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polyester composite: Water absorption, DOI: 10.1177/0021998318780227
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static and dynamic mechanical properties

MK Gupta and Rohit Singh

Abstract
In the present work, a novel physical treatment (PLA coating) of sisal fibres and its influence on the water absorption,
static and dynamic mechanical properties of its composites has been presented. The treated sisal fibres were used
consisted of alkali treatment and PLA coating to fabricate its polyester-based composites by hand lay-up technique
keeping constant fibres content as 20 wt.% . Water absorption analysis was carried out in terms of water uptake (%), and
sorption, diffusion and permeability coefficient. In addition, static properties were examined in terms of tensile, flexural
and impact test, and dynamic mechanical analysis was performed in terms of storage modulus ðE0 Þ, loss modulus ðE00 Þ,
damping ðTanÞ and glass transition temperature ðTg Þ. It was reported that the PLA-coated sisal composites showed the
best performance in water absorption, mechanical and dynamic mechanical properties than pure sisal and alkali-treated
sisal composites. There were 33%, 49%, 48%, and 27% improvement in water resistance, tensile strength, flexural
strength and impact strength, respectively, of PLA-coated sisal composites as compared to that of pure sisal composite.

Keywords
Sisal composite, PLA coating, water absorption properties, mechanical properties, dynamic mechanical properties

exhibited better mechanical and thermal properties.

