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Utilization of coconut shell biomass residue to develop sustainable

biocomposites and characterize the physical, mechanical, thermal, and water
absorption properties

Article in Biomass Conversion and Biorefinery · September 2022

DOI: 10.1007/s13399-022-03293-4

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Biomass Conversion and Biorefinery
https://doi.org/10.1007/s13399-022-03293-4

ORIGINAL ARTICLE

Utilization of coconut shell biomass residue to develop sustainable

biocomposites and characterize the physical, mechanical, thermal,
and water absorption properties
Santosh Kumar1 · Abir Saha2

Received: 17 June 2022 / Revised: 23 August 2022 / Accepted: 8 September 2022

© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2022

Abstract
The reliance on natural resources has gained extra attention from researchers and scientists due to population awareness,
greenhouse depletion, and oil reserve depletion. The development of sustainable and renewable materials from biomass
residues is promising biomaterials to substitute synthetic and plastic littering. The abundant availability of coconut shell
and husk residues is having great potential for fiber/filler sources to develop biocomposites for structural and industrial
applications. In this present study, five different types of biocomposite samples (CRS-0.0, CRS-2.5, CRS-5.0, CRS-7.5, and
CRS-10.0) have been fabricated at a 30% constant weight fraction of coconut fiber with bio-epoxy matrix and varying the
coconut particles weight faction by 2.5% and characterized their structural, physical, mechanical, and thermal behavior. The
results examined that the inclusion of coconut particles improved the overall mechanical performance of the biocomposites
and observed CRC-5.0 biocomposites have superior tensile strength (32.58%), and flexural strength (35.45%), and surface
hardness (23.61%) compared to CRC-0.0 biocomposites. The impact strength, fracture toughness, and fracture energy are
higher for CRC-2.5 biocomposites. CRC-5.0 biocomposites analyzed better thermal stability with a maximum degradation
temperature of 358 °C and 24% char residue of coconut biomass at 800 °C. The surface morphology has been also analyzed
to examine the fracture/failure behavior of biocomposites. Finally, the samples have been submerged in water, NaOH, and
NaCl solution to examine the water uptake and corrosion behavior of developed biocomposites. Therefore, the development
of bio-based product by utilizing agro/food waste has great potential and has the capabilities to replace conventional materi-
als for various industrial applications.

Keywords Biomass · Biocomposites · Natural fiber · Hybrid composite · Sustainable material

1 Introduction petroleum-based materials that decompose or degrade to

The advanced polymeric-based materials have replaced
the traditional glass, metals, and iron-based materials for
engineering applications due to abundant availability, low
cost, and easy processing. Conventional plastics and plastic
composites are the major sources of waste, environmen-
tal pollution, and greenhouse emissions [1]. The emer-
gence of biopolymers has a great potential to replace the
* Abir Saha
abir2016saha@gmail.com
1
Department of Mechanical Engineering, National Institute
of Technology Silchar, Silchar, Assam, India
2
Department of Mechanical Engineering, Indian Institute
of Technology Guwahati, Guwahati, Assam, India
save the environment. Therefore, researchers and scientists
are shifting their interest towards sustainable and biodegrad-
able materials to overcome the environmental effects and
improve the feasibility of waste residue [2–4]. Synthetic fib-
ers (carbon, glass, kevlar etc.) also known as artificial fibers
have been extensively reinforced with polymeric materials
to develop composite for various engineering applications.
But generations of high energy during processing, costly,
lesser availability, non-renewability, non-recyclability, and
non-biodegradability have limited their use and gained more
intention towards natural fiber/filler-based biocomposite [5].
The extraction of lignocellulosic natural fibers from vegetal
plants and agricultural and food residues not only is econom-
ical solutions but also increases the environmental impact,
renewability, and sustainability [6–8]. The usages of these
wastages as fibers/fillers are impending over-dependency

