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DOI: 10.1177/1528083719832851
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characteristics of
treated/untreated
Portunus sanguinolentus
shell powder-based jute
fabrics reinforced epoxy
composites

P Kumaran1, S Mohanamurugan2, S Madhu1, R Vijay3,

D Lenin Singaravelu3, A Vinod4, MR Sanjay5 and
Suchart Siengchin5

Abstract
The current study deals with the effective usage of Portunus sanguinolentus shell, which is a
solid waste in the seafood industry. This Portunus sanguinolentus shell waste was powdered
and used as untreated fillers in jute fabrics reinforced epoxy composites. Then Portunus
sanguinolentus shell waste powder was treated with chemicals to perform fat removal,
deproteination, decarbonization and deacetylation to obtain treated Portunus sanguinolen-
tus shell filler. Three different composites were developed with traditional hand layup
process consisting of four layers jute fabrics that were filled with 10 wt% untreated
Portunus sanguinolentus shell filler, chemical treated 10 wt% Portunus sanguinolentus shell
filler and unfilled one. The thermo-mechanical and fracture morphologies were assessed

1
Department of Automobile Engineering, Saveetha School of Engineering, Tamil Nadu, India
2
Department of Mechanical Engineering, Aarupadai Veedu Institute of Technology, Chennai, Tamil Nadu, India
3
Department of Production Engineering, National Institute of Technology, Tiruchirappalli, Tamil Nadu, India
4
Department of Mechanical Engineering, Sri Lakshmi Ammal Engineering College, Chennai, Tamil Nadu, India
5
Department of Mechanical and Process Engineering, The Sirindhorn International Thai-German Graduate
School of Engineering (TGGS), King Mongkut’s University of Technology North Bangkok, Bangsue, Bangkok,
Thailand

Corresponding author:
MR Sanjay, Department of Mechanical and Process Engineering, The Sirindhorn International Thai-German
Graduate School of Engineering (TGGS), King Mongkut’s University of Technology North Bangkok, Bangsue,
Bangkok, Thailand.
Email: mcemrs@[Link]
2 Journal of Industrial Textiles 0(0)

by tensile, flexural, compression, shear, impact, hardness thermogravimetric analysis,

Fourier-transform infrared spectroscopy and scanning electron microscopy analysis.
The results showed an increase in the thermo-mechanical property of chemical-treated
Portunus sanguinolentus shell powder-filled jute fabrics-based epoxy composite. This phe-
nomenon is due to the increase in the chitosan, mineral contents and decrease in the
organic content in the Portunus sanguinolentus shell powder due to chemical treatment,
thus enhancing the bonding between the filler and fiber matrix with reduction of the void.
A showcase stand was developed with the best performer, as an attempt in the perfection
of application. The application is then analyzed using ANSYS to predict the deformation
behavior when subjected to 0.25 kg, 0.5 kg and 1 kg loads.

Keywords
Portunus sanguinolentus shell powder, chitosan, jute fabrics, thermal stability, filler

Introduction
Polymers reinforced with fibers, namely glass and aramid, increase several proper-
ties like stiffness, toughness and better strength-to-weight ratio when compared
with the addition of fillers, namely wood, and many types of fillers alone.
Though the addition of glass and aramid increases several properties, the cost
associated with it is very high, and it has disposal problems too. On the other
hand, the interest among the natural fiber reinforced polymers has increased due
to the environmental impact and increase in several properties of polymers [1–3].
The increase in mechanical strength of natural fiber reinforced polymers has gained
interest among certain researchers and industrial sectors [4]. Broad research has
been carried out in the area of polymers reinforced with jute fibers, coir fibers, rice
husk and straw, seashells and many more fillers, which have also been proved to be
a vital reinforcement in both types of plastics (i.e. thermosets and thermoplastics)
[5–8]. Even now the effect of waste filler and its surface treatment needs more focus.
Some of the literature related to it are discussed below. Boopalan et al. [9] manu-
factured hybrid epoxy composites based on jute and banana fibers and tested for
mechanical, water absorption characteristics. From the results, the mechanical and
resistance to absorption characteristics were the best for the 50/50 weight ratio
composites. The fillers were added to the jute and banana fibers, which showed
better improvement in their mechanical properties. Thus, the addition of fillers
boosted good strength-to-weight ratio. Prabhakar et al. [10] reinforced waste
peanut shell powder on epoxy composites and studied their thermo-mechanical
characteristics. It was reported that the thermo-mechanical properties of epoxy
composites were higher when alkali-treated fillers were used compared to untreated
powder. Li et al. [11] developed polypropylene composites based on waste shellfish
shell bio-filler and calcium carbonate filler. It was proved that the addition of
shellfish shell bio-filler to polypropylene increased mechanical properties when
compared to the addition of calcium carbonate. Sathiyamurthy et al. [12]
Kumaran et al. 3

