Study of variation in physical and thermomechanical properties of Kevlar epoxy composite with bi-filler (NiCo2O 4 nanoparticles and wood sawdust) reinforcement

doi:10.21203/rs.3.rs-4820066/v1

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Study of variation in physical and thermomechanical properties of Kevlar epoxy composite with bi-filler (NiCo2O 4 nanoparticles and wood sawdust) reinforcement

https://doi.org/10.21203/rs.3.rs-4820066/v1

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The advancement in the development of hybrid filler-reinforced composites widens its usability in structural applications as a replacement for conventional materials. Filler incorporation into the composites imparts out-of-the-ordinary enrichment to material properties and plays a significant role in enhancing its physical, mechanical, and thermal characteristics. In this work, Kevlar epoxy composites are fabricated with bi-filler reinforcement viz, wood sawdust (natural filler – fixed as 5 wt%) and NiCo₂O₄ nanoparticles (synthetic filler – varying as 0.5, 1, 1.5, 2 wt%) using open-mold hand layup technique. Sol-gel synthesized NiCo₂O₄ nanoparticles are characterized with XRD and FESEM to ensure their purity and spherical morphology. Among filler-loaded composites, 1.5 wt% of NiCo₂O₄ nanoparticles reinforced Kevlar epoxy composite shows a superior tensile strength of 61.9 MPa. High thermal stability is observed for 1.5 wt% of NiCo₂O₄ nanoparticles/ 5 wt% wood sawdust reinforced Kevlar epoxy composite, wherein, it can be potentially efficient for thermal applications. Physical properties seem to be better for 1 wt% of NiCo₂O₄ nanoparticle reinforcement that prevents the composite from microcracking due to low wettability.

Kevlar

Epoxy composite

Bi-filler reinforcement

NiCo2O4 nanoparticles

Mechanical properties.

Composites are made by the combination of two or more constituent materials having dissimilar physical properties that are combined to create a new material with enhanced properties and thus improve the characteristics of the base material [1]. Composite material possesses the advantage of being with high strength, flexibility, low weight, resistance to heat and chemicals, and durability. Polymers are versatile materials that could be easily molded as per our application so they can preferably be used in composite fabrication [2]. Composite material that works in a sustainable diverse environmental condition adds an advantage to the emergence of new materials for various applications. Hence, polymer-based composite materials are potentially used as an emerging replacement material for metals [3]. Polymer composites are made with two parts, a reinforcement, and a matrix. The reinforcement can be a metal, ceramic, or polymer, whereas the extensively used matrix could be a thermoplastic or thermosetting resin. In the composite fabrication process, the epoxy resin acts as a binder and is poured along with a hardener onto the surface of the Kevlar fabric to make the fabric rigid. Epoxy resin is a thermosetting polymer with excellent moisture resistance, long shelf life, chemical resistance, and mechanical and fatigue strength. A thermosetting epoxy resin and hardener are primarily used to enhance the bonding strength of the fabricated composite [4].

In recent days, fiber-reinforced polymeric composites seek attention with their design and manufacturing technique, which opens these materials to be commercialized. These composites could be used in the application of electrical equipment, automobiles, aircraft, and e-vehicle structures [3]. Fiber-based composite materials are fabricated with the reinforcement of natural or synthetic fibers [5]. Natural fibers derived from living organisms are known to have less strength and durability in comparison with synthetic fibers obtained through chemical synthesis with tuned mechanical properties. Man-made synthetic fibers have the advantage of having good resistance to chemicals and water and are known to be a consumer-friendly fabric with low cost. Among various synthetic fibers, Kevlar is a well-known strong synthetic fiber with a relative density of 1.44 and tensile strength of 3620 MPa. Kevlar is a synthetic para-aramid fiber (poly-para phenylene terephthalamide) that has great potential to be used as a reinforcement material since it has a high strength-to-weight ratio, low-cost fabrication, lightweight, high thermal stability, good flame retardance, low elongation, low creep, high tenacity, and high young's modulus with good impact resistance [6, 7]. From body armor to aircraft/automobile structures, Kevlar serves as a desirable material for high-strength industrial applications [8].

