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Characterization of continuous Hibiscus sabdariffa fibre reinforced epoxy

composites

Article  in  Polymers and Polymer Composites · January 2022

DOI: 10.1177/09673911211060957

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Original Research Article

Polymers and Polymer Composites

Volume 30: 1–10
Characterization of continuous Hibiscus © The Author(s) 2022
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DOI: 10.1177/09673911211060957
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Atik Mubarak Kazi  and Ramasastry DVA

Abstract
The influence of fibre orientation on physical, mechanical and dynamic mechanical properties of Hibiscus sabdariffa fibre
composites has been studied. The composites with longitudinal (0°), transverse (90°) and inclined (45°) fibre orientation were
prepared using the hand layup technique. ASTM standards were used for characterization of continuous Hibiscus sabdariffa
fibre composites. The composite with longitudinally placed fibres yields improved mechanical characteristics. The addition of
longitudinal (0°) oriented continuous Hibiscus sabdariffa fibres to the epoxy enhances tensile strength by 460%, flexural
strength by 160% and impact strength by 603% compared to neat epoxy. The longitudinal (0°) fibre oriented composite offers
higher resistance to water absorption and thickness swelling compared to other types of composites. All continuous Hibiscus
sabdariffa fibre epoxy composites possess an improved storage modulus than the neat epoxy resin. The glass transition
temperature of continuous Hibiscus sabdariffa fibre composites is 8%–31% lower than that of neat epoxy. Scanning electron
microscopy (SEM) images confirm the existence of voids in the matrix, fibre pullout and crack propagation near the fibre
bundle, which indicates the stress transfer between fibre and matrix is non-uniform.

Keywords
Hibiscus sabdariffa fibre, fibre orientation, mechanical properties, dynamic mechanical analysis

Received 20 February 2021; accepted 31 October 2021

Introduction
Reinforcing polymers with synthetic fibres such as carbon, aramid and glass can improve their mechanical performance.1
Hence, these synthetic fibre polymer composites are widely used in aerospace, marine, automotive, sports and agricultural
applications.2,3 The heavy use of synthetic fibre composites raised many environmental issues.4,5 From the last few decades,
natural fibres are the most commonly used reinforcement in polymer composites. It is because of their benefits such as being
eco-friendly, cheap, light in weight and good strength.6,7 The natural fibres are readily available in nature, and their extraction
is also so simple. Natural fibres like jute, sisal, kenaf, hemp, banana, roselle, coconut coir, pineapple leaf, sugar palm and date
palm are frequently used to reinforce the polymers.8,9 Hibiscus sabdariffa is the scientific name of roselle plant. H. sabdariffa
is cultivated in South Asia and Africa for food and medicine purposes.8 H. sabdariffa bast fibres can be extracted from dried
Hibiscus sabdariffa plants using the water retting process.8 The mechanical properties of H. sabdariffa fibres are comparable
to those of jute and kenaf fibres.9
Singha and Thakur10–12 developed Hibiscus sabdariffa fibre phenol-formaldehyde composites. For this, they used Hibiscus
sabdariffa fibres in particle and chopped form. Kazi et al.13 investigated characteristics of woven Hibiscus sabdariffa fibre
epoxy composites and suggested these materials for automotive interiors, door panels, dashboards, etc. Chavali and Taru14
studied the tensile and wear behaviour of unidirectional banana fibre epoxy composites. They examined 0°, 15°, 45°, 75° and
90° fibre oriented composites and concluded that 0° fibre oriented composite performs better. Roa et al.15 investigated the
impact of fibre orientation and fibre loading on the mechanical behaviour of Hardwickia binata and bamboo fibre composites.
They prepared both Hardwickia binata and bamboo fibre composites with 0°, 45°, 60° and 90° orientations, and 8%, 16% and
24% fibre content by weight. They concluded that composites with a fibre content of 24% by weight and 0° orientation yield
better results. Cordin et al.16 examined the mechanical characteristics of 0°, ±22.5°, ±45°, ±67.5° and 90° oriented lyocell fibre

Department of Mechanical Engineering, Koneru Lakshmaiah Education Foundation, Vaddeswaram, India