13
Vol.:(0123456789)

and consumption on forest wood/plants reserves and syn-
thetic fibers to more ecological vegetal natural fiber alterna-
tives that have a low footprint of carbon with cheaply abun-
dant, non-toxic, recyclable, and biodegradable [9].
The development of biocomposites from waste biomass
resources and residues has played a major role in growing
environmental awareness and helped to make an ecologi-
cal balance between agriculture and industry [10–12]. After
consumption of coconut and pineapple fruits, the generation
of waste residues is highest among other agro/food wastes.
So, these residues can be more effective to develop biocom-
posites that boost the rural economy and also reduce global
warming pollution [13, 14]. Coconuts are the green energy
source to produce health drinks, fruits, animal feeds, heat,
fuel additives, electricity, fiberboards, and organic fertilizer
for an eco-friendly environment and cleaner emissions. It is
produced in 92 countries worldwide and is mostly cultivated
in Indonesia, the Philippines, and India. India is the second-
largest country to produce coconut after Indonesia. Accord-
ing to the Organization of Food and Agriculture department,
Fig. 1  Coconut plant biomass with auxiliary parts and extraction of coconut fibers/fillers from coconut residues
13
Biomass Conversion and Biorefinery
India produced around 11,706,343 tons of coconut in 2018
mainly cultivated in the southern part of India. Coconut con-
tains 40% fruits with the remaining shell, husk, and dust that
are called agricultural wastes. The coconut husk and shell
comprise 30% of fibers and 70% of dust, flesh and piths.
Figure 1a illustrates the coconut plant morphology with their
auxiliary parts. The coconut biomass is abundantly avail-
able in the form of coconut shells and coconut husks. After
harvesting and collection of fruits from coconuts, the shell
and husk are disposed of in the open areas which makes it
difficult to arrange the management of these residues. There-
fore, these residues are usually burnt or simply thrown away
which produces carbon and methane emissions and is haz-
ardous to human health and the environment [14–16].
Coconut shells and husk are solid fuels and are widely
used for producing charcoal using the pit method. The dry
weight of coconut shells and husks contains a charcoal yield
of 25–30% that is often contaminated and polluted with
extraneous soil and matter. The smoke produced during pit
methods is not only a nuisance but also a health hazard to
Biomass Conversion and Biorefinery
the environment [16, 17]. Therefore, the usage of these coco-
nut biomass residues will not only improve the sustainable
environment but also contribute to economic growth for the
development of healthy populations [14, 18]. The chemical
composition of coconut husks and shells consists of high
cellulose and lignin, contains potassium, pyro-ligneous acid,
tar, gas, charcoal, and tannin and has high calorific values
of 21–18 MJ/kg. Thus, the use of these coconut residues as
fiber reinforcements can be transformed into a value-added
material that has very much resistant to water, bacteria, and
fungi as well as have great potential to replace wood and
other traditional materials for various domestic and indus-
trial applications [19, 20].
The coconut fibers extracted from the mesocarp of coco-
nut fruits have the highest lignin contents 26–30% with
58–60% cellulose [21]. The presence of lignocellulosic
inside the fibers is characterized by high lignin contents;
distinct these fibers have harder than other natural fibers that
have less sensitivity to water/moisture and are unaffected by
dampness [22, 23]. In addition, coconut fibers have produced
interesting light-weight products with bulk density, resist-
ance to rot and fungi, mothproof, lowest thermal conductiv-
ity, excellent UV resistance and insulation against sound and
temperature that increased the toughness, resilient, thermal
stability, and mechanical performance of the final developed
biocomposites [24]. Numerous studies were conducted on
coir/coconut fibers and fillers reinforced composites to
examine their physical, structural, thermal, and mechanical
properties. The inclusion of micro/nano organic and inor-
ganic fillers/particles/concrete at different weight fractions
with fibers improved the thermo-mechanical characteristics,
dimension stability, and interfacial interactions with perfect
insulation and rigidity of developed hybrid biocomposites
[25–29]. The particle size and weight fraction of fillers also
influenced the performance of the composites and few stud-
ies concluded that the finer particles size up to 75 µm at
5.0–7.5% filler loading enhanced their thermo-mechanical
performance while decrement in their respective properties
was analyzed with further improvement of particle size and
loading [30–32]. However, most of the natural fibers have
some major limitations such as hydrophilic nature, the pres-
ence of carboxyl and hydroxyl groups in the structure that
results in intrinsic polarity, poor wettability, low moisture
resistance, and weaker adhesion between reinforcement
and matrix as well as reducing the physical, mechanical,
and dynamic mechanical properties of composites and also
affects the scope for their use in load-bearing and engineer-
ing structural applications [33–35]. To overcome these limi-
tations, the structure and surface of the fibers/fillers were
modified with surface modification, chemical treatments,
and hybridization to enhance the interfacial bonding, sur-
face energy, roughness, compactness, and stress interaction
between reinforcement and matrix [36–38]. Many research
studies also reported that the treatment and surface modifica-
tion of fibers and fillers improved the physical, mechanical,
thermal, fracture, damping, and structural properties of the
developed hybrid composites [39–41].
From previous studies, it concluded that extracted coco-
nut/coir fibers and filler are extensively used as reinforce-
ment to develop composite for structural and engineering
applications. The chemical treatment and surface modifi-
cation of these fibers and fillers have to be done more for
enhancing their interfacial bonding and overall perfor-
mances. Although, the inclusions of treated/modified organic
fillers at different weight fractions and particle sizes are yet
to be explored as well as no study has been reported on the
inclusion of coconut particles with coconut fiber. Therefore,
the present study is focused on the development of sustaina-
ble and biodegradable biocomposites from extracted vegetal
fibers and fillers (coconut mesocarp, piths, and shells) with
bio-epoxy matrix and investigates the chemical, physical,
mechanical, thermal, corrosion, and water uptake behavior
of the developed biocomposites.
2 Materials and methods
The bio-epoxy resin has been used as matrix materials that
are derived from natural phenolic materials obtained by dis-
tilling Cashew nutshell liquids (CNSL). The resins are sup-
plied by Cardolite India Pvt. Ltd. Mangalore, India and are
recognized as FormuLITE series with 44% of bio content. It
contains low density (1.082 gm/cm3) and viscosity (905 cPs)
with high glass transition temperature (> 95 °C), and flash
point (> 150 °C). It provided excellent bonding and wetting
properties and cured at room temperature. FormuLITE poly-
mer is encompassed of modified thermoset epoxy (2501A)
and amine hardener (2401B) that are mixed properly in the
ratio of 10:3 for use as matrix material in the development
of bio-composites. Coir fibers have been extracted from the
coconut layer called husks and shells. The botanical name
of the fiber is Cocos nucifera which belongs to the palm
family called “Arecaceae.” The extracted fibers and particles
from coconut shells and husks have been used as reinforcing
materials for the development of sustainable biocomposites.
2.1 Extraction process of coconut fiber and particles
The coconut husks collected from local resources and fibers
have been separated manually. The extraction process of fib-
ers and particles is described in Fig. 1b. The collected husks
have been soaked in brackish/lagoons waters for 5–6 days.
After submerged, the anaerobic fermentation process takes
place inside the husks causing them to soften and finally
separate. Now, separated fibers are washed with distilled
water and dried in an open atmosphere for 24 h to remove
13