In recent years, wood sawdust-reinforced polymer composites have emerged in the field of nanotechnology due to their improved physical, mechanical, and thermal properties [9]. The purpose of reinforcement of natural filler in the composite is to enhance the non-toxicity, non - corrosiveness, and biodegradability of the material. In addition to natural filler, NiCo₂O₄ nanoparticles are added as a synthetic filler to enhance the physicomechanical properties of the composite. Thus, the reinforced nano-fillers are capable of developing strong interfacial bonding that is essential in transferring load from matrix to fiber and enhancing the strength of the fabricated composite [10]. The composites fabricated in this study are made with reinforcing materials, NiCo₂O₄ nanoparticles, and wood sawdust, which is being laid onto the Kevlar epoxy matrix. The unique properties are attained by composites reinforced with multiple fillers that seem unattained from single filler/fiber-based composites [11]. In general, various studies reported that hybridization improves the interlaminar shear strength, and thus the mechanical property of the composite can be tuned as per the application [12]. Ramesh et al [13], investigated the properties of hybrid configured Kevlar/epoxy, basalt/epoxy, and Kevlar/basalt/epoxy fabricated using a hand layup procedure. Pranesh et al [14], reported the nano-silica filler incorporated hybrid woven carbon-Kevlar epoxy composite and its flexural property analysis. Mohanad et al [15] elaborated on variations in the mechanical behavior of a hybrid polymer composite made with the mixture of epoxy resin and polysulfide resin as a layer for reinforcement of carbon and Kevlar in 3 layers.

Nitin et al [16], synthesized nanopowder and intruded it to fabricate the Kevlar polymeric composite and studied its ballistic performance. Anurag et al [17], analyzed the mechanical properties of the graphene nanoplatelet (GNP) incorporated epoxy hybrid composite and reported its high thermal conductivity, heat deflection temperature, and tensile and flexural strengths respectively. Vinod et al [18], elaborated on the influence on adhesion of fiber matrix of Jute/hemp bio-epoxy made hybrid bio-composite showing a high tensile strength of 65.44 MPa. Ravindra et al [19], did an experimental comparison on mechanical property variation of hand-laid e-glass fiber reinforced epoxy composite and reported the improvement in tensile strength for hybrid composite than GFRP composite. Jenish et al [20], explained hybrid mudar/snake grass fiber-reinforced epoxy incorporated with nano-silica filler for structural application which shows higher mechanical properties for composite with 30% of fiber content addition.

This research work aimed at the fabrication of NiCo₂O₄ nanoparticles/wood sawdust reinforced bi-layered Kevlar epoxy composites using a simple open mold hand layup technique. The experimental data of the fabricated composites are ensured and reported with a notable increase in tensile strength, and physical and thermal properties. To fabricate an innovative and qualitative fiber-reinforced polymeric composite, wood sawdust (natural filler) and NiCo₂O₄ nanoparticles (synthetic filler) are used as reinforcement into the epoxy matrix and the enhancement in strength of the composite by varying filler concentration is contrived. This study portrays the outcome of the potentiality of the use of novel- NiCo₂O₄ nanoparticles/wood sawdust incorporated Kevlar epoxy composites for the structural application of automobiles and electric vehicles.

2.1 Materials

The chemical reagents Citric acid, Glycerol, Cobalt (II) nitrate hexahydrate, and Nickel (II) nitrate hexahydrate were purchased from Merck with 99% pure grade and are used for nanoparticle synthesis. Epoxy water clear casting resin is purchased from carbon black composites, which have flexural strength of 120–140 MPa, tensile strength of 55–70 MPa, and elongation at break of 1.5–3.0%. A para-aramid Kevlar fiber (K/1740 − 480 GSM), which has a density of 1.3–1.4 g/cm³, a size of 3 mm, pH of 0–14, withstanding pressure of 2–50 MPa, and a temperature (150 to ± 275°C) is used as a reinforcement fiber. Teak wood sawdust is collected from the wood-cutting industry and is used as a natural filler.