Introduction
In the last 30 years, tremendous interest has been
shown in natural fibres by the researchers to develop
its polymer-based composites owing to its benefits such
as abundant, low cost, low density, and high specific
strength and modulus.1–5 Moreover, these fibres also
offer advantages such as less wear and tear, recyclability,
non-corrosiveness and biodegradability.6–10 However,
these fibres have some disadvantages also such as
higher water absorption, lower strength and poor com-
patibility.11–14 Therefore, researchers have challenges to
minimize these disadvantages of natural fibres.
Many attempts have been carried out to improve the
interfacial adhesion between natural fibres and polymer
matrix by various chemical treatments. The main effect
of these chemical treatments is to decrease the surface
polarity of the natural fibres in order to increase
the interfacial adhesion with polymer matrix.
Arthanarieswaran et al.15 examined the effect of alkali
treatment on mechanical and thermal properties of
epoxy-based acacia leucophoea fibre-reinforced com-
posite. They prepared the composites by hand lay-up
method using 5% NaOH-treated fibres. It was observed
that the composites embedded with treated fibres
El-Abbassi et al.16 studied the effect of alkali treatment
on mechanical properties of alfa fibre-reinforced poly-
propylene composite and obtained that the mechanical
properties of alfa composites were found to increase
after the alkali treatments. Gupta and Gond17 investi-
gated the effect of concentrations of alkali treatment on
the mechanical and dynamic mechanical properties of
polyester-based hemp composites. It was concluded
that the mechanical and dynamic mechanical properties
were enhanced due to the alkali treatment up to 5%
and then declined.
A new approach, using of coated fibres, was used
by a few researchers to improve the fibres–matrix inter-
facial adhesion. Rodriguez and Francucci18 examined
the effect of reinforcement of PHB-coated jute fibres
into vinyl ester polymer matrix. It was reported that
the PHB-coated composites gave the best performance
Department of Mechanical Engineering, Motilal Nehru National Institute
of Technology Allahabad, Allahabad, India
Corresponding author:
MK Gupta, Motilal Nehru National Institute of Technology Allahabad,
Allahabad-211004, India.
Email: mkgupta@mnnit.ac.in; mnnit.manoj@gmail.com
2 Journal of Composite Materials 0(0)
in terms of decrease in water absorption properties and
increase in mechanical properties. Foruzanmehr et al.19
reported the study on effect of tunable amphiphilic
nano-TiO2 coating on flax fibres and observed that
the coating had significantly enhanced the mechanical
properties. Du et al.20 investigated the tensile and flex-
ural properties of graphene oxide (GO) coated-glass
fibre-reinforced polyethersulfone composites and
found an improvement in these properties due to the
enhanced interfacial adhesion between fibres and
matrix because of the GO coating.
Many efforts had been already made to overcome
the limitations of polymer-based natural fibres compos-
ites. In the present investigation, a new approach of
physical treatment as using of PLA-coated fibres has
been presented. PLA-coated sisal fibres were incorpo-
rated into the polyester resin to make the composites.
PLA was used to make reinforcement complete bio-
degradable, as PLA is itself biodegradable. PLA has
good mechanical properties and ease in processing,
and can be obtained from the fermentation of potato,
sugar beet, corn and other agricultural materials.
Treated and untreated sisal composites were prepared
using the hand lay-up technique followed by static com-
pression in order to study its water absorption, mech-
anical and dynamic mechanical properties.
Materials and methods
Materials
Sisal fibres were purchased from Uttarakhand Bamboo
and Fibre Development Board, Dehradun, India.
Unsaturated polyester resin and its hardener were pur-
chased from the Technopal Polychem Private Limited,
New Delhi, India. The physical and mechanical proper-
ties, and chemical composition of sisal fibre are given in
Table 1.21
Table 1. Physical and mechanical properties, and chemical
composition of sisal fibre.
Properties Values
3
Density (g/m ) 1.5
Diameter (mm) 50–200
Elongation at break (%) 2–2.5
Tensile strength (MPa) 511–700
Young’s modulus (GPa) 9.4–22
Cellulose (%) 65
Lignin (%) 9.9
Microfibrillar angle 22
Wax (%) 2%
Hemi-cellulose (%) 22
Alkali treatment
The sisal fibres were immersed in 5% NaOH solution at
30 C for 30 min. The fibres were then washed several
times with distilled water followed by immersion of
these fibres in very dilute HCl solution in order to
remove the NaOH adhering from the surface of the
fibres. Finally, the fibres were again washed several
times with distilled water and then dried in a hot air
oven maintained at 70 C for 24 h.
PLA coating of fibres
Initially, PLA pellets were immerged into the chloro-
form solution for 8 h. Subsequently, the solution was
stirred manually and heated to 60 C to make sure the
uniform dispersion of PLA into chloroform solution.
After making PLA solvent, sisal fibres were dipped and
then taken out after 5 min soaking time. Finally, coated
fibres were dried at room temperature for 24 h and then
finally dried at 40 C for 6 h in a hot air oven.
Fabrication method
Initially, PLA-coated sisal fibres were cut into 10 mm
size, and then reinforced into unsaturated polyester
resin for fabrication of the composites. The composites
were fabricated by the hand lay-up technique followed
by the static compression keeping constant 20 wt.% of
sisal fibres content in each composite. Polyester resin
was mixed with hardener to prepare the matrix. The
mixture was stirred thoroughly to ensure consistent
mixing. A stainless steel mould having dimensions of
300 mm  200 mm  3 mm was used to make the 3 mm
thickness of laminates. Silicon spray was used to facili-
tate the easy removal of the composites from the mould
after curing. The cast of each composite was cured
under a load of 50 kg for 24 h before it was removed
from the mould. Specimens were cut in proper dimen-
sions as per ASTM standard using a diamond cutter
subjected to analysis of water absorption, static and
dynamic mechanical properties. The notations of pre-
pared composites are given in Table 2.
Water absorption behaviour
Water absorption behaviour of sisal composites was
investigated according to ASTM D 570. The specimens
were immerged in the distilled water at 30 C to study
the kinetics of water absorption behaviour. The sam-
ples were taken out periodically and weighed immedi-
ately, after wiping off the water particles from the
surface of the specimen using a dry and clean cotton
cloth. The weight of the sample before and after
absorption was found out using an electronic balance
with an accuracy of 104 g. The percentage of water
Gupta and Singh
Table 2. Notations of treated and untreated sisal composites.
Symbol Composites
SC Untreated sisal fibre-reinforced polyester composite
SC (NaOH) NaOH-treated sisal fibre-reinforced polyester composite
SC(PLA) PLA-coated sisal fibre-reinforced polyester composite
absorption was calculated using the following
equation22
w2  w1
Water absorptionð%Þ ¼  100
w1
where w1 ¼ weight before soaking into water (g) and
W2 ¼ weight after soaking into water (g).
At several periods of time, the water absorption (%)
was calculated and then plotted against square root of
immersion time to calculate the diffusion coefficient.
Diffusion coefficient is calculated from the slope of
curve between water absorption (%) and square root
of immersion time using the following equation22
 2 2 
t m
Diffusion coefficient ðDÞ ¼  2
16W1
where m is the slope of linear portion of the sorption
curve and t is the initial sample thickness in (mm).
In addition, sorption coefficients that are related to
the equilibrium sorption was calculated as follows
Sorption coefficient S ¼ W1 =Wt
where W1 and Wt are percentage of water uptake at
saturation stage and at time t.
The permeability coefficient that is net effect of
sorption and diffusion coefficient was calculated as
follows22
Permeability coefficient P ¼ D  S
Tensile test
Tensile test of the composite samples was performed on
Tinius Olsen H 10 K-L (Bi-axial testing machine) with a
crosshead speed of 2 mm/min. Tests were conducted
according to ASTM D638 with dimensions of
165 mm  20 mm  3 mm. Five specimens of each com-
posite were tested and their average values and stand-
ard deviations are reported.
3
Wt.% (sisal fibres/polyester) Wt.% (treatment)
S20/P80 0
S20/P80 5 (NaOH)
S20/P80 5 (PLA)
Flexural test
Flexural test of the composite was carried out using a
three point bending test on Tinius Olsen H10 K-L
ð1Þ
(Bi-axial testing machine). Samples for the flexural
test were prepared in dimensions of 80 mm 
12.7 mm  3 mm as per ASTM D790. The flexural
test was carried out at room temperature with the cross-
head speed of 2 mm/min. Flexural strength and flexural
modulus were calculated as follows
3FL mL3
Flexural strength ¼ and Flexural modulus ¼
2bd 2 4bd 3
ð5Þ
where F is the ultimate failure load (N), L is the span
ð2Þ length (mm), b and d are the width and thickness of
specimen in (mm), respectively, and m is the slope of the
tangent to initial line portion of the load–displacement
curve. Five specimens of each composite were tested
and their average values and standard deviations are
reported.
Impact test
ð3Þ
Izod impact test of composite samples was performed
on Tinius Olsen Impact 104 machine. Samples for the
impact test were prepared in dimensions of 65 mm 
12.7 mm  3 mm with 2.5 mm notch thickness as per
ASTM D 256. Five specimens of each composite were
tested and their average values and standard deviations
are reported.
ð4Þ
Dynamic mechanical analysis
The dynamic mechanical properties of sisal composites
were studied using the dynamic mechanical analyser
(Seiko instruments DMA 6100). The dynamic mechan-
ical properties were carried out using three point bend-
ing test as a function of temperature. The laminates
were cut into samples with dimensions of 50 mm 
13 mm  3 mm as per ASTM D 5023. Experiments
were carried out at 5 Hz frequency within the tempera-
ture range of 30–200 C in order to study E0 , E00 , Tan
and Tg .
4 Journal of Composite Materials 0(0)