investigated the influence of different fiber length and addition of filler on calcium
carbonate-filled coir fiber composites on various mechanical properties. From the
results, it was proved that the optimized fiber length and filler contents would increase
the desired properties. Athith et al. [13] studied the effect of tungsten carbide on the
mechanical and tribological properties of jute/sisal/E-glass fabrics reinforced natural
rubber/epoxy composites. It was observed that the filler loading with an optimal
percentage (10%) increased the mechanical properties and decreased the wear rate.
Agarwal et al. [14] manufactured chopped glass fiber reinforced in epoxy matrix
composites and chopped glass fiber epoxy composites filled with SiC. From the
results, it was shown that the addition of SiC by 10 wt% improved tensile and flexural
properties while the addition of SiC by 15 wt% showed better impact and hardness
characteristics. Vijay et al. [15] reinforced Azadirachta indica seed powder and spent
Camellia sinensis powders as fillers in jute epoxy composites; the results revealed
10 wt% of azadirachta seed powder showed increase in mechanical properties and
10 wt% of spent Camellia sinensis fillers in composites showed better thermal stability
due to the inorganic constituents present in it. Vinod et al. [16] studied the thermo-
mechanical behavior of calatropsis gigantea powder-filled jute-epoxy composites and
found that 10 wt% of the fillers-based composites showed enhanced thermal stability
and mechanical properties. Pawar et al. [17] studied the mechanical properties of
granite powder-filled jute fiber-based epoxy composite. It was found that an increase
in filler percentage more than 10 wt% caused a decrease in the ultimate tensile
strength and ultimate flexural strength properties of the composites. Raghavendra
et al. [18] studied the effect of fly ash filler loading wt% on the mechanical and erosive
characteristics of Woven Jute/Glass Hybrid Polymer Composite. It was found that
10 wt% of fly ash-based hybrid composites showed better flexural, tensile and erosive
resistance characteristics. From the literature survey, it was found that there are many
works related to the natural fiber reinforced with epoxy composites, mostly 10 wt% of
fillers produced good performance due to the prevention of agglomeration when
mixed in the matrix. Less number of works have been reported with different shell
reinforced composites and there is no work reported with the use of Portunus sangui-
nolentus shell powders and chemical treated shell powders in the epoxy composites.
Thus, in this study, the jute fabrics-epoxy composites were developed by reinforcing
treated and untreated Portunus sanguinolentus shell powder with 10 wt%. For com-
parison purposes, jute fabrics-based epoxy composites without reinforcement were
also developed. The developed composites were characterized for their mechanical
behavior viz. hardness, tensile, flexural, impact, compression strength and thermal
stability using thermogravimetric analysis (TGA). The morphology of the tested
composites was studied using scanning electron microscope (SEM).

Materials and methods

Jute fibers are abundantly found in the Bengal regions of India and Bangladesh.
The fibers are separated from the stem of the jute plant using manual retting pro-
cess followed by dehydrating in the air. Jute fibers used in the present study are
4 Journal of Industrial Textiles 0(0)

fabrics (bi-woven fiber mat). The fabric used was 300  300 mm. It has  126
threads longitudinally and latitudinally, possessing 160 GSM. It possesses tensile
strength ranging from 647 MPa, cellulose and lignin contents 62% and 13%,
respectively, and having a density of 1.32 g/cc [16]. The epoxy resin with grade
LY556 usually called as Bisphenol A Diglycidyl Ether and Hardener possessing
HY951 grade called as tri-ethylene tetramine was used as matrix. They were mixed
in 10:1 ratio for enhancing the adhesion and strength [16]. Portunus sanguinolentus
belongs to the Portunus crab family commonly known as Blood-spotted Swimmer
Crab (three spot crab) in the coastal regions of Chennai, South India (Latitude 13
040 N, Longitude 80 170 E). Its shell is a solid waste which is thrown after con-
suming the Portunus sanguinolentus as eating. This shell was procured from a local
seafood dealer and was thoroughly washed in the distilled water, ground in a
mortar and sieved to 150–200 microns. Generally, Portunus sanguinolentus bouli-
gand structure comprises the cuticle, the outer non-cellular layer, comprising three
sub-layers namely endocuticle, which is the inner and thickest layer made up of
chitin and arthropodin, a soft, colorless and flexible layer. Exocuticle layer is the
middle layer, which is much thicker, dark and rigid due to the chitin and sclerotin
composition. The outer thinnest layer is the epicuticle. This layer is subdivided into
inner epicuticle which contains wax filaments, while the outer epicuticle makes
contact with cuticulin. Cuticulin is the non-chitinous polymerized lipoprotein
layer, and the wax later presents consisting of closely packed molecules to prevent
desiccation and the cement layer which forms the outermost layer protects the wax
layer. The cuticle mainly constitutes chitin which is the main constituent of cuticle
made of Nitrogenous polysaccharide and polymer of N-acetylglucosamine, which
is insoluble in water but soluble in dilute acids, alkalis and organic solvents. The
Arthropodin is an untanned cuticular protein soluble in water. Sclerotin is a tanned
cuticular protein that is insoluble in water [19]. Figure 1 explains the presence of
protein, chitin fibers and the overview of the bouligand structure. The Portunus
sanguinolentus consist of bouligand structure which comprises chitin fibers that are
covered with protein. Upon chemical treatment chitin gets converted to chitosan.
To remove protein and other ingredients, the following procedure was followed.
In order to eliminate the fat content, sieved shell powders were treated with a
solution of chloroform and methanol (ratio 2:1) at room temperature for 1 h.
Followed by deproteination by immersing in 5 wt% of sodium hydroxide solution
for 24 h and then decarbonization of the samples was done using 4 wt% of hydro
chloric acid solution for 1 h. Deacetylation was done with 50% sodium hydroxide
solution at 100 C for 4 h to get chitosan-based shell powder. At last, filtration was
done to remove the solution and dried at normal environmental conditions to get
desired treated powder filler, the percentage of chemicals was considered as per the
literature findings [20,21]. The photographic images of untreated Portunus sangui-
nolentus shell powder, Treated Portunus sanguinolentus shell powder and Biwoven
Jute fiber mat (fabrics) are shown in Figure 2(a) to (c) and SEM image of treated
Portunus sanguinolentus shell powder is shown in Figure 2(d). The alkali treatment
breaks the chitin to form chitosan as shown in Figure 1. Figure 2(d) shows that
Kumaran et al. 5

Figure 1. Shell structure of Portunus sanguinolentus and chitosan formation from chitin.

Figure 2. Photographic images of (a) untreated Portunus sanguinolentus shell powder; (b) treated
Portunus sanguinolentus shell powder; (c) Biwoven jute fiber mat; and (d) SEM image of treated
Portunus sanguinolentus shell powder. SEM: scanning electron microscope.
6 Journal of Industrial Textiles 0(0)

Figure 3. Overview of the manufacturing of the composites. (a) First jute fabrics layer followed
by application of Portunus sanguinolentus shell powder-based matrix mixture; (b) second jute
fabrics layer after application of filler-matrix mixture; (c) stacking of third jute fabrics layer over
the previous layer; and (d) fourth jute fabrics layer and finished composite.

the treated Portunus sanguinolentus shell powder which has a rough surface since it
is treated with chemicals thereby removing protein and other organic matters from
its surface.