2.2 Synthesis of NiCo₂O₄ nanoparticles

The precursors, cobalt (II) nitrate hexahydrate and nickel (II) nitrate hexahydrate are dissolved in double distilled water and stirred at 450 rpm for 30 mins. The addition of citric acid and glycerol to the solution mixture and stirring it for 45 minutes aids in the enhancement of gel formation during the reaction. Meanwhile, the solution mixture is heated for 15 hrs at 60–80°C to fasten the gel formation. Then, the obtained powder is scrapped and kept in a furnace for calcination at 450°C for 5 hrs. The obtained NiCo₂O₄ nanoparticles are then grounded and used for further characterization. Figure 1(a) represents the steps undergone to synthesize the NiCo₂O₄ nanoparticles (hybrid metal oxide nanoparticles).

2.3 Nanocomposite fabrication

Structural polymer composites are fabricated using a fabric of Kevlar (para-aramid) and water-clear casting epoxy resin reinforced with NiCo₂O₄ nanoparticles and wood sawdust using an open mold hand layup technique as shown in Fig. 1(b). Thick stainless steel (SS) plates are being used as a mold [21]. The mix is made in a ratio of three parts of epoxy resin to one part of hardener as instructed by the manufacturer. The resin mixture is made by adding a proper proportion of epoxy resin, wood sawdust, and NiCo₂O₄ nanoparticles, which are manually stirred and ultrasonicated. The hardener is then added to the resin mixture and the homogeneous solution is poured onto the surface of the Kevlar layer kept on the SS mold. The Second Kevlar layer is placed on the resin-poured surface and the setting time of one hour is maintained by keeping a dead weight onto the composite. The curing is done by keeping the fabricated composite in the vacuum oven at 70°C for 24 hrs. The Kevlar epoxy composites are made with different weight percentages of NiCo₂O₄ nanoparticles (0, 0.5, 1, 1.5, 2%), and constant 5% of wood sawdust incorporation, and the fabricated composites are named Pure, CN0.5, CN1, CN1.5, and CN2. Thus, the fabricated composite is cut into the desired dimension as per the ASTM standard and further tests are being carried out.

2.4 Characterization

The crystalline structure of the nanoparticles is analyzed using X-ray diffraction (XRD), carried out on Ultima III, Rigaku, using copper Kα target radiation under an operating voltage of 40 kV with a wavelength of λ = 1.54 Å. Carl Zeiss instrument is used for Field emission scanning electron microscopy (FESEM) to analyze the morphological structure. The chemical bonding and functional group analyses are studied using Fourier transform infrared spectroscopy (FTIR), Nicolet iS5 from Thermofisher Scientific. For a tensile test, the gauge length, gauge width, and thickness (80 mm x 10 mm x 3.2 mm) with a strain rate of 1 mm/min are maintained as per ASTM standard D3039. The dimensions of the composites are made to 80 mm x 10 mm x 3.2 mm as per ASTM standard D790 for carrying out the flexural test. The % water absorption is calculated by soaking the composite in double distilled water for 50 days. The water is placed as a sessile drop on the sample and the contact angle measurement of the fabricated composite is carried out using the apex instrument contact angle system by tangent fitting method. The thermal stability of the Kevlar epoxy composites is studied using Thermogravimetric analysis (TGA) under a nitrogen atmosphere with a heating rate of 15°C/min.

3.1 XRD of synthesized NiCo₂O₄ nanoparticles

XRD aids in determining phase purity and crystal structure with the aid of distinct diffraction peaks corresponding to NiCo₂O₄ structure [22]. Figure 2(a) shows the XRD pattern of the synthesized NiCo₂O₄ nanoparticles with the 2θ values as 19.12°, 31.4°, 36.9°, 43.6°, 59.3°, 65.1°, and 76.2°, which are respectively identified as (111), (220), (311), (400), (511), (440) and (533) plane. The extra peaks noted at 44.8° and 62.9° correspond to the peak of nickel oxide and cobalt oxide respectively. The crystallite size was calculated by the Debye Scherrer formula as,

$$\:D=\frac{0.9\lambda\:}{\beta\:Cos\:\theta\:}$$

where D is the crystallite size, λ is the wavelength of the X-ray, θ is the Braggs angle (radian), and β is the full width at half the maximum of the peak (radian). The crystallite size is calculated using Scherrer’s formula and it ranges between 16 to 22 nm. The elemental composition of the NiCo₂O₄ nanoparticles is explained using EDAX as mentioned in Fig. 2(b) and Table 1.

