Abstract
The focus of this research was to study how process parameters including fibre alignment, fibre length, fibre volume percentage and alkali pretreatment affected the mechanical and dynamic mechanical characteristics (DMA) of the sansevieria fibre composite. The nonwoven fabric was produced through the needle punching technique. 18 composite samples have been produced according to L18 Taguchi design. Four different process parameters were considered for investigation, such as fibre length, fibre volume fraction, the concentration of alkali and fibre alignment. Using Design S/N ratio analysis, the optimized process parameters for achieving maximum tensile, flexural and compression properties of the composite were measured. In the case of DMA analysis, three different parameters have been calculated only for selected samples such as storage modulus, loss modulus and loss factor. Variance analyses were carried out to measure the statistical influence of the process parameters on response. After this, validation of experiments was also done. SEM study was also carried out to understand the damage pattern of the composite sample.
Introduction
Over the past few decades, the research interest towards natural fibre composite as a replacement for synthetic and mineral fibre based composite due to the stringent environmental policies.1,2 Natural fibres such as hemp, kenaf, bagasse, jute, ramie, oil palm etc … have been investigated as reinforcements for the fabrication of fibre reinforced polymer composites. 3 Natural fibres possess essential properties such as high strength, lightweight, low density, low specific gravity and biodegradability. 4 Sansivieria plant contains bold succulent spiky leaves that grow eight feet, and the number of leaves in the plant is one and rarely two or three. 5 The present utility of sansivieria fibre is only a small percentage of the potential total world production of coconut husk. 6 Devaki and Kumar studied the mechanical properties of sansevieria fibre and its suitability for composite fabrication. 5 The coconut fibres were treated with surface-active agents to improve resin-fibre interfacial bonding. The treatment agents used, such as alkali, acetylenes, peroxide and potassium permanganate, have significantly influenced the mechanical strength of the composites. 7 Similarly, Lai et al. studied the mechanical and electrical properties of coir fibre reinforced polypropylene composite and found that surface-modified coir fibre has shown higher bonding strength than untreated fibre composite structures. 8 Kalaprasad et al. studied the sisal/glass fibre composite using polyester resin with a different range of fibre length. They found that the variation in fibre length and distribution made considerable differences in the strength and modulus values. The tensile strength and Young’s modulus were increased up to a fibre length range between 6 and 8 mm; after the tensile properties were reduced. 9 Majid et al. studied the effect of fibre content and length on mechanical and dynamic mechanical properties of the composite material and found that the fibre length and fibre content has significantly influenced both the properties. 10 Arib et al. 11 investigated the flexural behaviour of pineapple fibre composite by modifying the fibre volume fraction of the reinforcement and found the composite’s flexural strength was largely affected by the reinforcement. Mariatti et al. investigated the flexural property of banana fibre reinforced composite by changing the number of reinforcement layers and reported that the stacking method of reinforcement structure exhibits great influence on the flexural strength of the composite. 12 Dynamic mechanical analysis is an important characterization technique to study the visco-elastic characteristics of the composite material. There are three essential parameters that have been analysed under DMA studies such as storage modulus (E′), loss modulus (E″) and loss factor (tanα). 13 The loss factor is the ratio between the storage modulus to loss modulus, and the higher loss factor indicates the higher damping factor. 14 Higher storage modulus is indicated as higher stiffness of the composite and it is affected by the filler type, geometry of the reinforcement and the filler distribution pattern inside the matrix. Murugan and Kumar investigated the DMA analysis for banana fibre reinforced composite material and reported the fibre volume fraction of has highly influenced all the parameters pertaining to DMA. 13 There were many research studies conducted towards the influences of reinforcement properties on mechanical strength; however, combined analysis of multiple parameters on the static and dynamic mechanical properties has not been studied much. Hence, this research aims to know the effect of the four process parameters such as fibre alignment, fibre length, fibre volume fraction and alkali pretreatment on the mechanical and dynamic mechanical composite properties of the composite and obtain the optimum parameter array.
Materials and methods
Sansevieria fibre has been extracted from the leaf of the plant. The extracted fibres were kept at room temperature for about 3 days for drying. All the dried fibres were cut into three different ranges such as 4 cm, 6 cm and 8 cm, then washed and oven-dried for obtaining a constant weight. The average fineness of the fibres is 0.98 g/cc, tensile strength was 113 Mpa, modulus of the fibre was 6.5 Gpa and the breaking extension was 16%. Standard low temperature curing epoxy resin (LY 556) and its hardener (HY 951) are utilized for composite fabrication. The mixing ratio between resin and hardener was maintained as 10:7 by weight, and the mechanical stirrer was used to mix the resin. A cast-iron mould was fabricated with the dimension of 15 cm X 15 cm X 2 cm for composite preparation. Aluminium foil was also used as a base material to protect the resin leakages during the moulding process.