Manufacturing of composites
The overview of the manufacturing process of the developed laminates is given in
Figure 3. A conventional hand layup method was used for fabricating the
Kumaran et al. 7

Table 1. Designation and composition of the developed composites.

Filler (wt%) Fiber (wt%)

Untreated Treated
Portunus Portunus Jute
sanguinolentus sanguinolentus (4 layers Epoxy-hardener
S. No. Designation shell powder shell powder of jute) mixture (wt%)

1 CF-1 0 0 40 60
2 CF-2 10 0 40 50
3 CF-3 0 10 40 50

composite material in this present study. Jute fibers were purchased in the form of
bi-woven mats and kept in a hot air oven for 1 h at 60 C to remove the traces
of moisture, though it was dried in the hot sun for 24 h. The flat and smooth surface
of size 300 mm * 300 mm was considered and coated with a layer of wax, followed
by wiping with a soft cloth. A layer of polyvinyl alcohol, a releasing agent, was
applied for easy removal of the cured composites. Then, the coated surface was left
in the hot sun for drying and setting. In order to make filler-based composites CF-2
and CF-3, 10 wt% of untreated and treated Portunus sanguinolentus shell powder
fillers were mixed with 90 wt% of resin and hardener mixture. The fillers were
added to the resin and mixed using mechanical stirrer until it gets dispersed prop-
erly. Then vacuum processes were used to remove the entrapped air. After that
hardener was added and mixed manually. Again, vacuum processes were used to
remove the entrapped air. Then a layer of resin-hardener and filler mixture was
applied to the necessary dimensions, and a layer of bi-woven mat jute fiber was
placed as shown in Figure 3(a), followed by a layer of resin hardener and filler
mixture, over which a jute fiber mat was placed as shown in Figure 3(b). A coat of
resin, hardener and filler was given with the roller, and again jute fiber mat layer
positioned as seen in Figure 3(c). Finally, a layer of jute fiber mat was placed, and a
final coat of resin-hardener and filler mixture was given as shown in Figure 3(d).
Rollers were used to remove the air traps from the laminates during stacking. For
proper distribution in the developed composites, a 25-kg per square feet of the load
was applied in order to attain good distribution of matrix and better packing. It
was kept untouched for 24 h in an ordinary environmental situation [15,16]. Care
was taken to ensure that there were no air traps. In the case of CF-1 composite,
100 wt% of resin and hardener were used to develop the composite with the similar
procedure stated above, and no filler was used. The designation and composition of
the developed composites are given in Table 1.

Characterization of manufactured composites

The experimental density (ex) of the developed laminates was measured using a
simple water immersion method. Distilled water was used for this test.
8 Journal of Industrial Textiles 0(0)

Five measures were carried out for each sample, and average values were recorded
[13]. To find out the theoretical density (th), the following equation (1) is used

wf þ wp þ wm
th ¼  
wf wp wm ð1Þ
þ þ
f p m

where ‘Wf’ is the fiber weight, ‘Wp’ is the filler weight, ‘Wm’ is the matrix weight, ‘f’
is the fiber density, ‘p’ is the filler density and ‘m’ is the matrix density.
The fraction of void content (c) was determined from the theoretical and experi-
mental densities of the composites using equation (2). Where th is the theoretical
density and ex is the experimental density

th  ex
c ¼ ð2Þ
th

The weight, volume and density values for the materials used in the developed
composites are given in Table 2. The weight percentage of the fillers varies due to
the varying density of the fillers due to treatments. However, the volume of the
composite remains constant. Untreated and treated fillers in the below table
denoted untreated and treated Portunus sanguinolentus shell powders, respectively.
Fourier transform infrared (FTIR) spectroscopy was used to find the functional
groups present in the treated and untreated Portunus sanguinolentus shell powder
and the constituent that corresponds to the functional group. The IR spectrum was
recorded using Perkin Elmer/Spectrum 2 (Diamond UTAR). The spectrum was
captured from 4000 cm–1 to 400 cm–1 with a resolution of 2 cm–1 signal-to-noise
ratio at the rate of 32 scans per minute. In order to perform various mechanical
tests, the developed laminates were cut using a saw cutter as per required dimen-
sions. The mechanical properties were analysed for the laminated composite spe-
cimen according to the ASTM. Each test was performed at room temperature. The
three specimens were tested, and consistent results were reported for each test.
Tensile tests were conducted using the servo-hydraulic universal testing machine
(Model No.: UTES-40, Make: Fuel Instruments & Engineers Pvt. Ltd.) with max-
imum capacity 400 kN according to the ASTM D 638-14 with a loading rate of
2 mm/min. The specimen was cut to the dog-bone-shape having dimensions
165 mm  19 mm, and the mid-span length was 57 mm. The samples were held
between grippers of the UTM, and the load was increased until a fracture occurred.
Flexural tests were carried out according to the ASTM D790-10 using the universal
testing machine with model and make as stated above with a loading rate of
2 mm/min. The dimensions of the specimen are 165 mm  19 mm. Three-point
bending mode was applied for measuring the ultimate flexural load and strength,
with rollers of diameter 30 mm. The application of load was made until the fracture
occurred. The compression tests were carried out according to the ASTM D695-15.
 Kumaran et al.

Table 2. Weight, volume and densities of the materials used in developed composites.

