# Mechanical and microstructural characterization of laminate composites hybridised with carbon fibre and rice husk particulate fillers

Dayanidhi Jena, Shaswat Kumar Das

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Dayanidhi Jena, Shaswat Kumar Das. Mechanical and microstructural characterization of laminate composites hybridised with carbon fibre and rice husk particulate fillers. Journal of Umm Al-Qura University for Engineering and Architecture, 2025, 10.1007/s43995-025-00251-9. hal-05526647

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# Mechanical and microstructural characterization of laminate composites hybridised with carbon fibre and rice husk particulate fillers

Dayanidhi Jena<fnref n="1" /> · Shaswat Kumar Das<fnref n="2" />,<fnref n="3" /> †

Received: 13 June 2025 / Accepted: 16 October 2025

© The Author(s) 2025

## Abstract

This current work have investigated the mechanical properties of a polymer composite hybridized with particulate rice husk (PRH) and particulate carbon fibre (PCF). The hand lay-up fabrication process is adopted to develop the composite. Mechanical properties such as compressive strength, tensile strength, and flexural bending strength of the developed hybrid polymer composite, and composites with single fillers at different weight percentages of PRH and PCF, are analysed through the experimental program. It is observed from the experiments that both types of composites exhibit low mechanical strength in tension, but demonstrate good strength in both compression and bending. Furthermore, it is noted that the hybrid composite containing 5% weight of PRH and 5% weight of PCF exhibits superior mechanical properties in tension, compression, and bending compared to other compositions. The corresponding values are 17.89 MPa, 93.84 MPa, and 114 N, respectively. Scanning electron microscope (SEM) surface morphology analysis reveals that the tensile and bending fractures of the composite are of a brittle type.

**Keywords** Hybrid polymer composite · Particulate rice husk · Particulate carbon fibre · Mechanical properties · Filler volume fraction

## 1 Introduction

The incorporation of natural fibres in various polymer composites has gained significant attention due to their easy availability, lower cost, renewable nature, and various advantages over synthetic fibres [1–3]. Natural fibres such as rice husk, sisal, hemp, jute, banana, kenaf, bamboo, and flax etc. have gained scientific attention due to several

benefits such as lightweight, low specific gravity and density, tolerable specific properties, low energy requirement for processing, wide availability, ecofriendly, economical and relative non-abrasiveness compared to conventional reinforcing fibres such as glass and carbon [2, 4]. However, the utilization natural fibres in reinforced polymer composites face challenges due to their low mechanical performances, high variability, susceptibility to moisture, weak adhesion between fibre and matrix, which limit the of natural fibre reinforced composites (NFRPCs) in some applications [5]. To address these challenges, hybrid composites combining natural fibres with synthetic fibres like glass or carbon have been explored [1, 6–11]. In earlier studies, to overcome this issue of NFRPCs, experiments have been conducted taking glass fibre-reinforced composites hybridized with natural fibres such as pineapple leaf, kenaf, sisal, jute, and bamboo to enhance their mechanical properties [11–16]. Similarly, in some other studies, carbon fibre (CF)-reinforced composites hybridized with natural fibres have also shown promising mechanical properties compared to NFRPCs [17–21]. Overall, the amalgamation of synthetic

<footnote>Dayanidhi Jena
dayanidhijena_fme@gcekjr.ac.in</footnote>

<footnote>Shaswat Kumar Das
skd.gtcr@gmail.com</footnote>

<footnote n="1">¹ Department of Mechanical Engineering, Government College of Engineering, Keonjhar 758002, Odisha, India</footnote>

<footnote n="2">² BUILDERS Ecole D'ingénieurs, Unité de Recherche "Builders Lab", ComUE NU, Campus Caen, Épron 14610, France</footnote>

<footnote n="3">³ GeM - Institut de Recherche en Génie Civil et Mécanique, CNRS, UMR 6183, Saint-Nazaire 44600, France</footnote>
fibres with natural fibres offers the potential to overcome the limitations of NFRPCs while leveraging the benefits of both types of fibres to achieve desirable performances in various applications.