Alkali pretreatment
Physical properties of alkali-treated natural fibres.
Experimental methods
L18 Taguchi design with process parameters.
MM: Machine Direction; MX: Cross Direction.
Needle punching process
The necessary quantities of fibres were taken for nonwoven preparation based on three different fibre volume fractions such as 30%, 40% and 50%. The needle punching machine was used to convert the chosen mass of fibres into a compact bat for composite processing. These fibres were opened, carded and subsequently passed through a cross-lapper to form cross-laid webs and parallel laid webs. Both types of nonwoven batts were allowed to pass through the needle punching process to prepare the nonwoven fabric of nominal mass per unit area of 400 g/m2. The process parameters (punch density of 150 cm2, depth of needle penetration of 12 mm) were kept constant during the fabrication of nonwoven samples. According to the experiments, the fibres were aligned in both machine direction and cross-machine direction.
Composite fabrication
The mould of 200 mm X 200 mm X 10 mm was taken for composite fabrication. It was interlined with aluminium foil to avoid resin leakages. Then the epoxy resin was poured stage by stage into the mould. The nonwoven batt was laid into the mould cavity with resin. Once the process is completed, then the mould unit is transferred to the compression moulding machine. The mould was subjected to around 30 bar of pressure via the press. For 4–5 h at a time, the mould was cured within the press. Here, two types of layer stacking were followed: preferential stacking (cross-machine, MX) and non-preferential stacking (machine, MM). After that, composite samples were removed, and the specimens were prepared for various mechanical tests. Figure 1 shows the composite fabrication process. Composite fabrication process. (a) Sansevieria roxburghiana, (b) Fibre extraction, (c) Alkali-treated 
Characterization
Mechanical testing
The mechanical testing (tensile, flexural and compression tests) of the composite samples was performed using an Instron Universal testing machine (Zwick Roell-Z010 Universal Testing machine) in accordance with ASTM D3039M, ASTM D790 and ASTMD3410, respectively. The cross-head speed of 2 mm/min was maintained for tensile testing, whereas the bending tests were performed at a speed of 2.8 mm/min. It was ensured that the edges of composite samples were smoothened by sandpaper to avoid stress concentration during the tensile and bending tests.
Dynamic mechanical analysis
Rectangular specimens with 12 mm × 3 mm × 25 mm were used for this experiment. The dynamic storage modulus (E′), loss modulus (E″) and loss factor (tanα) of the specimen were measured as a function of temperature (25–1605°C) and at the frequency range of 0.3 Hz–1 Hz using a dynamic mechanical analyser (DMA4101 model).
Scanning electron microscopy analysis
Scanning Electron Microscopy (SEM) is a surface analysis; through this, the sample can be scanned with an electron beam to produce a magnified image. This method is very effective in micro-surface analysis. Damaged composite samples were studied through the scanning electron microscope (Model JSM-6360) to understand the pattern of deformation.
Results and discussion
Mechanical strength values of sansevieria fibre composite as per L18.
The average tensile, flexural and compression strength of 18 laminates are shown in Figure 2. It can be summarized that fibre alignment, fibre length, fibre volume fraction and alkali treatment have a significant influence on all the mechanical properties. Mechanical properties of the sansevieria fibre composite.
Specifically, experiments 10, 11, 13, 14 and 17 have shown the highest tensile, flexural and compression strength values. The process parameters of these specimens are such as fibre alignment was the cross direction, fibre length is concerned, 4 cm and 6 cm fibre lengths for two pair samples and remaining one sample was made with 8 cm fibre length. Similarly, one pair sample had a 30% fibre volume fraction, whereas the remaining three samples had a 40% fibre volume fraction. In the case of alkali pretreatment, two pairs of samples were made with alkali concentrations of 3% and 4%, respectively, and one sample was made with an alkali concentration of 5%. The reason behind this scenario is attributed that several factors can affect the strength of the composite. Increasing fibre length and fibre volume fraction up to the critical limit will increase the composite strength; later on, the composite strength will be reduced due to fibers’ improper agglomeration. Similarly, the alkali pretreatment on fibre will positively impact the composite’s mechanical properties up to the critical alkali concentration by increasing the fibre crystallinity and matrix adhesion. More than the critical level of alkali concentration damages the fibres, which in turn affects the composite strength.13,16
After this, the S/N ratio for all the mechanical properties was calculated as per the ‘higher is the better’ formula. Then the average S/N ratio of each factor was calculated by averaging out the corresponding S/N ratio values. After this, the average S/N ratios of each factor were graphically represented in Figures 3–5 for all the process factors. Average S/N ratios of tensile strength of sansevieria fibre nonwoven composite with the variation of process parameters. Average S/N ratios of flexural strength of sansevieria fibre nonwoven composite with the variation of process parameters. Average S/N ratios of compression strength of sansevieria fibre nonwoven composite with the variation of process parameters.