Figure 2(c) shows the FESEM of spherical morphological NiCo₂O₄ nanoparticles obtained using sol-gel synthesis [23]. There is an observance of agglomeration of the nanoparticles. FTIR peaks of fabricated Kevlar epoxy composites are shown in Fig. 2(d). The peaks of Kevlar are observed from 1300 cm^− 1 to 1502 cm^− 1 corresponding to the coupling between bending C-H and stretching C-N respectively. The band between 3200 cm^− 1 and 3300 cm^− 1 explains -NH stretching of the amide belonging to Kevlar [24]. 1025 cm^− 1 and 1174 cm^− 1 peaks relate to the C-N stretching of amine. The band overlap occurring between OH- and primary amines are ranging from 3200 cm^− 1 to 3600 cm^− 1. The peaks of 918 cm^− 1 and 1600 cm^− 1 correspond to epoxy and amine respectively [25, 26]. 3046 cm^− 1 peak matches the tension of the -CH group of the epoxide ring. NiCo₂O₄ peaks of 1381 cm^− 1, 2927 cm^− 1, and 3446 cm^− 1, which are associated with the presence of physically adsorbed Co₂, N-H of the aromatic ring, and transition metal ion of nickel to form coordination compound with -NH- (amine) and -N= (imine) respectively [27, 28].

Table 1

Elemental composition of NiCo₂O₄ nanoparticles observed using EDAX
Element	Elemental composition (atomic %)
Cobalt	20.38
Nickel	24.94
Oxygen	54.68

3.2 Mechanical studies

Figure 3(a) shows the tensile strength obtained for the fabricated NiCo₂O₄ nanoparticles/wood sawdust reinforced Kevlar epoxy composite. Pure (Filler-unloaded Kevlar epoxy composite) is noted to have 72.2 MPa of tensile strength, whereas CN1.5 (Filler-loaded Kevlar epoxy composite) is observed to have a tensile strength of 61.9 MPa, which seems to be higher than that of other filler-incorporated Kevlar epoxy composites. There is an increase in uniform interfacial stress transfer for the CN1.5 composite, which minimizes the stress concentrated at the center. So, tensile stress and young’s modulus tend to be higher for CN1.5 composite. The lower observance of tensile strength for other filler-loaded composites (CN0.5, CN1, and CN2) might be due to the aggregation of the filler with the matrix. During fabrication, the large surface area of the nanoparticles might result in the formation of more hydrogen bonds and thus frictional force seems to increase for other filler-loaded composites. The secondary reason behind the observance of decreased tensile stress is increased porosity [29]. In addition, strong filler/matrix bonding is important for having high tensile stress. The pure composite seems to be significantly stiffer than the filler-loaded Kevlar epoxy composites due to higher tensile strength. Here, the necking and cold-drawing mechanism resulted in the widening of the peak of the pure composite, whereas other composites show brittle behavior after the yielding point [30]. The reason for brittleness might be due to stress developed at the break. The filler-loaded composites have decreased stress at the break because of less interfacial adhesion between the matrix and reinforcement. The interfacial interaction happening between the filler and matrix plays a vital role in affecting the tensile property of the composite. Hence, filler-loaded composites are observed to have lower toughness except CN1.5 composite. Figure 3(b) shows flexural test of the fabricated NiCo₂O₄ nanoparticles/wood sawdust reinforced Kevlar epoxy composite. The % elongation at break is noted as 27.9% and 23.8% for pure and CN1.5 composites. NiCo₂O₄ nanoparticles incorporation to 1.5 wt% has higher % elongation and so it sustained high tensile strength. The incorporation of NiCo₂O₄ nanoparticles filler being aggregated on the Kevlar-epoxy matrix might result in the formation of a micro-deformation mechanism during elongation at break and so tensile strain to failure might occur. Here, the tensile test confirms that there is an increase in the elastic modulus. While elongation occurs, fibrils present in the amorphous region tend to get rearranged and result in the regeneration of intramolecular hydrogen bonds thus improving elongation at break.