It's interesting to note the trend of using hybridized natural fibres in polymer composites to enhance their mechanical properties is gaining more popularity in recent years and several studies have been undertaken by various researchers [22–27]. Rice husk (RH), in particular, has gained significant attention due to its easy availability and biodegradability [28, 29]. Many researchers have explored combining RH with other natural or synthetic fibres, such as talc, jute, waste glass, Nano hybrid silica, organ clay, and red mud, to further improve the properties of the composites [30–35]. For instance, Satapathy et al. [30] suggested that hybridizing RH-derived SiC (Silicon carbide) fibres with jute-epoxy composites can enhance the flexural, tensile, and inter-laminar shear strength of the resulting composite materials. This highlights the potential benefits of incorporating multiple types of fibres to achieve desired mechanical properties in polymer composites.

Furthermore, a study on the mechanical behaviour of a composite based on RH and glass fibre revealed that it was more optimal in terms of compressive strength, thermal conductivity, dynamic stiffness, enhancement in impact sound insulation and sound absorption, and transmission loss [36]. Based on experimental data, the authors [37] reported that the chemically treated pineapple leaf fibre samples give better water absorbing performance than the untreated fibre in the composite mixed with 6% nano RH. Further, experiments with the hybrid foam panel (HFP) composite, consisting of polyurethane and diphenylmethane with various compositions of white Portland cement and RHA (rice husk ash) fillers, indicate that it could be utilized as an interior solar heat blockade, especially in tropical fields [38].

In addition, rice RH-derived graphitic carbon finds its application an electrode material with hierarchical pores, reported by Wang et al. [39]. As observed by Sunday [40], carbon nanoparticles from RH modified with silver nanoparticles can be used to make high-friction brake pads and related applications. Furthermore, Kumagai and Matsuo reported that the composite of RH without binder shows the highest mechanical strength and optimal sliding properties when heated up to 1000 °C, which is better than the chopped carbon fibre (CF) filled samples [41]. Moreover, Falalu et

al. reported that the carbon nanotubes and RH powder can be used to make a new type of bio-composite that can significantly improve the performance of polymeric materials [42]. However, their study focused to develop composites for construction and building materials applications. The literature involving RH and CF to develop composites for various mechanical applications is scarce and need further investigations.

Overall, the study aims to fill a gap in the existing literature by investigating the mechanical properties of polymer composites hybridized with RH and particulate CF (PCF) fillers and provides insights into the performance of these composites under different loading conditions.

# 2 Experimental program

## 2.1 Materials

For the matrix material, epoxy resin (Araldite, Grade LY 556) was sourced from Hindustan Ciba Geigy Limited, Mumbai, India. The corresponding hardener for the matrix is of grade HY 951. The used PCF was sourced from Hindustan Ciba Geigy Limited, Mumbai, India with a particle size range of 100–200 µm. The rice husk (RH) used in this study is collected from Shiva Shakti rice mill situated in Dhenkanal, Odisha, India. After obtaining the RH, it was further converted to PRH of with a similar particle size range of 100–200 µm as like PCF. The physico-mechanical properties of the raw materials essential to fabricate the composite are listed in Table 1. The scanning electron microscopy (SEM) images of the PRH and PCF are shown in Fig. 1. From the SEM observations, it can be clearly noticed that the PRH has more of a spherical and spongy microstructure, whereas the PCF has needle like structures.

## 2.2 Sample preparation

The particulate rice husk (PRH) is first dried in a hot air oven at a temperature of 100–110 °C for 2 h. This step likely removes any moisture or volatile components from the material. After drying, the PRH is mixed with other required materials at different weight proportions to create the final composite mixture. This mixing process likely involves combining the PRH with reinforcing materials or fillers to enhance its mechanical properties. The composite mixture is then used to prepare specimens for mechanical testing using the hand lay-up method of vacuum moulding. This process involves laying the composite material into a mould and applying vacuum pressure (maintained at 500 torr) to remove air bubbles and ensure proper compaction of the material within the mould. After moulding, the