the wax, ash, and impurities from the surfaces. The coconut
fruit shells and residual piths have been used for prepar-
ing microparticles (filler). The piths and shells have been
crushed and then grind with the ball milling process and
sieved. Now, the obtained fine particles are washed with dis-
tilled water to remove impurities then dried at atmospheric
temperature for 24 h and finally dried in an oven at 60 °C for
6 h [33]. The prepared fine particles are named as untreated
coconut particles.
2.2 Surface modification of extracted coconut fiber
and particles
The chemical treatment has been done to modify the surface
of the fibers/particles and improve the bonding mechanism
of the surface [36]. The alkaline treatment process has been
used for surface modification of coconut fibers/particles and
is explained in Fig. 2a. The 5 g of sodium hydroxide (NaOH)
pellets has been dissolved with 100 ml of distilled water in
the beaker and prepared in the aqueous solution. The solu-
tion is mixed properly with the help of a magnetic stirrer
at 750 rpm for 15 min and then adding 15 g of coconut
particles into the solution and stirred the solution again at
48 °C at 850 rpm for 8 h. Now, the particle solution has been
washed by using distilled water and acetone to reduce the pH
value of up to 7 of the particles. Finally, obtained particles
are dried in an open atmosphere for 24 h and then dried in
the oven at 60 °C for 12 h [30]. The obtained particles are
named as treated coconut particles and these treated particles
Fig. 2  Treatment of coconut
fiber, micro-particles, and
fabrication process of
biocomposite plates
13
Biomass Conversion and Biorefinery
have been used for preparing the biocomposite samples with
coconut fiber reinforcements.
2.3 Fabrication process of biocomposites
The manual compression hand layup method has been used
to develop the biocomposite samples. The fabrication pro-
cess of biocomposites is described in Fig. 2b. First, bio-
epoxy resin (2501A) is taken in the glass at an appropri-
ate weight and treated coir particles are added at different
weight fractions (2.5%, 5.0%, 7.5%, and 10.0%). The mix-
ture is mixed properly with mechanical stirring for 10 min
and then sonication has been done to trap air and homogene-
ous mixture. Now, amine hardener is added to the mixture
as per standard ratio with bio-epoxy resin (10:3) and mixed
properly by the mechanical mixing process. The degassing
of the final solution has been done to detect the air bub-
bles from the mixture. Now, the collected coconut fibers
are spread at a constant weight of 30% over the lower mold
and the mixture of the final solution has been poured into
the fiber. The roller and brush are used to coat the matrix
properly on the fibers layer and it also detected the void
during preparations inside the samples. Finally, the upper
mold has been kept upon the prepared samples and applied
an external load of 50 kg for equal distribution of matrix
materials inside fiber reinforcements. The prepared samples
are cured at room temperature within 24 h and then removed
from the mold and kept inside the oven for the pre-curing
Biomass Conversion and Biorefinery
and post-curing process. The prepared samples are cut as per
ASTM standards for experimental testing.
The various experimental results reported that the inclu-
sion of fibers at 30% by weight recorded maximum mechani-
cal and dynamic mechanical properties [30, 42, 43]. Thus,
for this study, five different types of samples (CRS-0.0,
CRS-2.5, CRS-5.0, CRS-7.5, and CRS-10.0) have been
prepared at a constant weight of coconut fiber (30%) and
varying the coconut particles percentages (2.5%, 5.0%, 7.5%,
and 10.0%).
2.4 Characterization of coconut particles
The physical, thermal, and structural characterization of
prepared coir particles has been analyzed using scanning
electron microscopy (SEM), X-ray diffraction (XRD),
Fourier transform infrared radiation (FTIR), and thermo-
gravimetric analyzer (TGA) and single fiber tensile testing.
These processes helped to analyze the effects of chemical
treatments on molecular bonding, thermal stability, phase
transformation, surface modification, and interfacial struc-
ture of untreated coir particles.
The particle size distribution of treated reinforcing fiber
has been characterized by using a scanning electron micro-
scope and size distribution has been carried out by using
ImageJ software. Crystalline index and crystalline size of
the treated and untreated coir particles have been charac-
terized by performing X-ray crystallography. XRD analysis
has been carried out by using a Brucker D8 focus machine
operated at 30 kV/15 mA. The effect of surface modifica-
tion on functional groups of reinforcing materials has been
also characterized by performing Fourier transform infra-
red. The test has been performed by using a PerkinElmer
FTIR spectroscopy machine in a transmittance range of
400–4000 ­cm−1. The effect of chemical treatment on the
thermal stability of the reinforcement has been analyzed by
performing thermogravimetric analysis with an EXSTAR
TGA/DTA-6300 machine under an ­N2 gas environment with
a gas flow rate of 200 ml/min and heating rate of 10 °C/min.
The weight loss with respect to elevated temperature has
been recorded for treated and untreated coir. Single fiber
tensile testing has been carried out by using a ZwickRoell,
Model: Z005TNProline tensile testing machine with a 5KN
load cell. The 25 fiber samples for treated and untreated coir
fiber have been tested and statistical analysis of the test result
has been carried out by using Minitab software [44].
2.5 Characterization of biocomposite
The physical behavior of developed biocomposites has
been performed to find the experimental density, void con-
tents, and water uptake behavior. The thermo-mechanical
experimental testing has been done to examine the strength,
stiffness, hardness, toughness, and thermal degradation
behavior of developed biocomposite samples. The detailed
process of characterization with experimental testing of
developed biocomposites is described in Table 1.
3 Result and discussion
3.1 Characterization of coconut fiber/filler
The two major factors that influenced the thermo-mechani-
cal properties of developed composites are particle size and
morphology of the reinforcing material. The morphology of
the treated coconut particles has been observed under a scan-
ning electron microscope (SEM). Figure 3a is representing
the image of the morphology. With naturally derived bio-
fillers, there is a problem of poor interfacial interaction with
the matrix. The chemical treatment possibly increased the
interfacial interaction by roughening the surface of the bio-
filler. To identify the size distribution of prepared particles,
the obtained SEM image has been imported into ImageJ
software and the size of the particles has been measured.
Figure 3b represents the particle size distribution and normal
distribution curve of treated coconut particles. The average
size of particles has been observed as 27.750 μm with a
standard deviation of 15.145 and a median value of 25 μm.
The maximum and minimum values of particle size have
been observed as 65.45 μm and 5.85 μm respectively.
3.2 Physical characterization of coconut particles
The X-ray diffractometer (XRD) has been used to examine
the effects of alkaline treatments on the crystalline prop-
erties of extracted coconut particles. The XRD pattern
of treated and untreated coconut particles is presented in
Fig. 3c. From the XRD pattern, four major peaks have been
observed for both treated and untreated particles. The peaks
are at 2ϴ = 15.8, 16.1, 22.3, and 35.8 corresponding to the
crystalline plane of (1 1 0), (1 1 0), (2 0 0), and (0 0 4)
respectively [30, 44]. These peaks are due to the presence of
cellulose inside coconut residues biomass at the β phase. The
untreated particles showed a crystalline index of 51.08%,
whereas the treated particles showed a crystalline index of
63.45%. The surface modification with alkaline treatment
also increased the crystalline size of the particles from 3.42
to 3.86 nm.
The effects of alkalization on functional groups of coco-
nut particles have been observed using FTIR spectra. Fig-
ure 3d represents the FTIR spectrum of treated and untreated
coconut particles. The major peak information regarding
treated and untreated particles is tabulated in Table 2 and
observed that after chemical treatment, the peak shifted at
3433, 3286, 2893, 1655, 1559, 1504, 1416, 1306, and 1267.
13
 Biomass Conversion and Biorefinery