Weight (g) Density (g/cc) Volume (cc)

Jute Untreated Treated Jute Untreated Treated Jute Untreated Treated Total
Composites Fiber filler filler Matrix Fiber filler filler Matrix Fiber filler filler Matrix Volume

CF-1 262.8 – – 310.5 1.46 – – 1.15 180 – – 270 450

CF-2 262.8 150.75 – 236.25 1.46 0.59 – 1.15 180 45 – 225 450
CF-3 262.8 – 146.7 236.25 1.46 – 0.55 1.15 180 – 45 225 450
9
10 Journal of Industrial Textiles 0(0)

The dimensions of the compression specimen are 55 mm  55 mm. The compression

tests were carried out in the universal testing machine at room temperature until a
fracture occurred. The machine is fixed with a pair of compression plates, with
diameter 120 mm for compressing the sample. The variations of stress with response
to strain are obtained graphically for all the above tests. The double shear test was
performed according to ASTM: D5379 in Universal Testing Machine. The dimen-
sions of the specimen are 76 mm  20 mm, with notch angles of 90 on either side
held in a fixture, and load was applied till the material fracture. The energy absorbed
was measured as per the ASTM D256-10 in a Charpy impact testing machine (Model
No.: IT-30 (D) and Make: Fuel Instruments & Engineers Pvt. Ltd.) using a notched
specimen. The dimensions of the impact specimen are 76 mm  20 mm, with a notch
angle 90 . Three specimens were prepared for each test, and the best value (consist-
ent) was reported. The hardness was measured using Shore-D hardness tester (Model
No.: Type D VT-10D) as per the ASTM: D2240-15e1, tester possessing an indenter
1.25-mm diameter with a conical point having 30 angle and radius tip 0.1 mm with
4.550 kg applied load. Five readings were taken down for each specimen, and the
average was noted. TGA (Model: TGA4000; Make: PerkinElmer) was used for
finding the thermal stability in a nitrogen environment using 5 mg of sample
weight with temperature ranging from normal room temperature to 800 C with
10 C/min heating rate with the gas flow of 20 mL/min. The crucible used was
made of ceramic. The fractured interface (specimen) was cut into 15 mm  15 mm
using a diamond cutter, sputtered with conducting material (gold) and then analyzed
in SEM of Tescan VEGA 3LMU, the Czech Republic, to study the various morphol-
ogies of the tested specimen. The tensile, flexural, impact and compression tested
samples are shown in Figure 4(a) to (e).
The complete methodology involved in this work is given in the form of the flow
chart in Figure 5.

Results and discussions

The characterizations of the fillers and the developed composites are discussed in
the forthcoming sections.

FTIR analysis of treated and untreated Portunus sanguinolentus shell powder

The FTIR spectrograms of the untreated and treated Portunus sanguinolentus shell
powder are given in Figure 6. From the spectrograms, the first small ‘U’ bend at
3253 cm–1 and 3248 cm–1 denotes the regions of OH and NH, which attributes the
presence of -Chitin for the untreated and treated Portunus sanguinolentus shell
powder [22]. The second intensity peak is observed at 2882 cm–1 for the untreated
Portunus sanguinolentus shell powder, it is caused by the C-H stretching and vibra-
tion from CH, and CH2 attributes the presence of chitin biopolymer. The treated
Portunus sanguinolentus shell powder does not show the peak at this range because
the alkali treatment removes the excess amount of chitin present in it [23]. The next
Kumaran et al. 11

Figure 4. Tested specimens of developed composites: (a) tensile; (b) flexural; (c) impact;
(d) compression; and (e) shear.

corresponding peaks at 1645 cm–1 and 1629 cm–1 represents the presence of amide
groups of chitin polysaccharides [24]. The next intensity peaks at 1399 cm–1 and
1397 cm–1 corresponds to the asymmetric stretching and vibrations of C = O,
which attributes to the presence of CaCO3 [21,25]. A strong asymmetric stretching
of C-N-C is observed at the regions of 1014 cm–1 and 1029 cm–1 [25]. The last
intensity peaks at 873 cm–1 and 860 cm–1, respectively, for untreated and treated
Portunus sanguinolentus shell powder denote the out-of-plane bending of CO32–,
which attributes to the presence of calcite [23].

Density and void characteristics of the developed composites

The density of the developed composites is shown in Table 3 in which the experi-
mental density of filler-filled composites as well as CF-3 is high. Since the filler fills
the voids effectively, thereby preventing voids that are visible in the void content
12 Journal of Industrial Textiles 0(0)

Figure 5. Work methodology flow chart.

Kumaran et al. 13

Figure 6. FTIR spectrograms of untreated and treated Portunus sanguinolentus shell powder.
FTIR: Fourier-transform infrared spectroscopy.

Table 3. Theoretical, experimental densities and void content of the

developed composites.

Theoretical Experimental Void

Composite density (g/cc) density (g/cc) content (%)

CF-1 1.25 1.18 5.6

CF-2 1.04 1.01 2.89
CF-3 1.21 1.19 1.65

percentage [13]. The percentage of void in CF-3 is 3.39 times lesser than that of
CF-1 and 1.75 times lesser than that of CF-2.

Tensile properties of the developed composites

The tensile strength of the composites mainly depends on the fiber and filler-matrix
interaction. The composite CF-3 showed higher ultimate tensile strength followed
by CF-2 then by CF-1 as shown in Figure 7. The higher tensile strength values are
mainly due to the following reasons. Crab shell will have a protein layer in the
chitin structure which hinders the matrix-filler interaction as stated in the literature.
14 Journal of Industrial Textiles 0(0)

Figure 7. Ultimate tensile strength of the developed composites.

Upon the chemical treatment of deproteination, these proteins that act as polymer
matrix get removed and, thus, the adhesion level of the resin increases. This is in
good agreement with the literature findings that treated crab shell filler could be
used for Ni- Phosphorus coating due to its better adhesion properties [26]. The
translucent layer of chitin was present beneath the protein layer. The layer of
protein polymer is confirmed from the studies done [27]. Upon all treatments,
the protein layer gets removed, when the chitin was impinged into the resin and
coated on an acrylic sheet. The sheet became transparent, produced better results
and, thus, this material could be a breakthrough to meet out various optical trans-
parent applications with good thermal expansion/degradation resistance of the
polymer. The stability at high temperatures is shown in the TGA of Figure 17.
In the forthcoming sections, the literature states that moisture and protein play an
important role in the strength of the crab shell [28], but this postulate will not
match with the current study because the literature study was preformed for the
bare crab shell-based composite without reinforcement in the matrix. However, the
present investigation deals with the incorporation of fillers in the matrix. Thus,
protein removal becomes mandatory to enhance improved properties. The struc-
ture of chitin with protein is given in Figure 1; which confirms that protein is
present along with the chitin fibers in the bouligand structure.
The chemical treatment also enhances the surface roughness leading to more
wetting of the resin with fillers by forming interlocks that prevent the composite
from failing drastically. The surface roughness of untreated Portunus sanguinolen-
tus shell powders is 0.61 mm, while the treated Portunus sanguinolentus shell powder
Kumaran et al. 15

