Abstract
Composite industries use natural fibre as a sustainable resource to improve the sustainability and eco-friendliness of polymer composites. The characterization of alkali-treated Moringa oleifera fruit husk fibres (AMOFHFs) reinforced in unsaturated polyester resin matrix with varying weight percent of nano-sized silicon carbide (SiC) particles as filler material is presented in this paper. The AMOFHFs reinforced composite (AMOFHFC) specimens contain 20 wt.% AMOFHFs and nano-sized SiC particles ranging from 1 to 5 wt.% in 1 wt.% steps. The effect of wt.% variation in nano-sized SiC particles on the mechanical, morphological, tribological and water absorption behaviour of AMOFHFC specimens was thoroughly investigated. According to the findings, the AMOFHFC specimen with 4 wt.% nano-sized SiC particles as filler material has the best mechanical, tribological and water absorption properties. The hardness, tensile, flexural and impact strength of the AMOFHFC specimen with 4 wt.% nano-sized SiC particles improved by 14.86%, 23.11%, 9.6% and 23.22% respectively compared to the composite specimen without SiC nanoparticles as filler material. Similarly, the AMOFHFC specimen with 4 wt.% nano-sized SiC particles exhibited a lesser weight loss of 96.7% compared to the composite specimen without SiC nanoparticles as filler material during the Pin-on-disk experimentation which showcases its superior tribological characteristics. Furthermore, SEM images of fractured tensile AMOFHFC specimens aided in understanding the bonding nature of the AMOFHFs, SiC nanoparticles and unsaturated polyester resin matrix in the composite specimens. The findings above led us to the conclusion that AMOFHFCs with acceptable hydrophobic nature are best suited for light weight automotive and structural applications.
Introduction
Usage of environmentally harmful synthetic polymers derived from the processing of crude oil as by-products has increased exponentially in recent decades. The concern of environmentalists, regulations enforced by government bodies and recent climatic changes had made industries look into the possibilities of using green materials and greener processes as an alternative to crude oil-based synthetic products.1,2 The pursuit of environmentally friendly strategies and processes through green science, engineering and technology was at the centre of global efforts to promote sustainable development and environmental protection through social mobilization. Scientists and industrialists alike look to nature, especially natural fibres for answers to their concerns.3–5 Their global abundance and easy availability of agricultural waste conduct ongoing research on raw materials. The use of natural fibres and performance in the development of green solutions for the manufacture, use and disposal of automotive products have been optimized by scientists and researchers. 6 Financial logic to invest in raw material research, as well as productivity, is also influenced by the needs of consumers who are highly regarded. Natural fibres are often regarded as a solution to a variety of environmental issues, including obsolete vehicles, waste minimization and economic development projects.
Natural fibre-based polymer compounds have increased their use in a fast-growing number in the last few decades mainly due to their advantages such as natural decay, high strength and modulus, high strength to moderate weight, recycling and low cost. 7 Several researchers have reported on studies that focus on the plant fibre and its ability to modify synthetic fibres. Some of the sources of natural fibres in a plant are bark, leaves, seeds, fruits, grasses, stalks etc.8–10 Some of the common plants studied as sources of natural fibres include abaca, jute, coir, bamboo, oil palm, ramie, hemp, flax, okra and pineapple. Natural fibres found in different parts of the plant are extracted using various techniques such as manual decortication, hand extraction, dew repellent, water replenishment and chemical regeneration etc. 11
Moringa oleifera, a member of the Moringaceae family, grows in tropical and subtropical regions of Asia. It is considered to be one of the world's most important plants because almost all of its components can be used as food, in traditional medicine and for industrial purposes. 12 In addition, seeds and leaf flour have been used in the manufacture of baby food to increase protein content. The outer part of the fruit is hard and fibrous which comes out of the garbage and is discarded. It is rich in fibre and deteriorated in the commercial industry after producing its economic value. Various research projects have been carried out taking various parts of the Moringa oleifera tree to determine their use in the composite industry. Moringa oleifera fruit husk fibres (MOFHFs) were utilized by Binoj as reinforcement in unsaturated polyester resin to develop partially biodegradable polymer composites. 13 His studies concluded with the optimum weight percentage of MOFHFs in the polymer composite as 20 wt.%.