Results and discussion
Water absorption behaviour
Natural fibres show the tendency of water absorption
when immersed into water. It occurs because of its
hydrophilic nature due to the presence of hydroxyl
group. In case of natural fibre-reinforced polymer com-
posites, water absorption behaviour depends upon dif-
fusion of water molecules into micro gaps of polymer
chain and interface between fibres and matrix.
Moreover, it also depends upon propagation of micro
cracks due to the swelling of fibres.23
The water absorption (%) of pure sisal composite
(SC), alkali-treated sisal composites SC(NaOH) and
PLA-treated sisal composites SC(PLA) is plotted
against the square root of time as shown in Figure 1.
It can be seen that the initial rate of water absorption
was linear for all the three composites. After extending
the immersion time, percentage of water absorption
slows down and then approaches to saturation stages.
Therefore, for all sisal composites, behaviour of water
absorption could be considered as Fickian diffusion
process. It was observed that both treatments (alkali
and PLA coating) were effective in decreasing the
7 composites that results in higher resistance to diffusion
SC(PLA)
6 SC(NaOH)
SC
5
Water absorpon (%)
water absorption when compared with SC. The max-
imum value of water absorption at saturation stage was
found for SC followed by SC(NaOH) and SC(PLA).
The maximum water absorption of SC may be due to
the hydrophilic nature of sisal fibres due to the presence
of hydroxyl groups. Alkali-treated sisal composite has
the better water absorption resistance than SC. This
happening could be due to the removal of hemicellu-
loses and lignin from the surface of fibres due to alkali
treatment.24–26 Moreover, it was also confirmed that
the hydrophilic nature of natural fibres turn into hydro-
phobic nature by the alkali treatments as results
decrease in water absorption behaviour.27 SC(PLA)
has the best resistance to water absorption than those
of the composites SC and SC(NaOH) as PLA coating
keeps sisal fibres isolated from the water being
absorbed which results in decreased water absorption.
Furthermore, diffusion coefficient, sorption coeffi-
cient and permeability coefficient were also investigated
for treated and untreated sisal composites, and these
results are summarized in Table 3. Diffusion coefficients
were found in linear relationship with water uptake by
composites. The lowest value of diffusion coefficient
was observed for SC(PLA) followed by SC(NaOH)
and SC. The SC(PLA) has the lowest value of diffusion
coefficient because of the minimum voids present in
of water molecules into these voids. Permeability coef-
ficient followed the same trend like diffusion coefficient.
But sorption coefficient followed the reverse trend of