Figure 8. Tensile stress–strain graphs of the developed composites.

showed 0.95 mm. Poor wetting of fibers by polymer results in materials with defects
such as voids and fiber agglomerates, which promotes premature failure. Usually,
fiber reinforced composite depends considerably on the fiber-matrix interface because
only a well-formed interface allows stress transfer from the matrix to the fiber. Thus,
the presence of firm bonding of chemical-treated Portunus sanguinolentus fillers with
matrix along the crack growth region arrests the crack from propagating drastically.
This prevents ductility failure, thereby leading to the brittle failure, which is con-
firmed from the percentage strain of the stress–strain graph (Figure 8). The reason
behind the increase in strength is mainly the chitosan formation from chitin upon
chemical treatment as shown in Figure 1, which creates a permeable surface with high
strength leading to high wetting of resin [29]. The CF-2 composites were second in
quantity when compared to CF-1 as shown in Figure 7. This was mainly due to the
presence of fillers which got distributed uniformly instead of getting agglomerated in
the matrix, but the adhesion level was a little lower as compared to CF-3, but higher
than that of CF-1. The tensile modulus of the CF-2 and CF-3 is found to be
358.33 MPa and 550 MPa, respectively, the increase in the tensile modulus in CF-3
is because the alkali treatment has increased the surface roughness of the fillers, thus
enhancing the bonding between the fiber filler and matrix. The presence of fillers
always enhance better results, and this was in accordance with the literature [30].
A similar trend was also seen in the Argan nut shell particles reinforced poly-
ethylene composites, where the chemical-treated nut shell-filled composites showed
better results when compared to unfilled and untreated one [31]. It was also found
that, if the percentage of filler exceeds the certain optimal limit (preferably in
the range of 10–15%), then there exists a reduction in the strength values.
The increased stiffness shows the effect of matrix mobility reduction due to the
16 Journal of Industrial Textiles 0(0)

presence of fillers, which hinders the crack growth. The stress–strain curve of
Figure 8 shows non-linearity due to randomly oriented fibers, as well as the break-
age of salt regions of crab shell fillers present in the matrix of CF-2 and CF-3,
which is in accordance with the literature [32]. The ultimate tensile strength of CF-3
is 55 MPa, which is 1.3 times higher than CF-2 (43 MPa) and 1.75 times higher than
CF-1 (31.5 MPa) as shown in Figure 7. The ultimate tensile strength of CF-3
composite is also 1.12 times higher than 10 wt% Calotropis gigantea stem
powder-filled jute fiber reinforced epoxy composites (48.73 MPa) [16] and 1.6
times higher than granite powder-filled treated jute fiber reinforced epoxy compos-
ite (33.13  1.15 MPa) [17]. But this value is lesser than tungsten carbide-filled jute/
sisal/glass-based epoxy and natural rubber composites since glass fiber is used as
the stack layer in the composite [13]. The poor results of CF-1 are due to the voids
caused by poor wetting characteristics leading to poor fiber-matrix interactions,
though care was taken to remove air bubbles. This was overcome by CF-3 followed
by CF-2 due to the presence of fillers, which filled the voids. The other reason for
the poor results in CF-1 is the improper fiber-matrix interactions, which was caused
due to the poor bonding nature of the jute fibers with the matrix, though other two
composites consisted of jute fibers, the fillers present prevented the composite from
early breakage. The reduction in the strength of CF-1 composites is mainly due to
the presence of more voids, fiber agglomeration, fiber bending, fiber knitting, fiber
tear and also lagoon of fibers. Thus, the CF-3 composites could be a positive
solution for high-strength, lightweight applications.

Flexural properties of the developed composites

The CF-3 composites showed higher ultimate flexural strength values (5.45 MPa),
which were 1.29 times better than CF-2 (4.2 MPa) and 1.37 times than CF-1
(3.95 MPa) as shown in Figure 9. These values are higher than Azadirachta
indica seed/spent Camellia sinensis bio-filler-based jute fabrics-epoxy composites
(5.4 MPa and 3.15 MPa) [15]. The increased ultimate flexural strength values are
mainly due to the following reasons. The degree of mechanical strength of the
composites is mainly dependent on the reinforcing filler and the strong adhesion
between the matrix and filler. In the current study, the chemical-treated Portunus
sanguinolentus fillers have firm adhesion with the matrix, which had already been
described in the previous sections. The interlocks formed with the matrix prevented
the low strength failure of the composite. The ultimate flexural strength is also
dependent on the nature of failure based on the strain as shown in Figure 10. CF-3
resulted with high ultimate flexural strength and low strain rate when compared to
other flexural tested composites; this showed the difference in the current value.
There are more undulations seen in the stress–strain graph, as shown in Figure 10,
in case of CF-3 and CF-2 due to the presence of Portunus sanguinolentus shell fillers
along the path of the failure, and another reason was salt region breakage as
explained in the previous section. The literature findings also state that brittle
fracture occurs due to the inorganic phase at low strain, which leads the chitin
Kumaran et al. 17

Figure 9. Ultimate flexural strength of the developed composites.

Figure 10. Flexural stress–strain graphs of the developed composites.