<table><caption>**Table 1** Physico-mechanical properties of the Raw materials</caption><thead><tr><td>Materials</td><td>Density (g/cc)</td><td>Tensile strength (MPa)</td><td>Modulus of Elasticity (GPa)</td></tr></thead><tbody><tr><td>Epoxy</td><td>1.1</td><td>90–120</td><td>4.3</td></tr><tr><td>PCF</td><td>1.8–2.1</td><td>5–76</td><td>4.1–27.6</td></tr><tr><td>PRH</td><td>0.5</td><td>19–135</td><td>0.3–2.6</td></tr></tbody></table>
<figure><img src="image_3.png" /><figcaption>Fig. 1 SEM images of (a) Particulate rice husk (PRH) (b) Particulate carbon fibre (PCF)</figcaption></figure>

<figure><img src="image_4.png" /><figcaption>Fig. 2 Specimens for static tests</figcaption></figure>

manufactured specimens are allowed to stay for 24 h inside the vacuum chamber for solidification. This ensures that the composite material sets and cures properly before further processing. The prepared specimens are then subjected to a curing process at three different temperatures incrementally: 600 °C, 800 °C, and 1000 °C. Once cured, the specimens are prepared by using diamond cutter according to ASTM standards for mechanical testing as mentioned below.

* ASTM E8 standard specimens for tensile testing [43].

* ASTM E9 standard specimens for compressive strength testing [44].

* ASTM D790 standard specimens for three-point bending testing [45].

Overall, this process ensures that the composite specimens are properly prepared and cured to meet the required standards for mechanical testing, allowing for accurate assessment of their mechanical properties. Each temperature condition is maintained for two hours. This curing process helps to further strengthen the composite material and improve its mechanical properties. The specifications of three ASTM standard specimens are depicted in Fig. 2.

## 2.3 Experiments

In this study, the static tensile, compressive, and flexural tests are conducted using a BISS 100kN UTM at displacement control mode in Advanced Material Testing Lab at Government College of Engineering, Keonjhar, Odisha, India. During the experiment, displacement is set at 2 mm/min for every test. For each observation, 3 repetitions of experiments are conducted. Figure 3 shows the experimental set up for different experiments.
<figure><img src="image_5.png" /><figcaption>BISS 100 kN UTM</figcaption></figure>

<figure><img src="image_6.png" /><figcaption>Tensile Test</figcaption></figure>

<figure><img src="image_7.png" /><figcaption>Compressive Test</figcaption></figure>

<figure><img src="image_8.png" /><figcaption>Three-point Bending Test</figcaption></figure>

<figure><img src="image_9.png" /><figcaption>Fig. 4 Tensile Stress - % strain diagram for hybrid composite</figcaption></figure>

<figure><img src="image_10.png" /><figcaption>Fig. 6 Flexural bending test results for hybrid composite</figcaption></figure>

<figure><img src="image_11.png" /><figcaption>Fig. 5 Compressive stress - % strain diagram for hybrid composite</figcaption></figure>

# 3 Results and discussion

## 3.1 Static tensile, compressive and three-point bending test for hybrid composite

In the first part of the experiment, static tensile tests were

conducted on a hybrid composite material. The hybrid composites consisted of 5% wt. of PCF with varying wt% of PRH. The static tensile stress -% strain diagram, shown in Fig. 4 illustrates that stress varies linearly with strain for all compositions of the hybrid composite. Moreover, it was noted that the hybrid composite exhibited a brittle behaviour akin to glass, as evidenced by consistent proportional limit, elastic limit, yield point, ultimate point, and breaking point across all compositions.

Figure 5 illustrates a nonlinear stress-strain relationship for the composite, indicating distinct ultimate and breaking points. Notably, the ultimate stress surpasses the breaking stress, showcasing the material's ability to withstand higher stress levels before failure.

In the subsequent phase of the experiment, a three-point bending test was conducted on the hybrid composite to assess its static flexural bending strength. Figure 6 illustrates the bending load versus displacement diagram for the hybrid composite at different weight percentages of PRH. It is notable from Fig. 6 that as the percentage of PRH increases, the flexural load initially decreases before subsequently increasing. The minimum flexural load is observed
for the hybrid composite with 10% weight of PRH, while the maximum is at 20% weight of PRH.