3.3 SEM after tensile fracture

The surface micrograph of different percentages of filler-loaded Kevlar epoxy composite is shown in Fig. 4. SEM images show fiber pullout and debonding, which manifests quite weak interfacial interaction between the fiber-matrix interface. In Fig. 4(a-c), there is an observance of voids in the fractured surface due to non-homogeneous interfacial adhesion between Kevlar fiber and epoxy matrix due to the hydrophilic nature of epoxy resin [31]. Fiber pullout occurs at the beginning of crack propagation and this is caused due to fiber that is not strongly embedded with the matrix [32]. The SEM observation shows that the fractured filler-loaded Kevlar epoxy composites have fiber pull-out as a result of the failure mechanism. This transpires due to the reinforcement of hydrophilic epoxy onto the Kevlar surface. This might result in the forging of the composite to be a moisture-absorbing material and thus swells the composite on soaking to water [33]. In addition, small fibrils are found on the fractured surface of the composite, which signifies the traces of cold drawing during tensile failure. The surface roughness of the fractured composite illustrates the ductile fracture and thus shows elastic deformation [34]. Figure 4(e) shows delamination which signifies poor interfacial bonding between matrix and reinforcement. So, filler-loading plays a vital role in affecting the mechanical properties of the fabricated composites [28]. There might also be a reason for failure observance in composite, which occurs due to micro-buckling or splitting/shear happening during tensile fracture [35].

3.4 Physical properties

The investigation of the effect of moisture absorption is determined by calculating the percentage uptake of water by the composite. The fabricated composites are immersed in double-distilled (DD) water at room temperature. After 50 days, the composites are removed from DD water and the mass of the composite is measured using a weighing balance. The water absorption percentage for the different % filler-loaded composites CN0.5, CN1, CN1.5, and CN2 are evaluated using,

$$\:WA\%=\frac{Wf-Wi}{Wi}\times\:100$$

where WA% implies water absorption percentage after immersion in water for 50 days, $\:Wf$ is the observed weight of the composite noted after 50 days of DD water soaking and $\:Wi$ is the initial weight of the composite before soaking. The study includes the investigation of the moisture absorption behavior of the composite and its effect on filler proportion incorporation. Figure 5(a) shows the percentage of water absorption of all the composites loaded with wood sawdust (5 wt%) and NiCo₂O₄ nanoparticles (0.5, 1, 1.5, and 2 wt%) onto the Kevlar-epoxy matrix. The graph explains the weight gain noted for the composite in percentage according to the immersion of the composite in DD water for 50 days under room temperature. When the composite tends to be kept immersed in water for a few days, there is an occurrence of displacement of a water molecule from higher to lower concentration. This might result in notable wettability of the fiber composite, lower interfacial property, and micro-crack formation at the fiber-matrix interface. This significantly reduces the mechanical performance of composite in a water-driven environment. In the end, filler-unloaded Kevlar epoxy composite (pure) seems to have less weight gain than the NiCo₂O₄ nanoparticles/wood sawdust loaded Kevlar epoxy composites [36].

The water absorption percentage of the composites is highly influenced by the percentage incorporation of the filler. The NiCo₂O₄ nanoparticles filler is being added in 0.5, 1, 1.5, and 2 wt%, wherein, 1 wt% filler-loading shows 13.42% water absorption, which seems to be a little higher than pure composite. 1 wt% of filler-loading reduces wettability and agglomeration than other percentages of filler-loaded composites. Lower wettability tends to increase the void and thus enhance the water absorption uptake beyond a particular percentage of filler incorporation. Here, the nanofiller acts as a toughened layer for the matrix and prevents microcracking of the matrix due to swelling of the fiber for the CN0.5 composite. Figure 5(b) explains the thickness swelling observed for the composites being immersed in DD water for 50 days.

The contact angle measurement aids in measuring the wettability of filler-unloaded and filler-loaded Kevlar epoxy composites. All the composites are observed to be hydrophilic with a contact angle of less than 90°. Pure composite has a minimal water contact angle of 75.54° and CN1 has a high contact angle of 86.02° as represented in Fig. 5(c,d). Surface roughness decreases for filler-loaded composites which implies that the incorporation of fillers reduces the compatibility between fiber and resin. A higher contact angle signifies an improvement in bonding strength and provokes hydrophobicity of the composite. Here, the fiber-matrix interaction relates the wettability of the composite to the contact angle [37].