Corresponding author:
Atik Mubarak Kazi, Department of Mechanical Engineering, Koneru Lakshmaiah Education Foundation, Vaddeswaram, Andhra Pradesh 522502, India.
Email: [email protected]
Creative Commons CC BY: This article is distributed under the terms of the Creative Commons Attribution 4.0 License
(https://creativecommons.org/licenses/by/4.0/) which permits any use, reproduction and distribution of the work without
further permission provided the original work is attributed as specified on the SAGE and Open Access pages (https://us.sagepub.com/en-
us/nam/open-access-at-sage).
2 Polymers and Polymer Composites 0(0)

polypropylene composites. Yoganandam et al.17 explored characteristics of madar and gongura fibre reinforced hybrid
composites. Hassan et al.18 investigated tensile and flexural properties of 0°, 45° and 90° oriented oil palm empty fruit bunch
fibre composites. They observed excellent tensile and flexural properties for 0° oriented composite. Tholibon et al.19 studied
the tensile behaviour of continuous kenaf fibre polymer composites. Devireddy and Biswas20,21 explored the physical,
mechanical and thermal characteristics of unidirectional banana and jute fibre hybrid composites.
Venkatachalam et al.22,23 studied the impact of alkali treatment on the mechanical behaviour of jute and gongura hybrid
fibre polymer composites. Biswas et al.24 compared the mechanical and thermal performance of jute fibre composite with
bamboo fibre composite. Kumarsen et al.25 revealed that the longitudinal-oriented sisal fibre epoxy composite yields better
mechanical properties than the cross-ply sisal fibre composites. Badrinath and Sethilvelan26 compared the mechanical
properties of banana and sisal fibre composites. Mahjoub et al.27 studied the influence of fibre content on tensile characteristics
of the unidirectional kenaf fibre composites. Tensile and flexural properties of unidirectional sisal fibre composite are better
than mat-type sisal fibre composite.28 Laranjeira et al.29 compared the mechanical properties of unidirectional kenaf polyester
composite with short- and random-oriented kenaf polyester composite. Wazzan30 carried out a comparison between the
mechanical properties of woven and unidirectional date palm fibre composite. Herrera-Franco and Valadez-Gonzalez31
studied the influence of silane treatment on the mechanical properties of continuous henequen fibre composites. Lee et al.32
investigated the combined effect of fibre orientation (0°, 45°, 90° and random) and fibre loading (30%, 40% and 50%
by weight) on the mechanical properties of kenaf fibre composites. They found that the 0° oriented kenaf fibre composite with
40 wt. % fibre loading possesses improved mechanical properties.
The present study covers the physical, mechanical and dynamic mechanical performance of continuous Hibiscus sabdariffa fibre
reinforced epoxy composites. The composites with longitudinal, transverse and inclined fibre orientation are considered for this study.

Materials and methods

Materials
In this study, continuous Hibiscus sabdariffa bast fibres are used as reinforcement, and the mixture of epoxy (GY257) and
hardener (HY140) is used as matrix material. The Hibiscus sabdariffa fibres were purchased from the local market. Epoxy
(GY257) and hardener (HY140) were obtained from Shree Industrial Composite Products, Hyderabad, India.

Composites preparation
For this research work, continuous Hibiscus sabdariffa fibre epoxy composites with fibre orientation 0° (longitudinal), 90°
(transverse) and 45° (inclined) were prepared by using the hand layup method. The composite plates were fabricated using an
aluminium mould measuring 300 mm by 150 mm by 4 mm. At first, all mould surfaces coated with Carbonblack Composite’s
mould releasing wax for quick release of the composite plate from the mould. The resin is prepared by mixing epoxy and
hardener in a 2:1 weight ratio. The prepared epoxy resin is applied on the mould bottom surface, and then the continuous
Hibiscus sabdariffa fibres are arranged manually in the mould. The remaining epoxy resin is poured onto it. The trapped air
bubbles in the composites were eliminated with the help of a roller. Finally, the mould was closed, and the load of 60 kg was
put on it. After 24 hours, the cured composite plate was collected from the mould, and test specimens were cut as per ASTM
norms. The fibre loading for all these composites was maintained at approximately 30% by weight. For this, the required exact
amount of resin and fibre is determined using the composites rule of mixture. Figure 1 shows a schematic representation of the
continuous Hibiscus sabdariffa fibre composites used in this study.