Table 1  Process of characterization and testing of developed biocomposites

Tests conducted Measured properties Machine used/procedure ASTM standards

Density Experimental and theoretical density Archimedes’ principle has been used to identify ASTM-D 792–20 [45]
the experimental density of the biocomposites
with help of a weighing balance machine and
theoretical density has been found by using the
rule of mixture
Void content Void inside composite The difference in theoretical and experimental ASTM-D 2734–70 [46]
density is sported as void content of composites
Water absorption Water uptake behavior Samples have been weighed before and after ASTM-D 570–98 [47]
being submerged in water using a digital
weighing machine at regular intervals of time
Tensile test Tensile strength, tensile modulus, tensile strain The test has been performed on a 50kN universal ASTM-D 638–03 [48]
testing machine (UTM) at room temperature
with a gauge length of 50 mm and a testing
speed of 1 mm/min
Flexural test Flexural strength, flexural modulus, The test has been conducted on 50kN UTM at ASTM-D 790–03 [49]
and extension room temperature with a span length of 40 mm
and a testing speed of 1 mm/min
Hardness Surface hardness Surface hardness of biocomposites has been ASTM-D 2240–15 [50]
conducted on five different places of the
samples using Shore D-hardness tester
and reported the average values
Impact test Impact energy/strength The impact strength has been obtained using ASTM-D 256–06 [51]
the Roell pendulum tester where the samples
are fixed on the pendulum fixture to prevent
deformation
Fracture test Fracture toughness and fracture energy The plane strain fracture analysis has been done ASTM D5045-14 [52]
using UTM with a cross speed of 10 mm/min
Corrosion test Electrochemical behavior Characterized with help of poteniostatgalvanostat [36]
with an electrochemical impedance of NaOH
and NaCl salt solution at a frequency range of
0.01–100 Hz with 10 mV
TGA​ Thermal degradation of composite The mass degradation of developed composite [30]
with elevated temperature has been carried out
by performing thermogravimetric analysis
SEM Surface morphology Morphology of the fracture surface has been iden- [37]
tified and analyzed by using a screening electron
microscope

Most of these peaks belong to any function group vibration
present in lignin and hemicelluloses. Hence, FTIR confirmed
the delignification from extracted coconut particle residues.
The thermo-gravimetric analysis (TGA) has been per-
formed to analyze the effects of alkalization on thermal
stability and thermal degradation of coconut particles. Fig-
ure 3e represents the thermogram for treated and untreated
coconut particles. The thermal stability of the particles
has been examined in terms of weight loss at four differ-
ent stages under influence of temperature. The degradation
temperature details of untreated and treated particles are
tabulated in Table 3. The first stage of weight loss has been
sported between 25 and 150 °C corresponding to a weight
loss of moister present in the coconut particles. After that,
the second stage of weight loss has been spotted between the
temperature range of 151 °C to 250 °C due to the evapora-
tion of extractive, wax, and other impurities. Later on, the
temperature range of 251 to 380 °C is corresponding to the
weight loss of particles due to cellulose degradation, and the
fourth stage of weight loss is corresponding to a temperature
range of 381 to 600 °C. In this stage, major lignin and high
crystalline cellulose have been degraded. Due to the alkaline
treatment of extracted coconut particles, the cellulose-I has
been converted to a more thermally stable and higher crys-
talline structure, named as cellulose-II [44, 57, 58]. Due to
this, treated particles showed higher thermal stability and
lesser weight loss with elevated temperatures.
The effect of chemical treatment on tensile properties of
extracted coconut fibers has been examined by performing
single fiber tensile testing. Twenty-five numbers of fibers have