18 Journal of Industrial Textiles 0(0)

phase to bear the load and a steep failure occurs in the composite [32]. The dis-
persion of fillers in the matrix preventing agglomeration is the prime cause for
enhancing the strength; these findings are in accordance with the literature [33,34].
In the case of CF-3 composite, the cracking of the matrix was caused due to the
stress induced during the flexural testing. The SEM image shows that the fillers are
more uniform in size, which leads to better strength, which is in accordance with
the literature [35]. Interesting fact about the CF-3 composite is that the presence of
a hydroxyl group on the surface of the filler forms a good bond with the matrix as
stated in the literature [36]. This, in turn, increases the wetting and adhesion of the
filler with the matrix, i.e. there is an increase in the cross linking, leading to the
deflection of cracks in the composites, and also the pinning of cracks takes place
due to the treated fillers present along the path of the crack. Another interesting
mechanism involved in CF-3 composites is the percolation mechanism in which the
chitosan filler makes the resin matrix to enter into its structure wall, leading to the
very firm bonding with the matrix [37]. The ultimate flexural strength of the CF-1 is
low when compared to other two composites due to the presence of a void, which
makes the fibers to easily get pullout (debonding), fiber bending, matrix crack,
straining of the matrix, leading to the poor results. If the fiber-matrix adhesion
is poor due to improper wetting, there will be more crack formation paths, and an
absence of fillers does not obstruct the same. The flexural modulus of the CF-2 and
CF-3 are 100 MPa and 120.92 MPa, respectively. The increase in the flexural modu-
lus in CF-3 is because the alkali treatment has increased the surface roughness of
the fillers, thus enhancing the bonding between the fiber filler and matrix. The
optimal percentage of chemical treatment nature also plays a significant role in
the strength of the composites. In the present study, 5% of sodium hydroxide was
used for removing proteins from its surface, which also played a crucial role in
strength, since, the alkali solution is in optimal percentage for removal of organic
contents and made uniform. If there were more alkali concentration in the solution,
then there could be a reduction in the strength of chitosan fibers, which will
increase the porous nature of the chitosan leading to the reduced flexural proper-
ties, which is in accordance with the literature [38].

Compression properties of the developed composites

In the present work, CF-3 composites showed higher ultimate compressive strength
(93 MPa), which is 2.1 times for CF-2 composite (42.5 MPa) and 4.89 times for CF-
1 composite (19 MPa) as shown in Figure 11. These values are higher than
Azadirachta indica seed/spent Camellia sinensis bio-filler-based jute fabrics-epoxy
composites (53 MPa and 33.5 MPa) [15]. The treated Portunus sanguinolentus shell
fillers showed better bonding with the matrix due to the rough surface caused due
to the chemical treatment leading to the formation of chitosan from chitin and also
the hydroxyl group present in the filler will adhere to the matrix leading to higher
strength. It is proved in the literature that chemical treatment led to the interfacial
bonding with the matrix, thus, leading to better dispersion [39].
Kumaran et al. 19

Figure 11. Ultimate compressive strength of the developed composites.

Figure 12. Compression stress–strain graphs of the developed composites.

Generally, the treated filler-matrix showed better results as compared to

untreated and unfilled composites, which are in accordance with the literature
[40]. The typical stress–strain curves for the brittle and ductile natures for uni-
axial compression testing are illustrated in the literature [41]. In the present
20 Journal of Industrial Textiles 0(0)

study, graph of Figure 11 comes under the category of brittle failure since it shows
the shape of the hemisphere which is also non-linear. In Figure 12, the stress–strain
graph shows such shape due to the presence of fillers, which come along the crack
path preventing the crack at the early stage; this happens in the CF-3, so it pro-
duced higher ultimate compressive strength. Generally, the brittle nature will have
less strain when compared to the other. Similarly, CF-3 also showed less strain rate,
which was due to the presence of treated Portunus sanguinolentus shell powders in
the matrix preventing the mobility of the resin, due to the better wetting nature of
the resin with the filler, this is in accordance with the literature [42]. It is also said in
the literature that modified shell waste or treated shell powder can enhance the
mechanical behavior of the composites [43]. CF-1 showed poor ultimate compres-
sive strength results due to its large size of voids with more fiber tear, which shows
the improper wetting of the fiber in the matrix; even the voids present played a vital
role in the deterioration of the properties.

Shear properties of the developed composites

From Figure 13, it is very clear that the laminated composite CF-3 possess the
highest ultimate shear strength of 30.15 N/mm2 when compared to the other lami-
nated composites. The stress–strain graphs for the shear tested composites are
shown in Figure 14, in which the CF-03 composites showed the higher value of
strength with good strain while the CF-2 and CF-1 showed inferior strength as well
as the strain rates. The improvement in the ultimate shear strength is due to the
presence of treated Portunus sanguinolentus shell powders, which possess good
bonding with the matrix. The ultimate shear strength of CF-3 is 3.72 times
higher than CF-1 and 1.65 times higher than CF-2. The similar type of results is
reported in the literature [44].

Impact and hardness of the developed composites

Impact strength refers to the toughness of the material, i.e. the ability of the mater-
ial to absorb energy. The highly stiff material could not absorb the more amount of
energy during the failure, only ductile material can withstand high impact load.
But the current study shows the results against the above concept, in which CF-3
(6.21 J) showed 1.08 times higher strength than CF-2 (5.75 J) and 1.31 times higher
than CF-1 (4.76 J) composites as shown in Figure 15. These values are higher than
tungsten carbide-filled jute/sisal/glass-based epoxy and natural rubber composites
(4.10 J). This trend was in accordance with the literature findings [45]. Similarly, in
the literature snail shell-filled composites showed better trend till 30 volume per-
centage and the reason for it was the mineral contents present in it enhanced the
same [46].
In the current study, Portunus sanguinolentus shell powders are rich in calcium
carbonate without protein content (viscous layer on the surface of the shell) which
interacts with the strong fiber-matrix interfacial strength and energy dissipation by
Kumaran et al. 21

Figure 13. Ultimate shear strength of the composites.

Figure 14. Shear stress–strain graphs of the composites.

fiber pull-out is very limited owing to the presence of fillers, which enhance the
energy-absorbing nature during impact, to a considerable extent. It is also note-
worthy that impact strength is dependent on the particle size, shape and distribu-
tion of the fillers, in the case of CF-3 composites, where the particles are rough
enough and adhere to the matrix firmly.
22 Journal of Industrial Textiles 0(0)

Figure 15. Energy absorbed during impact conditions in the developed composites.