Figure 7 illustrates a comparison of the mechanical properties of the hybrid composite with increasing weight% of PRH. It is observed that up to around 15% weight% of PRH, there is a decrease in mechanical strength. After this point, the mechanical properties vary randomly. This phenomenon is attributed to the non-uniform dispersion of filler particles within the matrix materials. Interestingly, at 5% weight% of rice husk, superior mechanical properties are obtained. This suggests an optimal concentration of PRH for enhancing mechanical properties, likely due to improved dispersion and interaction between the filler particles and the matrix material at this concentration. Further adjustments in the weight% of PRH might be necessary to fine tune the mechanical properties of the composite material for specific applications.

In the conducted static compressive test for the hybrid composite, it was observed from the Fig. 7 that the tensile strength ranged from 9.25 MPa to 18.12 MPa across different compositions. Specifically, the minimum tensile strength was observed for the hybrid composite containing 10% wt. of PRH, while the maximum was observed at 15% wt. of PRH. Further, the compressive strength decreases with an increase in the weight% of PRH filler. The maximum compressive strength achieved was 93.84 MPa, recorded at a 5% PRH content. However, the hybrid composite with 5% weight of PRH exhibits favourable strength characteristics in tensile, compressive, and flexural tests. Specifically, the tensile strength is measured at 17.89 MPa, compressive strength at 93.84 MPa, and flexural strength at 114 N. These findings suggest that the addition of PRH to the composite material influences its mechanical properties differently depending on the weight%. At lower percentages, it may enhance certain properties, while at higher percentages, it might have a detrimental effect. The optimal balance appears to be achieved with 5% weight of PRH, as it demonstrates good strength across various tests.

Figure 7 likely presents the trend of compressive strength with varying PRH percentages. The observed decrease in compressive strength with increasing PRH content suggests a compromise between composite strength and the incorporation of PRH filler. Further analysis is warranted to elucidate the underlying mechanisms governing this behaviour and optimize the composite formulation for specific application requirements.

## 3.2 Static tensile, compressive and three-point bending test of composite with single filler

After conducting static tensile, compressive, and three-point bending tests on composites with a single filler, it

<figure><img src="image_12.png" /><figcaption>Fig. 7 Comparison of static tensile, compressive, and flexural strength of hybrid composite</figcaption></figure>

<figure><img src="image_13.png" /><figcaption>Fig. 8 Static tensile test results of composite with single filler</figcaption></figure>

was observed that the static tensile strength behaves differently depending on the filler type. With an increase in the weight% of filler, the static tensile strength decreases when using PRH filler, whereas it increases when using PCF filler. The highest static tensile strength was achieved with a composite containing 15% weight of PCF. Analysis of Fig. 8 indicates that PCF filled composites exhibit superior tensile strength compared to PRH filled composites. This is due to higher tensile property of PCF and improved dispersion and interaction between the PCF and the matrix material at this concentration.

The results depicted in Fig. 9 outline the outcome of static compressive testing on composites with single fillers. It is evident from the data that the compressive strength of the composite decreases as the weight% of PRH filler increases. Conversely, in the case of PCF filler, there is an initial increase in compressive strength with a rise in weight%, reaching its peak value of 101.138 MPa at 10% weight of PCF, followed by a subsequent decrease.
<figure><img src="image_14.png" /><figcaption>Fig. 9 Static compressive test results of composite with single filler</figcaption></figure>

<figure><img src="image_15.png" /><figcaption>Fig. 10 Static three-point bending test results of composite with single filler</figcaption></figure>

Figure 10 displays the results of static three-point bending test for composite with single filler. The flexural bending strength initially increases and then decreases with increase in % filler. For PCF filled composite the maximum value of flexural bending load is 132 N at 10% wt. of PCF and for PRH filled composite is 75.5 N at 10% wt. of PRH.

<figure><img src="image_16.png" /><figcaption>Fig. 11 SEM images of hybrid composite (5% wt. of PCF & 5% wt. of PRH) before and after tensile test at 10,000 X magnification</figcaption></figure>

The comparison study between hybrid composites and composites with a single filler indicates that composites containing 10% weight of PCF exhibit the highest strength in both compressive and bending tests. This suggests that the incorporation of PCF at a concentration of 10% by weight enhances the mechanical properties of the composite significantly, surpassing those of composites with a single filler material. Such findings hold potential implications for diverse applications where superior strength in compression and bending is crucial, such as in engineering structural components or construction materials.