13
Biomass Conversion and Biorefinery

Fig. 3  a SEM image of coconut

particles; b particle size distri-
bution of coconut particles; c
XRD pattern; d FTIR spectra;
e TGA thermogram for treated
and untreated coconut fiber/
filler; f tensile stress–strain
graph for treated and untreated
coconut fiber

been selected from treated and untreated coconut fiber and
performed the testing. Figure 3f represents the stress–strain
curve of coconut fibers. From the stress–strain curve, it was
observed that like other natural fibers, coconut also showed
a quasi-linear increment of stress–strain and when stress
reached its maximum, sudden rapture has been observed.
This type of failure is attributed to the brittle failure of natural
fiber [44, 54, 58]. Due to higher deviation in the tested results,
the statistical analysis has been performed using the Weibull
distribution function and Minitab software. The Weibull dis-
tribution for tensile strength and tensile modulus of coconut
fibers is presented in Fig. 4. The statistical parameters of the
estimation have also been added to the graphs. The estima-
tion has been done with the machine learning approach avail-
able in Minitab software. The tensile strength of untreated
coconut fiber has been reported as 420.645 ± 21.497 MPa
and tensile module of 33.11 ± 3.97GPa. After the chemical
treatment of fibers, the tensile strength has been increased to
530.514 ± 22.5122 MPa and the modulus has been increased
to 42.03 ± 5.86GPa. The increments in tensile strength and
tensile modulus are attributed to the increment in the crystal-
line index of lignocelluloses biomass fibers [44, 59]. A quan-
titative indicator of crystallinity is the crystallinity index (CI).
Crystallinity is a measurement of the degree of structural
order of the molecules in a polymer. An increase in crystal-
linity indicates that the atoms or molecules inside materials
are arranged in a more regular and periodic pattern [30, 36].
The chemical treatment resulted in the molecular rearrange-
ment of lignocellulose. Due to rearrangement, their molecu-
lar arrangements become more regular; this helps transmit
the load from one atom to another atom, resulting in

13
 Biomass Conversion and Biorefinery

Table 2  Assignment of transmittance spectrum bands of coconut particles

Wave number ­(cm−1) Assignment References Untreated Treated

3433; 3286 Stretching vibration due to the presence of a hydroxyl group in lignin and cellulose I­ β [36] P P (small)
2969 Stretching of C-H in methylene (= ­CH2) group present in cellulose [30] P P
2893 Stretching vibration of C–H bond presents in lignin [44] P A
1732 Stretch of the carbonyl group (-C = O) [44] P P
1655 Due to present of moister molecule [36] P A
1559 Skeletal vibration of aromatic ring present in lignin [36] P A
1504 Lignin aromatic ring stretching [53] P A
1416 Due to present of lignin [53] P A
1371 Stretching vibration of C–H and O–H group present in methyl and phenol [44] P P
1306 Ring breathing with C–O stretching in lignin [36] P A
1267 C–O stretching of acetyl group in hemicellulose [36] P A
1167 C–H stretching of the vibrations of different groups in the carbohydrates [44] P P
1137 Anti-symmetrical deformation of the C–O–C band [54] P P
1087 Functional group present in Cellulose and hemicellulose [55] P P
1057 C–O stretching of cellulose [54] P P
987 C = O stretching of carboxyl group [56] P P
891 C–H vibrations of cellulose [55] P P
664 The -COOH bending band [54] P P
641 Bending vibration of O–H (outer plane) [56] P P
511, 483 p-Hydroxyphenyl of propane [55] P P

P, presence of FTIR peak; A, absence of FTIR peak

Table 3  Degradation temperature of developed biocomposites
Biomass type IDT (°C) MRDT (°C) T50 (°C) Final residue (%)
Untreated 68.1 331.2 336.5 26.13
Treated 74.6 354.7 358.9 22.71
IDT, initial degradation temperature; MRDT, maximum rate degrada-
tion temperature; T50, temperature of 50% degradation
greater strength and Young’s modulus one lignocellulose
biomass.
3.3 Physical characterization of biocomposite
The density and void content of developed biocomposite
have been examined. The theoretical and experimental den-
sity of the developed biocomposites has been investigated
and is tabulated in Table 4. The theoretical density has been
found by using the rule of mixture formulation as formulated
in Eq. (1).
𝜌c(theo)= (𝜌f × vf ) + (𝜌p × vp ) + (𝜌m × vm )
where 𝜌c(theo) stands for theoretical density and 𝜌f ; 𝜌p
and 𝜌m stand for density of fiber, coir particles, and bio
epoxy matrix, respectively, andvf ; vp and vm stands for the
volume fraction of coir fiber, coir particles, and bio epoxy
respectively.
The void content (VC ) has been calculated by using
Eq. (2).
𝜌c(theo) − 𝜌c(exp)
VC =
𝜌c(theo)
× 100 (2)
where 𝜌c(theo) and 𝜌c(exp) stand for theoretical and experimen-
tal density of biocomposites.
It was observed that increasing the addition of coconut
particles leads to a continuous decrement in the overall den-
sity of hybrid biocomposite. This may be due to the less den-
sity of coconut particles compared to the bio-epoxy matrix.
The maximum experimental density has been reported for
CRC-0.0 biocomposite (1.089gm/cm3) and minimum exper-
imental density for CRC-10.0 biocomposite (0.954gm/cm3).
A difference has been observed between the theoretical and
experimental density of the developed biocomposite and
this difference is reflected as the void content of developed
biocomposites [30].
The void inside the material is one of the critical issues.
(1) Consequently, these voids act as crack nucleation points and
result in the decrements of performance of developed bio-
composites. An inversely proportional relationship has been
observed between void content and weight fraction of coco-
nut particles in developed biocomposites. The maximum

13
Biomass Conversion and Biorefinery

Fig. 4  Weibull distribution for a

tensile stress; b tensile modulus
for untreated coconut fiber;
Weibull distribution for c tensile
stress and d tensile modulus of
treated coconut fiber