Characterization of the composites

Physical properties
Density and void content. Experimental densities of continuous Hibiscus sabdariffa fibre composites are obtained according to
the ASTM D 792 standard. For this work, specimens are sized to 50 mm by 10 mm by 4 mm. The specimen mass in air and

Figure 1. Schematic representation of the continuous Hibiscus sabdariffa fibre composites with various fibre orientations.
Kazi and DVA 3

mass in distilled water were recorded using an analytical balance with 1 mg resolution. Based on equation (1), the composite
density is determined
a
ρ¼ × 997:6 (1)
ab
in this equation, ρ is the composite density, a is the specimen mass in air and b is the specimen mass in distilled water. For each
case, three specimens were examined, and the mean value is considered.
The void content is determined using ASTM D 2734 standard. The given equation (2) gives an expression for percentage
void content
Td  Md
V ¼ × 100 (2)
Td
in this equation, Td is the theoretical composite density, Md is the measured composite density and V is the percentage void
content.

Water absorption behaviour. Water absorption behaviour of continuous Hibiscus sabdariffa fibre composites studied as per
ASTM D 570 standard. For this test, specimens are sized to 76 mm by 25 mm by 4 mm. At first, the test specimens are dried in
the oven for 5 hours at 50°C. On cooling in a desiccator, the dried specimen mass is recorded using an analytical balance. The
specimen is then immersed in distilled water, and specimen mass is recorded at every 24 hour time interval for the next
15 days. An analytical balance with 1 mg resolution was used for this test. The percentage of water absorption is determined
based on equation 3
Mt  M0
WAðtÞ ¼ × 100 (3)
M0
where WAðtÞ is the percentage water absorption at time t, Mt is the wet specimen mass at time t and M0 is the oven-dried
specimen mass.

Thickness swelling behaviour. The specimens of size 76 mm by 25 mm by 4 mm were used for the thickness swelling test. The
oven-dried specimen thickness was measured using a Vernier calliper. The specimen is placed in distilled water, and the
thickness is recorded at every 24 hour time interval until no change in specimen thickness is observed. The percentage
thickness swelling is determined based on equation 4
Tt  T0
TSðtÞ ¼ × 100 (4)
T0
where TSðtÞ is the percentage thickness swelling at time t, Tt is the wet specimen thickness at time t and T0 is the oven-dried
specimen thickness.

Mechanical testing
Tensile and flexural behaviour of Hibiscus sabdariffa fibre composites studied using Zwick-Roell (model Z020) universal
testing machine with a load cell capacity of 20 kN. The tensile test specimens are as shown in Figure 2. Izod impact tester is
used to conduct an unnotched impact test. For the flexural test, the support span to thickness ratio of the specimen was

Figure 2. Tensile test specimens (a) Longitudinal (0°) fibre oriented composite, (b) Transverse (90°) fibre oriented composite and (c)
Inclined (45°) fibre oriented composite.
4 Polymers and Polymer Composites 0(0)

maintained at 32:1. The support span is the specimen length between two supports in the flexural test set up. Table 1 shows
details for mechanical testing.

Scanning electron microscopy

Scanning electron microscopy (SEM) analysis is done to inspect the tensile failure surfaces of the composites. FEI (Model:
Apreo LoVac) microscope with a magnification range from 10× to 300,000× is used for this study. At first, sputter coating is
done on tensile failure surface using Leica Ultra Microtome sputter coater (Model: EM UC7). Then, the sputter-coated surface
was studied under the microscope at magnifications of 100× to 650×.

Dynamic mechanical analysis

Dynamic mechanical analysis (DMA) test is carried out as per ASTM D 4065 standard. TA instrument DMA Q 800 is used for
this test. DMA test specimen is sized to 50 mm by 10 mm by 4 mm. The DMA test is done in dual cantilever mode at 1 Hz
frequency by varying temperatures from 0°C to 200°C.