Isiaka et al. used the pod waste of Moringa oleifera fruit to extract cellulose particulates for reinforcement in epoxy bio-composites. 14 Their investigations concluded that 15 wt.% of cellulose particulates from pod waste of Moringa oleifera fruit reinforcement in epoxy bio-composite maximizes its mechanical properties. The ground dried leaves of Moringa oleifera were used as reinforcement filler in epoxy composite by Kajal et al. 15 They adopted the hand layup technique to fabricate the composites and their findings conclude the optimum wt.% of ground dried leaves of Moringa oleifera in the polymer composite as 20 wt.%. The optimum loading of ground dried leaves of Moringa oleifera in the polymer composite maximized its water absorption and mechanical characteristics. Bharath et al. investigated the possibility of utilizing the alkali-treated Moringa oleifera fruit husk fibres (AMOFHFs) as reinforcement in polymer composites to widen its scope of application in industries. 16 The alkali treatment of MOFHFs improved the cellulose wt.% in MOFHFs and surface roughness which sure widen the scope of application of the reinforced polymer composites in industries. Subhakanta et al. used 5% alkali treated MOFHFs and areca sheath fibres as reinforcement to develop hybrid natural fibre reinforced polymer composites. 17 These treated fibres were reinforced in polyethylene terephthalate to fabricate composites and found their mechanical characteristics to be exceptional.
Several works of literature were reported with different parts of Moringa oleifera derivatives as reinforcement in polymer composites. But to the author's best of knowledge less work was reported on hybridized and surface-modified reinforcements along with Moringa oleifera derivatives as reinforcement in polymer composites. In the present work, AMOFHFs were used as polymer matrix reinforcement along with silicon carbide (SiC) nanoparticles as filler material to find its suitability for interior material in automotive industries. The AMOFHFs were reinforced in an unsaturated polyester resin matrix using a compression moulding technique with varied weight percentage (wt.%) of SiC nanoparticles as filler material to fabricate the AMOFHF reinforced composite (AMOFHFC) specimens. The composite specimens were tested as per ASTM standards to know their mechanical, wear and water absorption characteristics. Scanning electron microscopic images were captured for the failure specimens to know their failure mechanisms. The results of the investigation help to conclude the replacement of synthetic material by AMOFHFCs in automobile interiors.
Materials and methods
Materials
The waste of Moringa oleifera fruits was collected from the market garbage dump yard in Coimbatore, Tamilnadu, India. The inner fleshy layer along with seeds was removed from the collected Moringa oleifera fruits and the Moringa oleifera fruit husk was water retted for 7 days to loosen the fibres. The MOFHFs were extracted from the water-retted Moringa oleifera fruit husk by a mechanical combing process. The extracted MOFHFs were sundried for 48 h to reduce the moisture content and stored for further processing. 18 The matrix materials required such as unsaturated polyester resin, methyl ethyl ketone peroxide, araldite and cobalt naphthenate were supplied by M/s. Sathyam Fiber Tex Pvt Ltd, Coimbatore, India. The nanofiller particle SiC was supplied by M/s. Vruksha composites & services Pvt Ltd Chennai, India.
Chemical treatment
The MOFHFs were drenched in 5% alkali solution for 1 h in a glass beaker. 19 Then the alkali solution was drained out from the glass beaker and the fibres were washed using water to eliminate the attached sodium hydroxide in the fibres. At the end of the washing process, the fibres were washed with a few drops of acetic acid in water with a pH of around 7 and sundried for 24 h to obtain AMOFHFs.