Table 4  Density and void contents of developed biocomposites break of developed biocomposites are presented in Fig. 5b.
Composites Theoretical Experimental Void (%)
The addition of coconut particles up to 7.5% weight frac-
density (gm/cm3) density (gm/cm3) tion improved tensile strength and tensile modulus compared
to CRC-0.0 biocomposites. This is because the addition of
CRC-0.0 1.139 1.089 4.421 particles into fiber-reinforced composites has resulted in
CRC-2.5 1.102 1.064 3.427 an increment in the crystalline index in polymeric biocom-
CRC-5.0 1.067 1.035 3.012
posite and shows a directly proportional relation with coir
CRC-7.5 1.034 0.999 3.364
weight fraction [36]. The maximum tensile strength has been
CRC-10.0 1.003 0.959 4.366
observed with CRC-5.0 biocomposite (142.46 ± 6.228Mpa)
which is 32.58% higher than CRC-0.0 biocomposite. The
maximum tensile modulus has been examined with CRC-
void content has been observed for CRC-0.0 biocomposite 7.5 biocomposites (5.366 ± 0.222GPa) and 23.61% higher
and minimum void content has been reported for CRC-5.0 than CRC-0.0 biocomposite. Further increment in particle
biocomposite. The addition of coconut particles enhanced reinforcement percentage (CRC-10) resulted in a decrement
the interfacial bonding between fibers, fillers, and matrix, in tensile strength and modulus due to agglomeration and
thus reducing the void contents. But CRC-10.0 biocompos- inefficient bonding between reinforcement with the bio-
ites have recorded higher void % due to agglomeration and epoxy matrix [30, 33, 36]. The addition of particles of more
cauterization of particles at a higher % of filler loading with than 2.5% by weight made the biocomposite more brittle
the matrix [30, 36, 37]. that results in the decrement of elongation before the break
(strain). The maximum elongation before the break has been
3.4 Mechanical properties of biocomposites reported as 3.11% with CRC-2.5 biocomposites.
The three-point bending test has been used to determine
In order to determine the strength and stiffness of developed the flexural properties of the developed biocomposites.
biocomposites, a tensile test has been conducted. Figure 5a Figure 5c represents the flexural stress–strain curves of the
represents the tensile stress–strain curve of developed bio- developed biocomposites and showed linear behavior up to
composites. The stress–strain curved showed linear behavior failure with level buckling and without plastic deformations.
up to failure without any plastic deformation. The tensile Unlike the tensile strength and tensile modulus, the flex-
properties such as strength, modulus, and elongation at the ural strength and flexural modulus also correlate directly

13

Fig. 5  a Tensile stress–strain
curve of developed biocom-
posites, b variation of tensile
properties with coconut filler
weight percentage; c flexural
stress–strain curve; d varia-
tion of flexural properties with
coconut filler weight percentage
in biocomposite
with coconut particles. Figure 5d represents the flexural
strength and flexural modulus of developed biocompos-
ites under influence of coconut particles. The maximum
flexural strength has been reported for CRC-5.0 biocom-
posites (151.451 ± 7.45 MPa), whereas maximum flexural
modulus has been observed for CRC-7.5 biocomposites
(7.451 ± 0.54GPa). The addition of coconut particles along
with fiber increased the interfacial interaction between rein-
forcing materials and bio-epoxy matrix which resulted in
better stress transfer, and increment in strength and modu-
lus has been analyzed. The excessive addition of particles
(10%) formed a cluster between particles and bio-epoxy that
agglomerated and increased the stress concentration factor
in the developed biocomposites; thus, decrements in flexural
properties have been observed.
The ability of a material to absorb shock and energy is
known as the impact strength/energy of that material [36].
The Charpy impact test has been conducted to determine
the impact strength of the developed biocomposite and is
presented in Fig. 6a. The maximum impact strength has been
reported for CRC-2.5 biocomposites (88.41 ± 6.45 J/m) and
this value is 17.22% greater than CRC-0.0 biocomposites.
The result concluded that the impact strength may be cor-
related with elongation before the break of tensile testing. At
the low weight fraction of particles, better matrix-reinforce-
ment wettability has been observed; thus, stress has been
transmitted efficiently and resulted in higher toughness as
well as impact strength. While further addition of coconut
particles improved the brittleness of the biocomposites and
resulted in lower impact strength of the developed biocom-
posites [30].
13
Biomass Conversion and Biorefinery
Hardness is the resistance to localized plastic deforma-
tion of the material. The surface hardness of the devel-
oped biocomposites has been analyzed and is presented
in Fig. 6a. The addition of coconut particles (up to 5% by
weight) increased the resistance of localized plastic defor-
mation of developed biocomposites due to greater interfa-
cial bonding of fiber, particles, and bio-epoxy matrix. The
maximum hardness value has been observed for CRC-5.0
biocomposites (96.95) and is 23.61% higher than CRC-0.0
biocomposites. By adding micro-coconut particles in coco-
nut fiber–reinforced bio-epoxy biocomposite, indentation
resistance increased enhancing the Shore-D hardness value.
But in the case of CRC-7.5 and CRC-10.0 biocomposites,
excessive particle loading reduces the hardness value due to
a reduction in the binding strength of the matrix and rein-
forcing materials [30].
To understand the effect of particle addition on frac-
tural behavior of developed biocomposite, the fracture
toughness and fracture energy have been investigated and
are presented in Fig. 6b. The cross-linked structure of bio-
epoxy behaves brittle in nature which sustains low fracture
toughness. Thus, the addition of coconut fiber enhanced the
fracture toughness and fracture energy of the developed bio-
composite due to better stress transfer between fibers and
matrix. The analysis of the result showed that the addition
of coconut particles at a low weight percentage (up to 2.5%
by weight) improved the fracture properties. The maximum
fracture toughness (6.63 ± 0.44 MPa m ­ 0.5), and fracture
2
energy (1289.42 ± 8.452 J/mm ) have been observed for
CRC-2.5 biocomposite. These values are 18.6% and 6.4%
higher than CRC-0.0 biocomposites. This is because at lower
Biomass Conversion and Biorefinery
Fig. 6  a Impact and hard-
ness; b fracture toughness and
fracture energy; c corrosion; d
moister absorption; e thermal
degradation and f derivative
weight properties of developed
biocomposites
particle loading, crack front propagation may be interrupted
and there is a possibility that micro-particles of coconut
inside developed biocomposite may create obstacles at the
crack front, causing the crack front to bow. Thus, greater
interfacial interactions have been analyzed that resulted in
higher values of fracture toughness and fracture energy.
Further increments of coconut particles have declined the
fracture toughness and fracture energy values because, at
higher loading of particles, brittle behavior of biocomposites
increased that also increased the stress concentration spots
inside developed biocomposites and reduced their fracture
behavior [30, 36, 37].
3.5 Corrosion behavior of biocomposites
The corrosion test and water absorption test have been per-
formed to analyze the electrochemical and water uptake
behavior of the developed biocomposite. For the corrosion
test, the biocomposite samples have been soaked in 3.5%
NaCl and NaOH aqueous solution for 36 h. Figure 6c shows
the corrosion behavior of the developed biocomposites. The
CRC-0.0 biocomposite has been showing the least corro-
sion rate, and the addition of coconut particles increased the
corrosion rate of biocomposites. The maximum corrosion
rate has been reported for CRC-10 biocomposites, with a
corrosion value of 0.00594 mm/year in NaOH solution and
0.00598 mm/year in NaCl solution. In structural mechanics,
corrosion is one of the most important failure criteria. As a
result of the high corrosion rate, the stress concentration fac-
tor of the material increased, thereby reducing the strength
of the structure. Due to this, people are thinking optimistic
to use polymeric materials for industrial and structural prod-
ucts that resist lower corrosion resistance compared to the
metallic product [36].
3.6 Moister absorption behavior of biocomposites
Figure 6d shows the water absorption behavior of the devel-
oped biocomposites. The results analyzed that as the num-
ber of immersion days increased, the percentage of water
absorption also increased and eventually reached satura-
tion after 33 days. The CRC-0.0 biocomposite exhibited
13