Results and discussion

Physical properties
Density and void content. Table 2 compares the experimental values of composite densities with the theoretical ones. Also,
Table 2 provides details of the content of voids in the composites. The results show that experimental values are so close to
respective theoretical values. It indicates that composite samples are of good quality.

Water absorption behaviour. H. sabdariffa fibres are hydrophilic in nature. Hence, water absorption behaviour is a significant
physical property of the Hibiscus sabdariffa fibre composite. Figure 3 shows the percentage of water absorption for Hibiscus
sabdariffa fibre composites with water immersion time. The water absorption graph for all composites demonstrates quick
water absorption in the beginning period. It happens because the surface voids and roselle fibre cellulosic structure absorb
water quickly in the beginning. With increased immersion time-period, fibres absorb more water through capillary action until
saturation occurs.33 It is a slow process. Hence, the water absorption curve flattens with time and achieves an equilibrium
condition. All composites reached water absorption saturation after 240 hours of water immersion. The maximum water
absorption for 0°, 90° and 45° fibre orientated composites are 5.4%, 9.4% and 7.7%, respectively. The neat epoxy (NE)
saturates after 24 hours by absorbing only 0.4% water, which is negligible compared to composites.

Thickness swelling behaviour. The thickness swelling is directly proportional to the water absorption of the material. Figure 4
shows the thickness swelling percentage for the composites as a function of immersion days. The maximum thickness
swelling for 0°, 90° and 45° fibre orientated composites are 7.5%, 12.4% and 8.8%, respectively. The neat epoxy (NE) reflects
no change in thickness.

Mechanical properties
Table 3 displays the mechanical characteristics of the continuous Hibiscus sabdariffa fibre composites. The composite with
longitudinal (0°) fibre orientation performs much better than the composites with transverse (90°) and inclined (45°) fibre
orientation. The longitudinal (0°) fibre orientated composite has 460% increased tensile strength, 160% increased flexural
strength and 603% increased impact strength than neat epoxy. The longitudinally (0°) oriented fibres share a significant part of
tensile, bending and impact loads resulting in excellent mechanical properties. When fibres were arranged along the transverse
(90°) direction in the composite, they took only a shearing load resulting in inferior mechanical properties. The transversely
placed fibres fail to distribute stresses among the matrix and promote the localized stress concentration.18 Hence, the failure of
a 90° fibre oriented composite occurs at a lower stress value. The stress transfer from fibre to matrix plays a significant role in
deciding the mechanical performance of the composite. The smooth and uniform stress transfer from fibre to matrix results in
excellent mechanical characteristics of the composite. As the fibre angle increases from 0° to 90°, the stress transfer from fibre
to matrix becomes less effective.32 Compared to neat epoxy, the tensile and flexural strengths of the transversely (90°) fibre
oriented composites are reduced by 4% and 34%, while impact strength is improved by 14%. The composite with inclined

Table 1. Mechanical testing details.13

Sr No Test ASTM standard Specimen size Test speed

1 Tensile test ASTM D-3039 250 mm × 25 mm × 4 mm 2 mm/min

2 Flexural test ASTM D-7264 148 mm × 13 mm × 4 mm 1 mm/min
3 Impact test ASTM D-4812 63.5 mm × 12.7 mm × 4 mm —
Kazi and DVA 5

Table 2. Density and void content of Hibiscus sabdariffa fibre composites.

Density (g/cm3)

Fibre orientation Experimental Theoretical Voids (%)

0° 1.1544 1.1711 1.43

90° 1.1435 1.1772 2.86
45° 1.1505 1.1733 1.94

Figure 3. Water absorption of Hibiscus sabdariffa fibre composites.

Figure 4. Thickness swelling of Hibiscus sabdariffa fibre composites.

Table 3. Mechanical properties of Hibiscus sabdariffa composites.