Composite fabrication
The random orientation of fibres and compression moulding technique were followed in the fabrication of the composite plates. 20 A mould of size 300 mm × 300 mm × 3 mm was used in the fabrication of composite plates. Before starting the fabrication process the inner surface of the mould is covered with Araldite which helps in easy removal of the composite plates after curing. Now the AMOFHFs were placed in the mould and wetted with unsaturated polyester matrix containing SiC nanoparticles of varied wt.%. The unsaturated polyester matrix is prepared by mixing unsaturated polyester resin, methyl ethyl ketone peroxide and cobalt naphthenate in the ratio of 98:1:1, respectively. 21 The prepared matrix is added with the required wt.% of SiC nanoparticles and mixed well with a mechanical stirrer before pouring into the mould to ensure uniform spreading of SiC nanoparticles in AMOFHFCs. Then the mould is closed and loaded on the compression moulding machine to exert a pressure of 200 N for 24 h to be cured. The AMOFHFCs were manufactured as per the specifications listed in Table 1.
AMOFHFC plates and their composition.
Composite characterizations
Mechanical study
Tensile and flexural test was carried out in a universal testing machine of 400 KN capacity with 1 mm/min crosshead speed as per ASTM D 638-01 and ASTM D 790-00 standards, respectively. 22 AMOFHFC specimens were prepared as per ASTM standards to conduct the experimentations. Micro hardness test was conducted at ambient conditions with 65% relative humidity following ASTM D785-98 standard. 23 Notched AMOFHFC specimens were used to conduct Charpy impact test on impact testing machine adhering to ASTM D 6110-97 standard. 24 During the impact experimentation, incident energy and impact speed were maintained at 2.75 J and 3.46 m/s, respectively. An average of three values is taken in all the experiments to avoid error in the experimentation process.
Microscopic study
The fractured surface of tensile failure AMOFHFC specimens resized as per the requirement was viewed under a scanning electron microscope to know the failure pattern of the composite specimens and its bonding characteristics between the AMOFHF, unsaturated polyester resin matrix and SiC nanoparticle filler material. The surface of AMOFHFC specimens was covered with a thin film of gold to avoid electron charge gathering during the imaging process. 25
Wear study
The wear behaviour of AMOFHFC specimens was interrogated using the Pin-on-disk apparatus adhering to ASTM G-99 standard.
26
Before the wear experimentation, the AMOFHFC specimens and the counterface body was cleaned with Silica carbide abrasive paper to facilitate better contact between the composite specimen and the counterface body. The sliding velocity and the applied normal load were maintained at 1.5 m/s and 20 N respectively during the experimentation for a 1000 m sliding distance. The specific wear rate (WS) and friction coefficient (µ) were computed using equations (1) and (2).
Water absorption study
ASTM D 570-99 standard was followed to study the water absorption characteristics of AMOFHFC specimens.
27
Composite specimens sized 39 mm × 10 mm × 3 mm cut from the moulded composite plates were dipped in normal, seawater and NaOH solution for 100 min. After the specified time duration, the AMOFHFC specimens were taken out and wiped with a cloth to remove the water on the surface and weighed using an electronic weighing scale to observe the upsurge in weight of the specimens. Equation (3) gives the water absorption percentage of the AMOFHFC specimens.
Results and discussions
Tensile characteristics
Figure 1 depicts the tensile behaviour of the AMOFHFC specimens with variation in wt.% of SiC nanofiller material in comparison with pure unsaturated polyester resin matrix and composite specimen without SiC nanofiller material. The incorporation of AMOFHFs in the unsaturated polyester resin matrix improved the tensile strength considerably. 28 This is due to the better load-carrying capacity of the incorporated AMOFHFs and the improved bonding characteristics between the AMOFHFs and the unsaturated polyester resin matrix. Further, the impregnation of SiC nanofiller particles in the composite specimens improved the stress distribution within the composite specimen as well as improved their bonding characteristics when loaded with tensile force. 29 This improved the load-carrying capacity of the AMOFHFC specimens C, D, E, F and G. The AMOFHFC specimen F with 4 wt.% SiC nanoparticles as filler material showed a maximum tensile strength of 80.49 MPa. This may be due to the minimum voids and compact packing of AMOFHFC specimen F. On the other hand, adding 5 wt.% of SiC nanoparticles as filler material to AMOFHFC specimens showed a decline in tensile characteristics by 4.32% owing to the accumulation of SiC nanoparticles in AMOFHFC specimen G.