diffusion coefficient and permeability coefficient. The

4
higher value of sorption coefficient was seen for
SC(PLA) followed by SC and SC(NaOH).
3

2
Tensile properties
Tensile strength and tensile modulus of untreated and
1 treated sisal composites are given in Table 4, and cor-
responding data are plotted in Figure 2. It was observed
0
0 200 400 600 800 1000 1200
that both treated sisal composites have higher values of
Square root of me (√sec)
tensile strength and tensile modulus than untreated sisal
composites. The tensile strength and tensile modulus of
Figure 1. Water absorption (%) versus square root of time SC(NaOH) were observed to be 34.57 MPa and
graph of treated and untreated sisal composites. 2.11 GPa, respectively, which are 40% and 49%,

Table 3. Sorption, diffusion and permeability coefficient of treated and untreated sisal composites.

Percentages of Diffusion Permeability

water uptake at Sorption coefficient D coefficient P
Composites saturation stage coefficient S (mm2/s) (mm2/s)

SC 5.66 3.25 3.863E-6 1.256E-5

SC (NaOH) 4.74 3 4.542E-6 1.362E-5
SC (PLA) 3.8 4.75 1.778E-6 8.525E-6
Gupta and Singh 5

Table 4. Mechanical properties of treated and untreated sisal composites.

Tensile Tensile Flexural Flexural Impact

Composites strength (MPa) modulus (GPa) strength (MPa) modulus (GPa) Strength (kJ/m2)

SC 24.71  1.67 1.42  0.08 55.12  3.31 2.24  0.17 20.22  1.47
SC (NaOH) 34.57  2.01 2.11  0.07 72.70  4.45 3.52  0.20 23.55  1.98
SC (PLA) 36.78  2.21 2.32  0.15 81.33  5.45 3.67  0.22 25.75  2.01

40 3 100 5
90
80 4

Flexural strength (MPa)

Flexural modulus (GPa)

30
Tensile strength (MPa)

Tensile modulus (GPa)

70
2
60 3

20 50
40 2
1 30
10 20 Flexural strength 1
Tensile Strength
10 Flexural modulus
Tensile Modulus
0 0
0 0 SC SC (NaOH) SC(PLA)
SC SC (NaOH) SC(PLA)
Figure 3. Flexural strength and flexural modulus of treated and
Figure 2. Tensile strength and tensile modulus of treated and
untreated sisal composites.
untreated sisal composites.