Tensile properties Flexural properties Impact properties

Tensile strength Tensile modulus Flexural strength Flexural modulus Impact strength (kJ/
Fibre orientation (MPa) (GPa) (MPa) (GPa) m2)

Neat epoxy (NE) 13.18 ± 2.35 0.208 ± 0.026 32.23 ± 4.43 1.647 ± 0.321 3.34 ± 0.24
0° 73.87 ± 5.60 (460%) 0.369 ± 0.013 (77%) 83.90 ± 8.25 (160%) 7.180 ± 0.637 (336%) 23.48 ± 2.50 (603%)
90° 12.60 ± 0.45 (4%) 0.231 ± 0.016 (11%) 21.30 ± 0.46 (34) 1.600 ± 0.144 (3%) 3.81 ± 0.23 (14%)
45° 18.20 ± 1.00 (38%) 0.286 ± 0.056 (38%) 44.60 ± 2.52 (38%) 2.720 ± 0.395 (65%) 6.89 ± 1.20 (106%)
6 Polymers and Polymer Composites 0(0)

Figure 5. Stress–strain curves for continuous Hibiscus sabdariffa composites under tensile load.

Figure 6. Stress–strain curves for continuous Hibiscus sabdariffa composites under flexural load.

(45°) fibre orientation yields intermediate results. This composite has 38% enhanced tensile strength, 38% increased flexural
strength and 106% higher impact strength than neat epoxy. The mechanical characteristics of composites diminish as the fibre
angle increases from 0° to 90°. Hassan et al.18 found similar finding in their investigation. Figures 5 and 6 demonstrate tensile
and flexural stress–strain curves for Hibiscus sabdariffa fibre composites, respectively.

Scanning electron microscopy (SEM)

Scanning electron microscopy images for tensile failed continuous Hibiscus sabdariffa fibre epoxy composites are shown
in Figure 7. Figures 7(a) and (c) display fibre pullout and crack propagation near damaged fibres, which describes non-
uniform stress transfer between fibre and matrix. Figure 7(b) shows the failure of a 90° fibre oriented composite at the
fibre–matrix interface.

Dynamic mechanical analysis

Storage modulus (E’). Storage modulus is the measure of material stiffness. Storage modulus plot consists of three zones,
namely, glassy, transition and rubbery zones. Storage modulus values are found higher in the glassy zone. The polymer chain
mobility increases with increased temperature, which causes a sudden fall in storage modulus values. This zone is known as a
transition zone. In the rubbery zone, the storage modulus value falls considerably. Figure 8(a) shows the storage modulus plot
for Hibiscus sabdariffa fibre composites. The 45° fibre oriented composite has higher storage modulus in the glassy zone that
is up to 60°C. It is due to the 45° oriented fibres bear both the normal stress and shear stress generated in the composite during
cyclic loading of DMA.16 The 0° and 90° fibre orientations yield a unidirectional reinforcing effect, resulting in reduced
Kazi and DVA 7

Figure 7. SEM images of tensile failure surface of continuous Hibiscus sabdariffa fibre epoxy composites (a) longitudinal (0°) composite, (b)
transverse (90°) composite and (c) inclined (45°) composite.

Table 4. Peak tan δ and glass transition temperature (Tg ).

Temperature (oC)

Composites with fibre orientation Peak height of Tan δ Tg from Tan δ Tg from loss modulus

Neat epoxy 0.4933 94.80 85.95

0° 0.4223 87.68 67.60
90° 0.5465 82.56 59.11
45° 0.6001 85.96 73.21

storage modulus.16 In the rubbery zone, 0° fibre oriented composite has higher storage modulus. All Hibiscus sabdariffa fibre
epoxy composites possess a higher storage modulus than the neat epoxy resin.

Loss modulus (E’’). Loss modulus is the measure of energy dissipated under cyclic load. Figure 8(b) shows the loss modulus
plot for Hibiscus sabdariffa fibre composites. Loss modulus value increases with an increase in temperature up to a particular
temperature and then decreases. The temperature corresponding to the peak loss modulus value is known as glass transition
temperature (Tg). For all the composites, the peak loss modulus values occurred at a lower temperature than neat epoxy, which
explains Hibiscus sabdariffa fibre composites have a lower glass transition temperature than neat epoxy. The possible cause for
this is the improved mobility of epoxy polymer chains at low temperatures (60°C–80°C) due to poor bonding between fibre
and matrix.13 Table 4 shows glass transition temperature value based on loss modulus for Hibiscus sabdariffa fibre composites.
Similar to the storage modulus result, composite with 45° fibre orientation possesses more loss modulus value than 0° and 90°
fibre oriented composite. Also, 45° fibre oriented composite reflects higher glass transition temperature than 0° and 90° fibre
oriented composite.