Through Figures 3–5, the optimum combination of S/N ratios was chosen as A2B2C2D1 in all the mechanical properties. Cross-laid fibre alignment gives higher inter-fibre bonding than parallel lay alignment; the cross-direction fibre alignment composite sample has exhibited higher value in this optimum combination of process parameters. In the case of fibre length is concerned, 6 cm fibre intervention showed a higher impact on all the mechanical properties of the composite. Since the 4 cm fibre could not establish better fibre to fibre bonding, whereas the 8 cm fibre created more curly formation, and according to Kelly-Tyson tensile strength predictions, it was determined that increasing the length of the reinforcement fibre beyond the critical fibre length could not improve the mechanical properties of the composites. According to the Kelly-Tyson model stated that the sub-critical and supercritical lengths of the fibres affect the tensile strength of the short fibre reinforced composite, as well as that the composite strength is affected by fibre orientation, fibre length distribution and fibre dispersion in the composite material. 17 In the case of fibre volume fraction is concerned, the 40% fibre volume fraction showed higher mechanical properties than the other two combinations. It is interpreted that when 30% fibre volume fraction leads to lower composite stiffness, 50% fibre volume fraction leads to improper resin fibre wetting and improper strain wave distribution. 18 Similarly, the impact of alkali treatment enhances the surface roughness on the reinforcement; in this research work, 3% (W/W) alkali pretreatment improved the optimum surface roughness than the other two concentrations.
Experimental validation
The predicted optimized process variables are A2B2C2D1 for all the mechanical process parameters. Since the optimized combination of the experiment was not found in the matrix of experiments, an additional experiment has been conducted with the selected optimized process parameter. Further to this, the predicted S/N ratio has been calculated using the optimized process parameters of laying angle, fibre length, fibre volume fraction and alkali concentration. The formula-1 was utilized to find the predicted optimum S/N ratio
Experimental validation.
Using this S/N ratio, the predicted tensile, flexural and compression strength of the composite have been estimated through back transformation, which was 88.204 Mpa, 50.246 Mpa and 134.39 Mpa, respectively. Further, a composite was fabricated as per the optimized process parameters (A2B2C2D1). Its tensile, flexural and compression strength was measured as 73.34 Mpa, 52.812 Mpa and 130.21 Mpa, which are all much closer to the predicted estimated values.
Variance analysis
Analysis of variance for mechanical properties of sansevieria fibre composite.
Dynamic mechanical characteristics analysis
DMA analysis was carried out for five samples among the 18 experiments. The visco-elastic properties of the composite were measured through DMA analysis. The DMA analysis was referred to in three aspects such as storage modulus (E′), loss modulus (E″) and loss factors of the prepared samples
Storage modulus
The Storage modulus is referred as the energy absorbed by the sample due to the given cyclic oscillation load. In another way, it is the measure of the stiffness of the composite specimen. The variation in storage modulus as a function of temperature was studied for the composite samples. Figure 6 indicates the storage modulus of the sansevieria fibre reinforced composite from 25°C to 80°C. In general trend, the storage modulus decreases from the lower temperature range to the higher range. The values were obtained at the frequency of 1 Hz. But when the volume of the reinforcement increases, the storage modulus shows an increasing trend. Due to higher fibre loading the stiffness of the composite increases, and the fibre resin bonding also an important aspect for achieving higher.
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Among the 18 samples, the top five samples were considered for the investigation of DMA analysis. It was found that a similar trend was followed as per the mechanical study analysis. Experiment sample 17 showed the highest storage modulus; after this sample, the samples such as 14, 13, 11 and 9 were shown the next highest range of storage modulus. There will be no substantial changes in the storage modulus when the test temperature approaches a rubbery range, because the closely packed molecules are losing their arrangement and becoming a free state. The storage modulus values at the room temperature of composite samples are shown in descending order as follows: 17, 14, 13, 11 and 9. Sample reference 17 was found as superior stiffness properties than other specimen due to its optimized fibre parameters. The storage moduli (E′) vs. temperature of sansevieria fibre reinforced composites at the frequency range of 1 Hz.
The experiment 17 samples possessed the highest storage modulus value of 3.24 Gpa at room temperature because of the bonding strength between the fibre and resin, fibre stiffness, effective fibre length and optimized fibre volume fraction. Due to this reason, the interfacial bond strength of the composite has increased. Experiment sample 9 has got the lowest rating of 2.421 Gpa at room temperature. Though the difference between 17 and 9 samples was minimum, the cause of this difference is due to fibre orientation. The fibre orientation is the essential factor, which largely influenced the storage modulus of the composite.