## 4 SEM surface morphology

In this part, the surface morphology analysis of the hybrid as well as composite with single filler is carried out by using ZEISS SEM at Advanced Material Testing Lab, Government college of Engineering, Keonjhar, India. Gold coating is done for each specimen before conducting SEM test.

Figures 11 and 12 show the tensile fracture surface and bending fracture surface morphology of hybrid composite at 5% wt. of PCF and 5% wt. of PRH at different magnification. From normal surface morphology, it is observed that, there is a uniform distribution of fillers in matrix materials. We observed some voids in the structure of the composite. It may be due to adoption of hand moulding process of fabrication. Figure 11 describes tensile fracture surface morphology of hybrid composite at 5% PCF and 5% PRH. It is noticed that the tensile fracture is of brittle fracture followed by filler pull out. Here PCF is pulled out first in tension and then breaks down. There is no pull out of PRH in tension.

Figure 12 describes bending fracture surface morphology of hybrid composite at 5% PCF 5% PRH. It is observed that the bending surface morphology is like that of tensile fracture surface morphology. But there is less PCF pull out as compared to tensile fracture.

Figures 13 and 14 show the normal surface, tensile fracture surface and bending fracture surface morphology of
<figure><img src="image_17.png" /><figcaption>**Fig. 13** SEM surface morphology of composite (10% wt. of PCF) before and after tensile test at 10,000 X</figcaption></figure>

<figure><img src="image_18.png" /><figcaption>**Fig. 14** SEM surface morphology of composite (10% PCF) before and after bending test at 10,000 X</figcaption></figure>

<figure><img src="image_19.png" /></figure>

<figure><img src="image_20.png" /></figure>

<figure><img src="image_21.png" /></figure>

<figure><img src="image_22.png" /></figure>

composite of single filler (10% PCF) at 10000X magnification. It is observed that both tensile and bending fracture surface morphology is similar. The fracture of composite follows PCF pull out.

The EDX results of hybrid composite at 5% PCF and 5% PRH and composite with single fibre (10% PCF) is shown in the Figs. 15 and 16, respectively and describes the peaks of elements present in the above compositions. It is noticed that the weight% of carbon is the highest for all compositions.

The comparison of EDAX results for hybrid composite at 5% PCF & 5% PRH and composite with single fibre (10% PCF) is shown in the Table 2. It is seen that the weight%

and atomic % of carbon for both type of composite is nearly same but for other elements like sodium and silicon it is different, mainly due to the presence silica in PRH.

# 5 Physical characterization

## 5.1 Density measurement

After developing the samples at different wt% of rice husk, its mass and volume is calculated to know its density. Density is calculated as, $density = mass(gm)/volume(cc)$. The
<figure><img src="image_23.png" /><figcaption>**Fig. 16 EDX results of composite at 10% PCF**</figcaption></figure>

<figure><img src="image_24.png" /><figcaption>**Table 2 Comparison of EDAX results of hybrid composite and composite with single filler**</figcaption></figure>

<table><caption>**Table 3 Variation of density of hybrid composite**</caption><thead><tr><th rowspan="2">Element</th><th colspan="2">Weight%</th><th colspan="2">Atomic %</th></tr><tr><th>Hybrid</th><th>With single filler</th><th>Hybrid</th><th>With single filler</th></tr></thead><tbody><tr><td>C</td><td>94.3</td><td>94.7</td><td>97.5</td><td>97.6</td></tr><tr><td>Na</td><td>0.6</td><td>1.3</td><td>0.3</td><td>0.7</td></tr><tr><td>Si</td><td>4.6</td><td>3.4</td><td>2.0</td><td>1.5</td></tr><tr><td>K</td><td>0.5</td><td>0.5</td><td>0.2</td><td>0.2</td></tr></tbody></table>

<table><thead><tr><th>Wt. % of rice husk</th><th>Density in g/cc</th></tr></thead><tbody><tr><td>10</td><td>1.71</td></tr><tr><td>15</td><td>1.73</td></tr><tr><td>17</td><td>1.76</td></tr><tr><td>20</td><td>1.60</td></tr><tr><td>22</td><td>1.38</td></tr><tr><td>24</td><td>1.43</td></tr><tr><td>26</td><td>1.53</td></tr><tr><td>28</td><td>1.42</td></tr></tbody></table>

calculated value of density of hybrid composite with the variation of wt% of rice husk is mentioned in Table 3.