Tensile behaviour of AMOFHFC specimens.
Flexural characteristics
Figure 2 depicts the flexural behaviour of AMOFHFC specimens with variation in wt.% of SiC nanofiller material in comparison with pure unsaturated polyester resin matrix and composite specimen without SiC nanofiller material. The observed values of flexural strength on AMOFHFC specimens reveal that the incorporation of AMOFHFs and SiC nanofiller particles in the unsaturated polyester resin matrix improved the flexural strength of composite specimens by more than 135%. The improved flexural behaviour of AMOFHFC specimens with SiC nanoparticles as the filler material is due to the better rigidity of composite specimens. 30 Also, the presence of SiC nanoparticles in the AMOFHFC specimens interacts with the unsaturated polyester resin matrix based on the surface energy of SiC nanoparticles which improves the rigidity of composite specimens. The AMOFHFC specimen F with 4 wt.% SiC nanoparticles as filler material showed a maximum flexural strength of 103.95 MPa. This is due to the better distribution and interaction of SiC nanofiller particles in AMOFHFC specimen F. The AMOFHFC specimen G with 4 wt.% SiC nanoparticles as filler material showed a slight decline in flexural characteristics by 1.9%. The observed decline in flexural characteristics of the AMOFHFC specimen G is due to the weaker bonding nature between the SiC nanoparticles and the unsaturated polyester resin matrix in the composite specimen due to accumulation of filler material. 31

Flexural behaviour of AMOFHFC specimens.
Hardness characteristics
Figure 3 depicts the hardness behaviour of AMOFHFC specimens with variation in wt.% of SiC nanofiller material in comparison with pure unsaturated polyester resin matrix and composite specimen without SiC nanofiller material. The incorporation of 20 wt.% of AMOFHFs individually and along with 1 wt.% of SiC nanofiller material in unsaturated polyester resin matrix improved the hardness characteristics of AMOFHFC specimens by 15.82% and 19.54%, respectively. Increasing the wt.% of SiC nanofiller material in the AMOFHFC specimens improved the hardness value of the composite specimens. This is due to the reduced number of voids and compact packing characteristics of AMOFHFC specimens. 32 A peak hardness value of 85 HRRW is observed for AMOFHFC specimen F due to the minimum number of voids and better packing characteristics of composite specimen. Further increase in wt.% of SiC nanofiller particles in AMOFHFC specimen decreased the hardness value by 4.7%. This is due to the poor distribution and gathering of SiC nanoparticles in AMOFHFC specimen which leads to more voids and poor packing characteristics thereby declining the hardness behaviour of composites.

Hardness behaviour of AMOFHFC specimens.
Impact characteristics
Figure 4 depicts the impact behaviour of AMOFHFC specimens with variation in wt.% of SiC nanofiller material in comparison with pure unsaturated polyester resin matrix and composite specimen without SiC nanofiller material. Similar to other mechanical characteristics considerable improvement is noticed in the impact characteristics of AMOFHFC specimens by incorporating AMOFHFs and SiC nanofiller particles in the unsaturated polyester resin matrix. The energy absorption capacity and stiffness of AMOFHFC specimens are greatly improved by the presence of SiC nanoparticles in composite specimens. 33 The impact behaviour of AMOFHFC specimens improved with an increase in wt.% of SiC nanofiller particles in the composite specimens and the maximum value is observed for the composite specimen F as 8.66 J/cm2. The impact behaviour of AMOFHFC specimen G with 5 wt.% of SiC nanofiller particles declined by 3.92% due to the presence of more matrix discontinuities. The uneven distribution and accumulation of SiC nanofiller particles in the AMOFHFC specimen G result in a greater number of matrix discontinuities which facilitates crack initiation by exposing the composite specimens to sudden loads.