the lowest water absorption behavior and the addition of
coconut particles increased the water absorption behavior
of biocomposites. This may be due to the hydrophilic nature
of the natural fiber/fillers. The maximum water absorption
has been observed for CRC-10.0 biocomposite due to higher
coconut particle content and inefficient interfacial bonding
between matrix and reinforcement. Due to agglomeration
and inefficient bonding between reinforcements and matrix,
micro-level gaps have been created that act as capillary
action and caused higher water absorption [33, 44].
3.7 Thermal stability and degradation
of biocomposites
The thermo-gravimetric analysis (TGA) has been performed
to determine the thermal stability and thermal degradation
of the developed biocomposite. CRC-0.0 is the base material
and CRC-5.0 showed higher mechanical properties, so the
TGA has been performed on CRC-0.0 and CRC-5.0 biocom-
posites and compared the results. Figure 6e represents the
mass loss of biocomposites at elevated temperatures, and
Fig. 6f represents the DTG graph of biocomposites.
The analysis has been done at four stages of weight loss
and is tabulated in Table 5. The addition of particulates
along with coconut fiber affected positively the thermal
stability of biocomposites. The CRC-5.0 biocomposites
showed lower weight loss at every stage and higher residual
at 800 °C. It is due to the blocking of heat passage that
delayed weight loss. From the DTG graph, it is observed
that MRDT has also been shifted from 336.76 to 350.47 °C.
This increment is also evidence that overall thermal stability
has been increased by adding coconut particles with coconut
fiber–reinforced biocomposites.
3.8 Surface morphology of biocomposites
The distribution of coconut particles and fracture morphol-
ogy of developed hybrid biocomposite have been analyzed
by field emission scanning electron microscopy (FESEM).
The analysis has been focused to determine the surface
morphology with distribution and scattering behavior of
coconut particles in developed hybrid biocomposites as
shown in Fig. 7. The neat bio-epoxy samples showed a
brittle catastrophic fracture without plastic deformation
as shown in Fig. 7a. Figure 7b shows the morphology of
Table 5  Residual mass loss at Composites Stage-I
four different stages weight loss
(%)
CRC-0.0 8.30
CRC-5.0 6.22
13
Biomass Conversion and Biorefinery
CRC-0.0 biocomposites where the failure happened due to
fiber pull-out, breakage, and debonding with a matrix that
results in weaker interfacial bonding between fiber and bio-
epoxy. Figure 7c–e shows better interfacial bonding with
greater compactness with 2.5–7.5% of particle distribution
in developed hybrid biocomposites. Therefore, the high-
est thermo-mechanical properties and stability have been
analyzed with CRC-5.0 followed by CRC-7.5 and CRC-2.5
biocomposites respectively. Further inclusion of coconut
particles (10%) analyzed agglomeration and cauterization
of particles with a matrix that results in cavitations, more
voids, and poor interfacial bond between reinforcements and
matrix phase [36, 39]. Therefore, the performance of the
developed biocomposites has been reduced for CRC-10.0
biocomposites. All developed biocomposites analyzed brit-
tle fracture without plastic deformation of fibers with linear
behavior of stress where the failures are mainly revealed
due to breakage, pull-out, crushing, debonding, and level
buckling of coconut fibers [26, 29]. However, shear yielding
and agglomeration of particles with bio-epoxy also affect the
performance and sudden failure of developed biocomposites
has been examined [30, 36].
4 Comparative study
Nowadays, the development of naturally derived biocom-
posites has been used extensively for various industrial and
engineering applications due to their abundant availability,
lighter weight, lower cost, renewable, compatible, and eco-
friendly. These types of composites are not only economical
solutions but also more versatile and practical solutions to
reduce petroleum-based products with cost-effective bio-
products. Table 6 tabulates the comparative study of natu-
rally derived biocomposites based on their mechanical and
physical properties.
5 Conclusion
The hybrid biocomposites have been developed by reinforc-
ing the coconut fiber and coconut particles with bio-epoxy
matrix using the compression molding method. First, the
extracted bio-fiber/bio-filler has been characterized chemi-
cally and physically and then developed five different types
Stage-II Stage-III Stage-IV MRDT (°C) Final residual (%)
weight loss weight loss weight loss
(%) (%) (%)
2.94 60.67 30.57 336.76 20.73
1.16 59.57 25.46 350.47 24.61
Biomass Conversion and Biorefinery
Fig. 7  SEM image of a neat epoxy; b coconut fiber–reinforced non-hybrid composite and c–f different coconut fiber/filler hybrid biocomposites
of biocomposites by varying the weight fraction of coconut
particles. The physical, mechanical, thermal, and structural
characteristics of the developed biocomposites have been
investigated following conclusions have been drawn.
• Treatment of coconut fiber-filler with 5% NaOH solution
increased the crystallinity index and crystalline size. It
also removed the dust, wax, and impurities from fiber-
particle surfaces and reduced the moisture absorption
capabilities.
• Treatment of fiber-filler resulted in increments of cel-
lulose contents percentage by decreasing the lignin and
hemicellulose content. This phenomenon has been spot-
ted by FTIR results. The alkaline surface treatment also
enhanced the thermal degradation and stability of the
biomass fiber. The reliability of tensile testing results
for coconut fiber has been analyzed by the Weibull dis-
tribution function and reported that treatments of fiber
improved the tensile strength by 25.98% and Young’s
modulus by 27.05% respectively.
• The addition of coconut particles up to 7.5% impacted
positively the mechanical performances of the developed
biocomposites. CRC-5.0 biocomposites observed maxi-
mum tensile strength (142.46 MPa) and flexural strength
(151.72 MPa), whereas CRC-7.5 biocomposites revealed
maximum tensile modulus (5.37 GPa) and flexural modu-
lus (7.45 GPa). The maximum degradation temperature
has been recorded at 350.47 °C for CRC-5.0 biocompos-
ites with better thermal stability.
• The addition of particles restricted the elongation before
the break and improved the brittleness of the biocom-
posites. Therefore, CRC-2.5 biocomposites examined
higher impact strength (88.41 J/m), fracture toughness
(6.63 MPa-m0.5, and fracture energy (1289.42 J/mm2)
compared to other developed biocomposites.
• The developed biocomposites showed comparatively less
water absorption behavior as compared to other natu-
ral fiber composites due to the presence of high ligno-
cellulose contents. The rate of corrosion has also been
observed at 0.006 mm/year which is much lower as com-
pared to traditional materials.
• The excessive addition of coconut particles (more than
7.5% by weight) resulted in the agglomeration and clus-
terization with the bio-epoxy matrix. This resulted in a
decrement in thermo-mechanical behavior that also has
been analyzed.
Thus, the utilization of agro/food waste from coconut
mesocarp, shell, and husk has great potential to develop
sustainable and eco-friendly biocomposites and could lead
to the development of a bio-based economy and boost the
agro-based rural Indian economy. Furthermore, the devel-
oped biocomposites are also capable and suitable for indus-
trial applications like automobile interior parts, packaging
industries to develop delivery boxes, construction industry,
and development of wind turbine blades and solar cell back
sheets.
13
13
Table 6  Comparative study of experimental results with previously reported results
References Matrix Reinforcement Tensile Tensile Flexural Flexural strength (MPa) Impact Water
modulus (GPa) strength (MPa) modulus (GPa) strength/impact absorption
energy (%)