It is observed that up to 17% PRH the packing density increases which leads to maximum density at this composition. Then after, there is a random variation of density. It is due to dispersion problem in mixing fibre and matrix materials, and the random orientation of fibre particles inside the matrix.

## 5.2 Micro hardness measurement

The Vicker's hardness test method: A right pyramid with a square base and an angle of 136° between opposite faces subjected to a load of 100 Kgf. The load is applied for 20 s. Two diagonal indentations left in the material is measured. The Vicker's Hardness is the quotient obtained by dividing the square of the load by area of indentation (Fig. 17).

The results of micro hardness of samples with varying % of PRH is presented in Table 4. Interestingly at 15 wt% of PRH, the packing density increases which leads to the
<figure><img src="image_25.png" /><figcaption>**Table 4** Hardness values of the hybrid composite</figcaption></figure>

<table><thead><tr><th>Wt.% PRH</th><th>Load in Kgf</th><th>Dwell Period(sec)</th><th>Hardness (Hv)</th><th>Average (Hv)</th></tr></thead><tbody><tr><td>10</td><td>100</td><td>20</td><td>34.5</td><td>29.1</td></tr><tr><td>10</td><td>100</td><td>20</td><td>23.7</td><td></td></tr><tr><td>15</td><td>100</td><td>20</td><td>41.9</td><td>43</td></tr><tr><td>15</td><td>100</td><td>20</td><td>48.7</td><td></td></tr><tr><td>15</td><td>100</td><td>20</td><td>38.8</td><td></td></tr><tr><td>15</td><td>100</td><td>20</td><td>43.4</td><td></td></tr><tr><td>20</td><td>100</td><td>20</td><td>19.1</td><td>16.35</td></tr><tr><td>20</td><td>100</td><td>20</td><td>13.6</td><td></td></tr></tbody></table>

increase in density and hence the hardness, as shown in both the Table 4; Fig. 18.

## 6 Conclusions

The study investigated the mechanical properties of a polymer composite reinforced with particulate rice husk (PRH) and particulate carbon fibre (PCF) through experimentation. The fabrication process involved hand lay-up, and the analysis focused on comparing the mechanical properties of the hybrid composite and composites with single fillers at varying wt% of PRH and PCF. The conclusions from this study are:

1. Both types of composites exhibited low mechanical strength in tension but demonstrated good strength in compression and bending.

2. The hybrid composite containing 5% PRH and 5% PCF showed superior mechanical properties in tension,

<figure><img src="image_26.png" /><figcaption>**Fig. 18** Indentations at 15% wt. of PRH</figcaption></figure>
compression, and bending compared to other compositions. The observed values were 17.89 MPa for tension, 93.84 MPa for compression, and 114 N for bending.

3. SEM surface morphology analysis revealed that the tensile and bending fractures of the composite exhibited brittle characteristics.

4. Energy Dispersive X-ray Analysis (EDAX) indicated that the weight% and atomic % of carbon and potassium were similar for both types of composites. However, there were differences in the weight% and atomic % of other elements such as sodium and silicon.

These findings suggest that the hybrid composite with 5% PRH and 5% PCF has promising mechanical properties, indicating its potential for various applications where a combination of tensile, compression, and bending strength is required. Additionally, the differences observed in the elemental composition between the composites could provide insights into their respective material characteristics and behaviours.

**Acknowledgements** The authors would like to acknowledge Government College of Engineering, Keonjhar, Odisha, India, for their laboratory support to conduct all experiments. This research did not receive any specific grant from funding agencies in the public, commercial, or not-for-profit sectors.

**Authors' contribution** DJ: Conceptualization, Investigation, Methodology, Software, Data curation, Writing- Original Manuscript Draft; SKD: Validation, Analysis and interpretation, Writing- Reviewing and Editing.

**Funding** This research did not receive any external funding.

**Data availability** All the manuscript data will be available upon request from the corresponding author(s).

## Declarations

**Competing interests** None.

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