Loss modulus
The loss modulus (E″) is referred to as the measure of energy dissipated as heat per cycle of deformation, and it is the viscous component of the composite material. The variation in viscous modulus was measured between the ranges of 20°C–160°C at the frequency of 1 HZ, which was indicated in Figure 7. The viscose response of the composite depends upon the molecular motion of the sample.
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Figure 7 has shown the Loss modulus (E″ (pa)) for all five samples in the different temperature ranges. All composite specimens were found to achieve the maximum loss modulus value in the glassy zone before dropping to the lowest range. As similar to the storage modulus, experiment sample 17 has shown the highest loss modulus. Subsequent to this sample, the experiment samples 14, 13, 11, 9 were shown the next highest loss modulus. This is because, the fibre is elastic in nature, and the polymer surrounded is also elastic, so increased energy absorption of the optimized fibre configuration such as fibre length, fibre volume fraction, and fibre to resin interface is the primary reason for obtaining the higher loss modulus
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The Loss Modulus (E″) vs. temperature of sansevieria fibre reinforced composites at the frequency range of 1 Hz.
The experiment 17 samples possessed the highest storage modulus value of 0.508 Gpa at a temperature of 30°C because of the bonding strength between the fibre and resin, fibre stiffness, effective fibre length and optimized fibre volume fraction. Due to this reason, the interfacial bond strength of the composite has increased. Experiment sample 9 has got the lowest rating of 0.463 Gpa at 300°C temperature.
Loss factor
The ratio between the storage modulus to loss modulus is known as loss factor (damping factor). The damping property of the composite gives the balance between the elastic phase to viscous phase of the composite. Damping is the dissipation of energy in a composite material under cyclic load. It is a measure of how well a material can get rid of energy and is reported as the tangent of the phase angle. It tells us how good a material will be at absorbing energy.
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Figure 8 shows the loss factor (tanα) for all the five samples in the different temperature ranges. The loss factor analysis was done between the temperature range of 20°C and 60°C with a frequency of 1 Hz. Sample 17 shows the lowest loss factor than other samples due to its optimized process variables. Since this composite was produced through epoxy resin, the fibre resin bond has also played a vital role in this higher storage modulus. On the other hand, the mechanical loss factor (tan α) shows an increasing trend from lower temperature to higher temperature. Around 73°C, the tan α value started decreasing while the temperature increases; this change point is referred to as a damping peak. Moreover, this loss factor is lower for higher volume fibre reinforced composite than lower volume fibre reinforcement or tanα decreases with fibre loading. This damping peak is due to the reduction in crystallinity of the resin component. As reported by Joseph et al.,
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this damping scenario is higher for high fibre volume fraction since the fibre reinforcement affects the crystallization of the resin compound. The Loss Factor (tan α) vs. temperature of sansevieria fibre reinforced composites at the frequency range of 1 Hz.
The experiment 17 samples possessed the lowest loss factor of 0.164, and experiment sample 11 has got the highest value of 0.207. Since sample 11 has got a comparatively lower fibre volume fraction than experiment sample 17, this fibre addition has acted as a barrier to reduce the energy loss rate and degree of the polymer molecule chain.
Scanning electron microscopy
The fibre–matrix interfacial bonding behaviour of transverse tensile fracture is shown in Figure 9. It is a kind of ductile breakage due to the improper penetration of the matrix in certain places inside the fibre. The fibres are not visible due to the optimized viscosity of the resin. The fibre impregnation was also found in many places in the images. The resin accumulation is found more in certain places, due to which the resin broke directly during the fracture testing. Figure 9(b) shows the fibre pull-out during fracture testing, which again reconfirms the ductile failure of the matrix. SEM. Image of the sansevieria fibre reinforced composite.
Conclusion
In this research, various mechanical characteristics and dynamic mechanical properties of the sansevieria fibre reinforced composite was examined under the change of fibre alignment, fibre length, fibre volume fraction and alkali pretreatment. Optimized process variables have been arrived at using S/N analysis. It can be concluded from ANOVA that most of the selected process parameters have affected the tensile, flexural and compression strength at 95% confidence level. Generally, the adhesion between sansevieria fibre and matrix is poor. However, the adhesion can be improved by surface modification of coir fibres through alkali pretreatment. The optimized tensile, flexural and compression strength of the samples are 73.34 Mpa, 52.812 Mpa and 130.21 Mpa respectively. In the case of DMA analysis, the maximum storage modulus, loss modulus and loss factor were found as 3.24 Gpa, 0.508 Gpa and 0.164 at room temperature. The nature of the composite failure was discovered by SEM research, and it is largely related to the ductile nature of the resin.
Footnotes
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.
Funding
The author(s) received no financial support for the research, authorship, and/or publication of this article.