Material loss factor or Tan δ

The ratio of energy dissipated to energy stored under cyclic load is known as the material loss factor. Figure 8(c) shows the
material loss factor plot for Hibiscus sabdariffa fibre composites. The composites with 45° and 90° fibre orientation have
higher peak values of loss factor, and the composite with 0° fibre orientation has a lower peak value of loss factor than neat
epoxy. For all composites, loss factor peak values appeared at a lower temperature as compared to neat epoxy. The in-
corporation of continuous Hibiscus sabdariffa fibres in epoxy enhances epoxy polymer chains mobility resulting in reduced
glass transition temperature than neat epoxy. The peak of loss factor (tan δ) and glass transition temperature (Tg) based on loss
factor are as shown in Table 4.
8 Polymers and Polymer Composites 0(0)

Figure 8. Dynamic mechanical behaviour of continuous Hibiscus sabdariffa fibre epoxy composites (a) Storage modulus, (b) Loss modulus,
(c) Loss factor and (d) Cole–Cole plot.

Cole–Cole plot. The Cole–Cole plot exhibits structural behaviour of polymer composite like material homogeneity, the
interaction between fibre and matrix, etc. The material is said to be homogeneous when the Cole–Cole plot is pure
hemispherical. Figure 8(d) shows the Cole–Cole plot for Hibiscus sabdariffa fibre composites. The Cole–Cole curve for neat
epoxy is smooth and semi-circular which indicates homogeneity of the material. Whereas the graphs for longitudinal (0°),
transverse (90°) and inclined (45°) fibre oriented composites are rough semi-circular, indicating composites heterogeneity.

Conclusion
The influence of fibre orientation on physical, mechanical and dynamic mechanical properties of Hibiscus sabdariffa fibre
composites has been studied. From this experimental study, we arrived at the following conclusions:
• Result proves that longitudinal (0°) fibre oriented composite possesses excellent mechanical properties than other
composites. The longitudinal (0°) fibre oriented composite yields tensile strength of 73.87 MPa, flexural strength of 83.9 MPa
and impact strength of 23.48 kJ/m2.
• The longitudinal (0°) fibre oriented composite offers higher resistance to water absorption and thickness swelling
compared to other types of composites. At saturation point, the thickness of the longitudinal (0°) fibre oriented composite
increased by 7.5% after absorbing 5.4% water by weight.
• DMA result shows that all continuous Hibiscus sabdariffa fibre epoxy composites possess an improved storage modulus
than the neat epoxy resin. The longitudinal (0°) fibre oriented composite has a lower loss factor value than other composites.
• It is observed that the glass transition temperature of continuous Hibiscus sabdariffa fibre composites is 8%–31% lower
than that of neat epoxy.
• Scanning electron microscopy (SEM) images confirm the existence of voids in the matrix, fibre pullout and crack
propagation near the fibre bundle, which indicates the stress transfer between fibre and matrix is non-uniform.

Acknowledgements
Authors thank Department of Mechanical Engineering, Koneru Lakshmaiah Education Foundation, Vaddeswaram, Andhra Pradesh for
providing facilities to carry out this research. Authors also thank Central Analytical Laboratory, Department of Chemistry, BITS Pilani
Hyderabad Campus for to carry out SEM analysis. Authors also thank Plastic Testing Centre, CIPET: Institute of Plastic Technology (IPT),
Chennai for extending DMA testing facility.

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.
Kazi and DVA 9

Funding
The author(s) received no financial support for the research, authorship, and/or publication of this article.

ORCID iD
Atik Mubarak Kazi  https://orcid.org/0000-0002-8758-6600

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