respectively, higher than SC. A similar type of result as 30

improvement in tensile properties due to the alkali
treatment had been already reported in the past litera- 25
ture.28–30 The improved tensile properties in alkali-trea-
(kJ/mm2)

ted composite may be due to the increase in surface 20

roughness of fibres by removal of hemicelluloses and
Impact strength

lignin results improved interfacial adhesion between 15

fibres and matrix. Furthermore, it can be also observed
that SC(PLA) exhibits better performance in terms of
10
tensile strength and tensile modulus than those of com-
posites SC(NaOH) and SC. PLA-coated composite
5
SC(PLA) has the maximum tensile strength
Impact strength
(36.78 MPa) and tensile modulus (2.72 GPa), which
are 6% and 10%, respectively, higher than that of 0
SC SC (NaOH) SC(PLA)
SC(NaOH). The maximum values of tensile strength
and tensile modulus possess by SC(PLA) can be Figure 4. Impact strength of treated and untreated sisal
explained, as natural fibre-reinforced polymer compos- composites.
ites have poor interfacial adhesion due to the
interaction of polar natural fibres and non-polar poly-
mer matrix.13 After coating of polymers on natural corresponding data are plotted in Figure 3. A similar
fibres, they partially behaves like non polar and pro- trend like tensile test was noticed for flexural tests in
vides better interfacial adhesion between fibres terms of strength and modulus. It was observed that
and polymeric matrix as results increase in tensile both treated sisal composites have the higher values
properties. of flexural strength and flexural modulus than that of
the untreated sisal composites, which shows a positive
effect of treatments. The flexural strength and flexural
Flexural properties
modulus of SC(NaOH) were observed to be 72.70 MPa
Table 4 shows the flexural strength and flexural modu- and 3.52 GPa, respectively, which are 32% and 57%,
lus of untreated and treated sisal composites, and respectively, higher than that of SC. This could be
6 Journal of Composite Materials 0(0)
because of improved wet ability and better interfacial
bonding between fibres and matrix.29 In addition, it can
be also observed that coated composites exhibited
better flexural performance than alkali-treated compos-
ite as well as untreated sisal composite. The flexural
strength and flexural modulus of SC(PLA) were
observed to be 81.33 MPa and 3.67 GPa, respectively,
which are 12% and 4%, respectively, higher than that
of SC(NaOH) .
Impact properties
Table 4 shows the impact strength of untreated and
treated sisal composites, and corresponding data are
plotted in Figure 4. Similar trend like tensile and flex-
ural test was found for the impact test also. In case of
impact test, it was also observed that both treated sisal
composites have the higher values of impact strength
than untreated sisal composites. The impact strength
of SC(NaOH) was observed to be 23.55 kJ/mm2
which is 16% higher than that of SC. The composite
SC(PLA) has the highest value of impact strength
(25.75 kJ/mm2), which is more than 9% and 27%
than those of composites SC(NaOH) and SC, respect-
ively. The reason may be due to the enhancement in
stiffness of fibres, and adhesion between fibres and
matrix by PLA coating that increases the capability
of sisal composites to absorb more energy as well as
to resist crack transmission.
Storage modulus
Storage modulus gives an estimate of temperature-
dependant stiffness behaviour and load-bearing cap-
ability of the composite material.31 Figure 5 shows
the variation of the storage modulus of untreated and
treated sisal composites as a function of temperature at
1200
SC(PLA)
1000 SC(NaOH)
Storage modulus (MPa)
SC
800
600
400
200
0 0
30 80 130
Temperature (°C)
Figure 5. Variation in storage modulus with temperature of
treated and untreated sisal composites.
5 Hz frequency. It was interesting to notice that both
treated sisal composites have the higher values of stor-
age modulus than untreated sisal composites in glassy
region. The maximum value of storage modulus found
for PLA-coated sisal composite SC(PLA) was followed
by SC(NaOH) and SC. In all cases, the storage modu-
lus of the composites was found to be decreased as the
temperature increased, probably due to the loss in stiff-
ness of fibres.32 Similar types of results were earlier
reported by many researchers.9,33–35 In transition
region, there was a gradual fall in the value of E0
when temperature was increased as shown in
Figure 5. In the rubbery region, SC(PLA) has the high-
est value of storage modulus followed by SC(NaOH)
and SC. This might be due to the increase in stiffness of
fibres due to PLA coating.
Loss modulus
Loss modulus represents the viscous response of the
materials. The peak of loss modulus curve of polymer
material is known as dynamic glass transition tempera-
ture. The glass transition temperature can be obtained
from the peak of either E00 or Tan curve. The variation
of the loss modulus as a function of temperature at 5 Hz
frequency is shown in Figure 6. On increasing the tem-
perature, the value of E00 was found to be increased up
to glass transition temperature and then decreased. The
increase in peaks of loss modulus follows the order:
SC(PLA) > SC(NaOH) > SC. From the loss modulus
curve, the higher value of Tg was found for the com-
posite SC(PLA) due to the incorporation of PLA-
coated sisal fibres which caused decrease in the mobility
of polyester resin. The values of glass transition tem-
peratures for sisal composites obtained from the peak
of loss modulus curve are given in Table 5.
140
SC(PLA)
120
SC(NaOH)
Loss modulus (MPa)
100
SC
80
60
40
20
180 30 80 130 180
Temperature (°C)
Figure 6. Variation in loss modulus with temperature of
treated and untreated sisal composites.
Gupta and Singh 7