Hardness is defined as the resistance to indentation of the indenter in any mater-

ial being tested. The composite CF-3 showed good results of hardness with the
highest value of 67, while the CF-2 showed the second highest value of 61 and
the third i.e. least value by CF-1 composites by 57 as shown in Figure 16. The
enhanced results of CF-3 composites are mainly due to the presence of treated shell
powders, which got mixed evenly with resin and filled the voids as explained in the
previous sections and Table 3. In the case of CF-2 though the untreated shell
powder filled the voids, it does not adhere well to the matrix due to the presence
of protein content in it. The CF-1 composites possess more voids, and it is unfilled,
so the value is purely dependent on the fiber and the resin in this case. In general, it
is very clear that the highly stiff composite will always have more hardness, which is
in accordance with the literature work on wood flour as a filler in the composite
[47]. These values are also higher than Azadirachta indica seed/spent Camellia
sinensis bio-filler-based jute fabrics-epoxy composites [15].

Thermal stability of the fillers and developed composites

The thermal stability of the developed composites and raw fillers are found out
using TGA, and the graph is shown in Figure 17. The parameters like onset, end
set, decomposition temperatures and residue percentages are found out and
reported. The treated Portunus sanguinolentus shell powder possesses three
stages. The first stage is in the range of 100–230 C, where there is the degradation
of moisture and low, stable constituents, followed by the second stage, i.e. decom-
position of chitosan, which was formed due to the chemical treatment of chitin in
Kumaran et al. 23

Figure 16. Hardness of the developed composites.

Figure 17. Thermal stability of the raw fillers and developed composites.

the range of 230 to 425 C. Then, the third stage where the decomposition of the
mineral constituent calcium carbonate is in the range of 430 to 650 C [48]. The char
residue percentage was 44%, which was mainly due to the calcium oxide and some
other mineral constituents in it; and this is in accordance with the literature [25].
24 Journal of Industrial Textiles 0(0)

The third stage undergoes the steps of degradation namely the calcium carbonate
degradation by liberating carbon dioxide and retaining calcium oxide. This stage is
also the phase transformation stage where calcite crystals are formed from the
aragonite. The highest residue is mainly due to the presence of the high content
of calcium oxide with some traces of mineral contents. The presence of residue also
confirms that evaporation of the substances takes place with the decomposition of
the constituents; which is in good agreement with the literature [49,50].
The untreated Portunus sanguinolentus shell powder was subjected to TGA. The
degradation followed the same three stages in which 90–200 C, in which the mois-
ture, water content present in the cuticle layer and the protein degradation took
place, since this untreated one has more protein layer as explained in the previous
section i.e. Figure 1. Then the degradation undergoes the next stage of 213 to
415 C, where the chitin present with the traces of protein present in the structure
will undergo degradation. Then the third stage is the decomposition of mineral
ingredients namely, calcium carbonate, which decomposes in the temperature
range of 423 to 645 C. The maximum degradation occurs at 597 C, which was
mainly due to the decomposition of calcium carbonate to form calcium oxide
liberating carbon dioxide. The residue char left behind after the testing was
33%, there was more reduction in the char percentage when compared to the
treated filler, mainly due to the protein, water molecules and wax layer present
in it, that is in accordance with the literature [19].
The composite CF-1, which is made of jute fibers without the presence of fillers
undergoes degradation in three stages. Again in the first stage the degradation of
moisture, lignin, proteins of jute fibers and matrix degradation till 200 C, while the
degradation of hemicelluloses undergoes in the range of 300 C, while the maximum
degradation of cellulose occurs during the temperature of 360 C, which is in
accordance with the literature [51]. The end of degradation occurs at 490 C.
Then the degradation continues due to the presence of some inorganic minerals
present in the composite. The char residue present after the testing is 22%. In the
case of CF-2 composite, the degradation followed the similar trend of CF-1, but
the fillers present in the matrix came into existence during the testing leading to the
changes in the residue char percentage to 28 due to its inorganic mineral constitu-
ents as explained in the previous sections. The maximum degradation occurred at
412 C and the onset and offset temperatures were 200 C and 560 C. In the case of
CF-3, which was filled with treated Portunus sanguinolentus shell powder showed a
better trend when compared to others in which the onset and offset temperatures
got shifted to 226 and 640 C, with maximum degradation temperature occurring at
495 C, which was due to the decomposition of calcium carbonate. The char residue
percentage of CF-3 composite was 35%, which is closely associated with the raw
filler percentage, though there may be a deviation in the percentage due to the bare
and resin-filled powders. It is stated in the literature that material which is having
more molecular weight will undergo less degradation when compared to the less
molecular weight. The presence of Portunus sanguinolentus shell powder in the
CF-2 and CF-3 composites followed the same trend when compared to CF-1.
Kumaran et al. 25

The molecular weight shown in the literature for crab shell was 1.2  105 g/mol
[52], thereby increasing the thermal stability of the composite and also the literature
findings stated that higher stable material present in the composites increases the
stability, this postulate is in accordance with the current study. Thus, the thermal
stability followed the trend of CF-3 > CF-2 > CF-1 (higher to lower stability).

Morphological characterization
The morphological characters of the tensile-tested specimens are shown in
Figure 18. Figure 18(a) shows the rough composite surface, fiber-matrix interaction
and the crack path filled with fillers corresponds to the tensile tested specimen of
CF-3. From the Figure 18(b), it can be seen that the fillers fill the voids in the case
of CF-3, thus leading to better adhesion of the fiber and matrix leading to an

Figure 18. (a) SEM image shows the roughness and other characteristics formed due to treated
filler in the CF-3 tensile tested composite; (b) SEM image represents void filled with fillers in
tensile tested CF-3 composite; (c) SEM image represents various failure defects in tensile tested
CF-1 composite; and (d) SEM image represents knitting and fiber bending at the interface of
tensile-tested CF-1 composite.
26 Journal of Industrial Textiles 0(0)

Figure 19. (a) SEM image shows proper mixing of filler, its effect on filler distribution and
crazing of resin matrix in flexural tested CF-3 composite; (b) SEM image shows the deflection of
cracks and pinning of cracks due to the treated filler on the CF-3 flexural tested composite; and
(c) SEM image shows the various features which are responsible for the failure of CF-1 composite.