3.5 Thermal studies

The thermal characteristics of the Kevlar epoxy composite with and without filler-loading are observed using TGA as shown in Fig. 6. On increasing the temperature, there is an observance of percentage weight loss for the composite. Till 100°C, the composites seem to be thermally stable, wherein, there is a notable weight loss with increasing temperature due to moisture loss, volatile impurity, and vapourization. The weight loss that occurs for the filler-loaded and filler-unloaded composite corresponds to the epoxy degradation between 330°C − 420°C. The cross-linking between the NiCo₂O₄ nanoparticles and an epoxy matrix is due to enhanced interfacial bonding that might result in increased decomposition temperature of the composite. A relatively high reduction in weight loss is noted for CN0.5 (0.5 wt% of NiCo₂O₄ nanoparticles/ 5 wt% wood sawdust incorporated Kevlar epoxy composite) and so CN0.5 seems to be thermally stable than other filler-loaded composites. The main reason to be associated with high thermal degradation is the high thermal conductivity of NiCo₂O₄ nanoparticles. The increase in weight loss of the filler-loaded composite might imply better thermal conductivity of the matrix system for different filler loading (0.5, 1, 1.5, and 2 wt%). As a result of good NiCo₂O₄ nanoparticles dispersion with the matrix, the matrix plastification effect occurs and the nanoparticles interfere with the polymer matrix, which decreases the crosslink density [37].

NiCo₂O₄ nanoparticles were synthesized using the sol-gel technique wherein, XRD and FESEM revealed their crystallinity and spherical morphology respectively. The facile open mold hand layup technique was used to fabricate the NiCo₂O₄ nanoparticles/wood sawdust reinforced Kevlar epoxy composites. The microstructural analysis and interfacial bonding of the fabricated composites were investigated using FTIR spectroscopy. The filler-loading into the Kevlar epoxy matrix shows two significant effects, the enhancement in interfacial compatibility and the improvement of the tensile strength of the composite. CN1.5 showed a significant upraised mechanical strength and improvement in failure mode during the flexural test than other filler-loaded composites (0.5, 1, and 2 wt%). TGA results signified the increase in decomposition temperature for CN0.5 composite with high thermal stability, which was lesser for other filler-loaded Kevlar epoxy composites.

The authors declare no conflict of interest.

Data Availability

All data used in this study are included in the manuscript.

Funding statement

There is no funding provided to carry out this research work.

Author Contribution

N.B. carried out the experimental characterization and manuscript writing.A. M Lab facility and guidance, writing supervision and research administration.

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You are reading this latest preprint version

Study of variation in physical and thermomechanical properties of Kevlar epoxy composite with bi-filler (NiCo2O 4 nanoparticles and wood sawdust) reinforcement

Status:

Version 1

Abstract

Figures

1 Introduction

2 Experimental materials and methods

2.1 Materials

2.2 Synthesis of NiCo₂O₄ nanoparticles

2.3 Nanocomposite fabrication

2.4 Characterization

3 Results and Discussion

3.1 XRD of synthesized NiCo₂O₄ nanoparticles

3.2 Mechanical studies

3.3 SEM after tensile fracture

3.4 Physical properties

3.5 Thermal studies

4 Conclusion

Declarations

Author Contribution

References

Additional Declarations

Status:

Version 1

Study of variation in physical and thermomechanical properties of Kevlar epoxy composite with bi-filler (NiCo2O 4 nanoparticles and wood sawdust) reinforcement

Status:

Version 1

Abstract

Figures

1 Introduction

2 Experimental materials and methods

2.1 Materials

2.2 Synthesis of NiCo2O4 nanoparticles

2.3 Nanocomposite fabrication

2.4 Characterization

3 Results and Discussion

3.1 XRD of synthesized NiCo2O4 nanoparticles

3.2 Mechanical studies

3.3 SEM after tensile fracture

3.4 Physical properties

3.5 Thermal studies

4 Conclusion

Declarations

Author Contribution

References

Additional Declarations

Status:

Version 1

2.2 Synthesis of NiCo₂O₄ nanoparticles

3.1 XRD of synthesized NiCo₂O₄ nanoparticles