Impact behaviour of AMOFHFC specimens.
Fractography analysis
The observations through SEM on the tensile failure cross-section of AMOFHFC specimens are shown in Figure 5(a) to (e). The failure pattern and bonding nature between the AMOFHFs, SiC nanoparticles and the unsaturated polyester resin matrix in AMOFHFC specimens are well exposed through the fractography of tensile failure cross-section of composite specimens. 34 A considerable number of AMOFHF pull-outs and voids are noticed in the fractography of AMOFHFC specimen C shown in Figure 5(a) which represents its weak mechanical behaviour compared to the composite specimens D, E, F and G. The increase in wt.% of SiC nanoparticles in AMOFHFC specimen reduced the voids and improved the bonding characteristics between the AMOFHFs, SiC nanofiller particles and the unsaturated polyester resin matrix by its even distribution throughout the composite specimens. 35 This is ensured by the reduced number of voids and AMOFHF pull-outs observed in the fractography of AMOFHFC specimens D and E shown in Figure 5(b) and (c). The fractography of the composite specimen F shown in Figure 5(d) exhibits a minimum number of voids, AMOFHF pull-outs and matrix cracks showcasing better interaction between the AMOFHFs, SiC nanofiller particles and the unsaturated polyester resin matrix in the composite. The observation in the fractography of AMOFHFC specimen F supports its better mechanical behaviour. The gathering of SiC nanofiller particles is noticed in the fractograph of the AMOFHFC specimen G shown in Figure 5(e). These SiC nanofiller particle gatherings result in matrix discontinuities which favours easy failure of AMOFHFC specimens when subjected to loads. 36 Hence, the AMOFHFC specimen G exhibited a decline in mechanical characteristics.

SEM images of the tensile failure cross-section of AMOFHFC specimens: (a) specimen C, (b) specimen D, (c) specimen E, (d) specimen F, and (e) specimen G.
Wear analysis
The wear characteristics of AMOFHFC specimens for the input parameters such as 20 N applied load, 1000 m sliding distance and 1.5 m/s sliding velocities are depicted in Table 2. The presence of SiC nanofiller particles and AMOFHFs in AMOFHFC specimens gave a good resistance to wear as noted from the weight loss value of composite specimens B and C. Also, the observed values on weight loss behaviour of AMOFHFC specimens help to understand that the weight loss is highly influenced by the wt.% of SiC nanofiller particles in AMOFHFC specimens. 37 In addition, this is understood from the increase in wear resistance behaviour of the composite specimens as noted in D, E and F. Also, the improvement in wear behaviour of AMOFHFC specimens is due to the better surface energy of the SiC nanoparticles which improves the interaction between the AMOFHFs and the unsaturated polyester resin matrix with better wettability in the composite specimens. 38
Wear characteristics of AMOFHFC specimens.
The other observed parameters such as wear, coefficient of friction and specific wear rate showed a declining trend with an increase in wt.% of SiC nanoparticles in AMOFHFC specimens. This is supported by the weight loss values of AMOFHFC specimens observed and discussed earlier. The maximum wear resistance behaviour is noticed in composite specimen F with 4 wt.% of SiC nanofiller material owing to the better dispersion and wettability of SiC nanoparticles with higher surface energy in AMOFHFC specimen resulting in better compactness and thereby leads to higher wear-resistant behaviour. 39 The decline in wear resistance property of AMOFHFC specimen G with 5 wt.% of SiC nanofiller material is due to the accumulation of SiC nanofiller particles in the composite specimen G. The accumulation of SiC nanoparticles in AMOFHFC specimen G restricts the wettability of AMOFHFs and SiC nanoparticles in the composite specimen by the unsaturated polyester resin matrix and thus leading to poor wear characteristics.