0.4 obtained from the present study, the following conclu-

SC(PLA)
0.35 sions can be drawn:
SC(NaOH)
0.3
SC . Both treatments (alkali and PLA coating) showed
0.25 better performance in terms of water absorption
Tanδ

0.2 resistance, and mechanical and dynamic mechanical

0.15 properties as compared to untreated sisal composite.
. PLA-coated sisal composite had the best mechanical
0.1
performance than those of alkali-treated composite
0.05 and pure sisal composite.
0 . The maximum water absorption resistance was
30 50 70 90 110 130 150 shown by PLA-coated sisal composite followed by
Temperature (°C) alkali-treated sisal composite and pure sisal
composite.
Figure 7. Variation in Tan d with temperature of treated and . Dynamic mechanical properties such as storage
untreated sisal composites. modulus, loss modulus and glass transition tempera-
ture were shown maximum by PLA-coated sisal
composite.
Table 5. The values of peak heights and Tg from loss modulus
and tan delta curve.
Declaration of Conflicting Interests
Peak height Tgð CÞ The author(s) declared no potential conflicts of interest with
of loss Peak height from loss Tgð CÞ respect to the research, authorship, and/or publication of this
modulus of tan modulus from tan article
Composites Curve (MPa) delta curve curve delta curve

SC 100.64 0.357 68.86 82.78 Funding

SC (NaOH) 104.50 0.278 64.81
SC (PLA) 123.80 0.297 72.25
Damping
Damping or Tan is the ratio of the loss modulus to the
storage modulus. It depends upon fibre–matrix adhe-
sion, and strength and stiffness of fibres.6 Weak fibre–
matrix adhesion shows the higher value of Tan and
vice-versa.6 The effect of Tan on sisal composites as
a function of temperature is shown in Figure 7. The
increase in peaks of Tan follows the order:
SC > SC(NaOH) > SC(PLA). The values of Tan
peaks and Tg for sisal composites are given in
Table 5. It was observed that SC(PLA) has the
lowest peak of Tan curve, which shows lower damping
results improvement in load-bearing capacity. This
trend can be explained, as coated fibres exhibit
improved fibre matrix adhesion that restrict the move-
ment of polymer chain, thus improved load-bearing
capacity.
Conclusions
Effects of physical and chemical treatments on water
absorption, mechanical and dynamic mechanical prop-
erties of polyester based sisal composites have been
experimentally carried out. Based on the results
85.73 The author(s) disclosed receipt of the following financial sup-
89.18 port for the research, authorship, and/or publication of this
article: The authors would like to thank the Head of
Mechanical Engineering Department of Motilal Nehru
National Institute of Technology Allahabad-India for their
support in allowing them to perform the tests in Materials
Characterization Lab. The study is supported by Cumulative
Professional Development Allowances (CPDA) and R & C
fund for teachers of Motilal Nehru National Institute of
Technology Allahabad-India.
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