sliding speed on the coefficient of friction of the composites, very little change is observed. A more prominent effect is observed when higher loads are applied. An increase of 52% was noticed when the applied load is changed from 10N to 40N. A higher graphite content would certainly mean much lower friction coefficients but that will lead to instability of the composite as it becomes weak and crumbles easily due to the weak bonding between the matrix and the filler [31].

3.4.2 Wear

The variation of wear rate of neat epoxy and the graphite epoxy composites under different conditions are presented in Fig. 13. The experimental results show that the wear rate reduces with increase in graphite content as the specimen with 1wt% graphite exhibited a reduced wear rate compared to the neat epoxy of more than 75%. The difference was similar for the higher sliding speed of 600rpm which was 73% in reduction. This is as a result of the solid lubrication abilities of graphite particles [32]. An interesting trend that was observed in this study is the reduction of wear rate with increase in sliding speed. This can be attributed to the faster formation of a sliding film on the specimen and counterface which then reduces further disintegration of the composite, the film generated stabilises the stick-slip process which becomes a low adhesion region where the wear rates are low. But this trend was not in agreement with the conclusions in literature [33, 34]. But a study by Tripathy et al. [35] stated that wear rate increases with increase in sliding velocity but with an exception. In their research, there was a sharp decrease in wear rate at velocities ranging between 3–4 m/s but then increases exponentially up to 7m/s. It could be argued that the reduction in wear rate with increase in sliding speed in this research is still between the 3-4m/s decrease observed in the research above and hence acceptable. Figure 14 shows the specific wear rate of graphite/epoxy composite for 10N applied load at different sliding distances.

The Worn surface of the specimens tested during friction were studied to determine the wear mechanism and surface morphology. From Fig. 15, it can be seen that the difference between the worn surface of the neat epoxy composite was much more coarse and having deep scratches due to the high frictional force and the brittle nature of the epoxy while the composite with 1wt% graphite particle had a smoother surface even though some scratches where visible. These smooth scratches were as a result of the initial friction and break-off of the surface of the composite before a smooth lubrication film was generated which in-turn becomes a layer with low friction and less debris formation. This is in agreement with results gotten in previous studies on the review of tribological properties of polymer composite [36]. Worn surface of the specimen with graphite filler in higher quantity can be described as quality surface [37] because there is no sign of extreme debonding or high porosity. The relative appearance of micro cracks shows a good resistance to shear stresses displayed by graphite particles. Similar things have been reported with carbon fibre and epoxy polymer where there was relatively less damage than the glass fibre epoxy polymer [38]. In other words, it can be concluded that graphite has excellent properties in reducing both friction and wear rates in polymer composites.

The mechanical tribological properties of graphite filler epoxy matrix composite was investigated in this study and the following conclusions were drawn:

Graphite can be successfully incorporated into the epoxy resin to fabricate a particulate filler epoxy composite with homogenous mixing before agglomeration at higher percentages.
Mechanical properties are greatly influenced by the addition of graphite particles; tensile strength reduced with increase in graphite content with an addition of 1wt% graphite particle reducing the tensile strength by 56%, flexural strength was improved with addition of graphite but not in a linear path as the composite with 0.1wt% graphite had the highest flexural strength, hardness and impact values are both improved with higher addition of graphite particles.
Wear and friction properties were also influenced by the graphite particles; specific wear rate was seen to decrease with increase in graphite content, this is as a result of the solid lubrication capabilities of graphite. Friction coefficient was affected by both graphite content and the applied load, as higher applied loads meant higher friction coefficients and higher graphite content means lower friction coefficient. Wear track studied under a microscope shows a the worn surface to the composite with 1wt% graphite content to be smooth as the lubrication film developed during friction reduced the surface roughness of the system.

FUNDING

The authors declare that no funds, grants, or other support were received during the preparation of this manuscript.

COMPETING INTEREST

The authors declare no conflict of interest.

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No competing interests reported.

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An Experimental Study on the Effect of Graphite Microparticles on the Mechanical and Tribological Properties of Epoxy Matrix Composites

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Version 1

Abstract

Figures

1.0 Introduction

2.0 Materials And Methods

2.1 Materials used

2.2 Mixing and preparation

2.3 Mechanical properties

2.4 Friction and wear test

3.0 Results And Discussion

3.1 Tensile behaviour

3.2 Flexural behaviour

3.2.1 Homogenously mixed composite

3.2.2 Layered composite

3.3 Hardness and impact values

3.4 Friction and Sliding wear results

3.4.1 Friction

3.4.2 Wear

4.0 Conclusions

Declarations

References

Additional Declarations

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