Water absorption analysis
Table 3 presents the water absorption behaviour of AMOFHFC specimens immersed in normal water (pH = 6.14), seawater (pH = 7.22) and NaOH solution. The AMOFHFC specimens immersed in different liquid mediums were taken out and weighed to note their increase in weight. The observations show that the AMOFHFC specimen B shows greater affinity towards the liquid medium compared to pure unsaturated polyester resin which is evident from the increase in weight of composite specimen B. This is due to the hydrophilic nature of reinforced AMOFHFs in composite specimens. 40 Also, the usage of SiC nanoparticles in AMOFHFC specimens reduced the hydrophilic nature of the composite specimens. This is also evident from the less increase in weight of composite specimens C, D, E, F and G compared to B. This observation is due to the minimum number of voids and compact packing of the materials in AMOFHFC specimens with SiC nanoparticles as filler material. 41 The minimum hydrophilic nature is noticed in the composite specimen F with 4 wt.% SiC nanoparticles as filler material whereas the hydrophilic nature started to decline on further increase in wt.% of SiC nanoparticle filler material in AMOFHFC specimens as noticed in composite specimen G. This is due to the accumulation of SiC nanoparticles in composite specimens resulting in poor wetting of filler material and reinforcement by matrix leading to declining in water absorption behaviour. 42 Similar water absorption behaviour of AMOFHFC specimens is noticed in all the liquid mediums.
Water absorption property of AMOFHFC specimens.
Conclusions
Mechanical, tribological and water absorption behaviour of AMOFHFC specimens were investigated in detail to figure out the possibility of using it in structural applications. The presence of SiC nanoparticles in varied wt.% in AMOFHFC specimens highly governed the mechanical, tribological and water absorption behaviour of the composite specimens. The peak mechanical characteristics are showcased by the composite specimen F with 4 wt.% of SiC filler material having a hardness value of 85 HRRW, the tensile strength of 80.49 MPa, flexural strength of 103.95 MPa and impact strength of 8.66 J/cm2. The hardness, tensile, flexural and impact strength of the composite specimen F improved by 14.86%, 23.11%, 9.6% and 23.22% respectively compared to the composite specimen B without SiC nanoparticles as filler material. These enhanced characteristics were further endorsed by SEM images of the tensile failure cross-section of the AMOFHFC specimen F which has a minimum number of AMOFHF pull-outs, voids, unsaturated polyester resin matrix cracks and interfacial ruptures. Also, the AMOFHFC specimen F showcased a minimum weight loss of 0.012 g during pin-on-disc wear experimentation which is 96.7% lesser compared to the composite specimen B without SiC nanoparticles as filler material. Moreover, the same specimen exhibited a weight gain of 0.015 g in normal water, 0.016 g in seawater and 0.010 g in NaOH solution which is 91.52%, 90.58% and 92.95% lesser respectively compared to the composite specimen B without SiC nanoparticles as filler material. The observed values in the investigation confirm the use of AMOFHFCs in structural applications requiring lightweight materials.
Highlights
Alkali-treated Moringa oleifera fruit husk fibres/nano-sized silicon carbide (SiC) particle composites characterized here.
Influence of wt.% variation of nano-sized SiC particles on properties of composites investigated in detail.
Composites with 4 wt.% of nano-sized SiC particles exhibited maximum properties.
Poor dispersion and accumulation of SiC nanoparticles in composites declined the overall characteristics at 5 wt.% SiC particles.
Footnotes
Author contributions
Palanisamy Saravanakumar: Investigation (lead); Validation (supporting); Writing – review and editing (supporting). Palanisamy Karuppuswamy: Writing – review and editing (supporting). Joseph Selvi Binoj: Resources (lead); Writing – original draft (lead).
Declaration of conflicting interests
The authors declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.
Funding
The authors received no financial support for the research, authorship, and/or publication of this article.
Ethics approval and consent to participate
All the authors demonstrate that they have adhered to the accepted ethical standards of a genuine research study. Also, individual consent from all the authors was undertaken to publish the data prior submitting to journal.