increased tensile strength. The low tensile strength of CF-1 is due to the voids
caused by poor wetting characteristics leading to poor fiber-matrix interactions,
though care was taken to remove air bubbles. This was overcome by CF-3 followed
by CF-2 due to the presence of fillers, which filled the voids. As represented in the
SEM image of Figure 18(b). The reduction in the strength of CF-1 composites is
mainly due to the presence of more voids, fiber agglomeration, fiber bending, fiber
knitting, fiber tear and also lagoon of fibers that are seen in the SEM images
Figure 18(c) and (d).
The improper mixing leads to the decreased flexural strength. Proper mixing is
shown in SEM image of Figure 19(a), showing the area covered by the matrix
surface. The increases in the wetting and adhesion of the filler with the matrix,
i.e. increase in the cross-linking leading to the deflection of cracks in the composites
and also the pinning of cracks takes place due to the treated fillers present along the
path of the crack, as clearly seen from the SEM image of Figure 19(b). The ultimate
flexural strength of the CF-1 is low when compared to other two composites due to
Kumaran et al. 27

Figure 20. (a) SEM image shows the void filled with untreated fillers and debonding of fillers
from the matrix for CF-2 composite; (b) SEM image shows voids and fiber tear in case of CF-1
composite.

the presence of void, which makes the fibers to easily get pullout (debonding), fiber
bending, matrix crack and straining of the matrix leading to the poor results, which
can be clearly visualised from the SEM image in Figure 19(c).
The SEM image in Figure 20(a) shows filler debonding in the case of CF-2
composites since the protein layer will not adhere well with the matrix leading to
the debonding though the fillers filled the voids of the composites for considerable
stress transfer. In this property also CF-1 showed poor ultimate compressive
strength results due to its large size of voids with more fiber tear, which shows
the improper wetting of the fiber in the matrix; even the voids present also played a
vital role in the deterioration of the properties. These features are visualized in
SEM image of Figure 20(b).
The SEM image of Figure 21(a) represents the voids present in the CF-3 com-
posites, and those voids also got filled with fillers, where there is no fiber pullout
witnessed in the composite. Then in the case of Figure 21(b) shows the voids, more
fiber pullout, resin- poor fiber bonding, deep resin crack, which detorite the results
on CF-1 composite considerably. The voids were measured for their size using
Image-J software, and it was noted that CF-3 showed 0.237 mm, while the CF-1
composite showed 0.513 mm.

Development of showcase using CF-3 composite and

deformation analysis using ANSYS
A showcase stand was developed using the best performer CF-3 composite as
shown in Figure 22(a). In order to predict the deformation of the developed
CF-3 laminate before the manufacture of the showcase, deformation analysis
was carried out using ANSYS R 15. The prediction was made for three loading
conditions (0.25 kg, 0.5 kg and 1 kg), respectively, on each rack. In order to perform
28 Journal of Industrial Textiles 0(0)

Figure 21. (a) SEM image of impact tested CF-3 composites showing the voids; (b) SEM image
of impact tested CF-1 composites showing voids and other characteristics which resulted in poor
strength.

Figure 22. (a) Showcase developed using JC-3 composites with things placed weighing 0.25 kg
per rack. (b) Deformation analysis done for showcase with 0.25 kg load per rack. (c) Deformation
analysis done for showcase with 0.5 kg load per rack and (d) Deformation analysis done for
showcase with 1 kg load per rack.
Kumaran et al. 29

a deformation analysis, the ANSYS R-15.0 software was used. The 3D model was
developed using CREO Parametric and was exported to the ANSYS R15 in IGES
format [53]. The material library was developed using the material properties
obtained from the experimental results with ultimate tensile strength 55 MPa,
ultimate flexural strength 5.45 MPa, ultimate compressive strength 93 MPa, hard-
ness 67 and Poisson’s ratio of 0.3. The model developed is considered as a single
homogenous mathematical model. So that the 3D model posses the same material
property throughout the model [54]. The mesh chosen was tetrahedron which
produced 32,881 nodes and 16,174 elements. Then, the discretized model was sub-
jected to total deformation. At 0.25 kg load per rack showed 0.098484 mm, and
0.5 kg load per rack showed 0.19697 mm, while 1 kg load per rack showed
0.39393 mm distortion as shown in Figure 22(b) to (d), respectively. The reduced
deformation is mainly due to the load-withstanding nature of the composite as
explained in the previous sections.
The scope of the future study is to study the effect of moisture and biodegrad-
ation of the developed composites. Also, many more applications can be made like
laptop stand, tray, ceilings etc., which could be analyzed further. The crab shell
filler can also be compared with other fillers.

Conclusions
In the present research work, jute fabrics reinforced epoxy composites were devel-
oped with and without the incorporation of solid seafood waste untreated and
treated Portunus sanguinolentus shell powder by using the hand lay-up process.
Based on the results obtained from this research work, the following conclusions
can be drawn:

. The 10 wt% treated Portunus sanguinolentus shell powder-filled jute fabrics-

epoxy composites showed enhanced tensile, flexural, compressive, shear,
impact and hardness properties due to its rough structure leading to percolation
of the matrix, i.e. better matrix-filler interaction, void filling nature.
. The thermal stability of the treated Portunus sanguinolentus shell powder-filled
jute fabrics-epoxy composites were also higher due to the presence of calcium
carbonate (i.e. chitosan) without the protein contents.
. SEM analysis visualized the defects such as the voids, fiber pullout, matrix-filler
interaction, fiber tears, crazing, pinning of cracks etc. for the different mechan-
ical properties.
. A showcase developed using best mechanical performer composite showed less
deformation proving its better strength in nature.

Overall, 10 wt%-treated Portunus sanguinolentus shell powder-filled jute fabrics-

epoxy composites showed superior results when compared to the other two com-
posites. This research will be a positive solution to reduce the solid waste landfills
produced by Portunus sanguinolentus shells after food consumption and also
30 Journal of Industrial Textiles 0(0)

composite could be beneficially used in lightweight applications since these results

further enhance the strength of the natural fiber composites.

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, author-
ship, and/or publication of this article.

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

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