Present study Bio-epoxy Coconut fiber and 5.366 ± 0.222 142.46 ± 6.228 7.451 ± 0.54 151.451 ± 7.45 88.41 ± 6.45 J/m 6.25
(FormuLITE) coconut shell husk
Balaji et al. [11] Vinyl esters coconut particles/nano clay 3.8 72.6 ± 9.228 186.42 ± 6.45 2.7 kJ/m2 11.62
Thiagamani et. al [60] SR greenpoxy 56 Hemp and sisal 1.095 30.76 ––- –– 11.86
Chaudhary et. al [61] Epoxy resin Sisal 1.64 43.32 1.78 86.6 10 ± 2.425 kJ/m2 ––-
Senthilkumar et. al [62] SR green poxy 56 Hemp 2.893 33.30 2.860 60.56 19.19 ± 1.425 kJ/ ––
m2
Raman et. al [63] Epoxy Bamboo and coconut shell 2.685 62.42 3.624 58.79 –– ––
Kishnasamy et. al [64] Epoxy resin Aloevera; Flax; Hemp ––- 46.41 –– 134.28 21.107 J/m 4.48%
Oladele et. al [65] Polyvinyl chloride coconut fiber and 3.12 ± 0.522 51.42 ± 7.23 3.8 ± 0.46 48.962 ± 8.752 98.42 ± 7.845 J/m2 ––
corn cub ash
Ashraf et. al [66] Epoxamite 100 epoxy Flat and glass 10.5 ± 1.53 241.2 ± 18.4 0.364 140.8 ± 11.3 ––- –––
Saha et. al [33] Epoxy LY-556 Hemp and flax 4.4 84.67 11.413 134.663 –– 5.06%
Lalta Prasad et. al [67] Polyester Flax –––- 74.61 ––– 18.35 6.7 J 2.43%
Saha et al. [30] Epoxy LY556 PALF and PALF particles 3.032 89.432 4.521 103.521 87.56 J/m 70%
Biomass Conversion and Biorefinery
Biomass Conversion and Biorefinery
Author contribution Santosh Kumar: investigation, methodology, writ-
ing—original draft and review and editing; Abir Saha: investigation,
methodology, writing—original draft and review and editing.
Data availability The authors declare that the data supporting the find-
ings of this study are available within the article.
Declarations
Ethical approval Not applicable.
Competing interests The authors declare no competing interests.
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