Received: 3 January 2021 Revised: 30 April 2021 Accepted: 30 May 2021

DOI: 10.1002/pc.26164

RESEARCH ARTICLE

Investigation of the effect of water absorption

on thermomechanical and viscoelastic properties
of flax-hemp-reinforced hybrid composite

Abir Saha1 | Santosh Kumar2 | Divya Zindani3

1
Department of Mechanical Engineering, Indian Institute of Technology Guwahati, Guwahati, Assam, India
2
Department of Mechanical Engineering, National Institute of Technology Silchar, Silchar, Assam, India
3
Department of Mechanical Engineering, Sri Sivasubramaniya Nadar (SSN) College of Engineering, Kalavakkam, Tamil Nadu, India

Correspondence
Abir Saha, Research Scholar, Indian
Institute of Technology Guwahati,
Guwahati, Assam, India.
Email: abir2016saha@gmail.com
Abstract
The recent development of natural fiber-reinforced polymer composites have
shown innumerable economic and environmental benefits for a vast array of
engineering applications. It is quintessential to investigate the effect of water
absorption on the composites that remain in the water for a maximum of their
intended service period. This study is an effort in this direction that investi-
gates the effect of water absorption on thermo-mechanical properties of flax-
hemp-reinforced epoxy composites fabricated using compression hand layup
technique with different weight fraction of fiber. The fabricated composites
have been characterized physically (density and water absorption), thermo-
mechanically (tensile, flexural, thermal conductivity, and dynamical mechani-
cal analysis), and morphologically (scanning electron microscopy [SEM]). The
analysis revealed that hemp-reinforced composites (S1) had the highest water
absorption capabilities in comparison to the flax-reinforced composites (S5).
Higher water absorption capability had an adverse effect on the mechanical
properties of fabricated composites. However, hybrid composites (S2, S3, and
S4) reported better performance with regard to S1. The increased water con-
tent, however, increased the thermal conductivity of composites and maximum
has been revealed for S1 (0.82 W/mK) and minimum for S5 (0.48 W/mK). The
water molecules showed detrimental effects on the viscoelastic properties and
revealed S3 have better interlocking bond with the lowest reduction in storage
modulus (12%) and glass transition temperature (4
C) in comparison to S1
(30%) under wet conditions. A comparative analysis of the thermo-mechanical
properties was also made for developed composites under dry, saturated, and
re-dried conditions. The SEM has been used to characterize the morphological
and fracture behavior of the fabricated composites under the influence of water
uptake. The effects of water molecules on the hygrothermal aging index and
diffusion co-efficient have also been discussed. Overall, the hybridization of

Polymer Composites. 2021;1–20. wileyonlinelibrary.com/journal/pc © 2021 Society of Plastics Engineers. 1

2 SAHA ET AL.
flax with hemp fiber showed better results over the hemp fiber-reinforced com-
posites (S1).
KEYWORDS
flax fiber, hemp fiber, hybrid composites, mechanical properties, viscoelastic properties,
water absorption
1 | INTRODUCTION
Fiber-reinforced composites have gained a wide range of
acceptance in the different industrial domain as such
automotive, marine, and aerospace.1,2 This is owing to
the flexibility that they offer to tailor the mechanical
properties as per the design requirements. Numerous
reinforcements have been used in composite materials.
Glass fibers are one of the commonly employed rein-
forcing agents in such composites. However, these fibers
possess major health concerns with high energy con-
sumption and therefore are being replaced with cellulosic
fibers.
There has been an exponential rise in natural fiber-
reinforced composites owing to the environmental sus-
tainability provided by the natural fiber over their syn-
thetic counterpart. The other benefits have
biodegradability, renewability, low energy consumption,
lightweight, etc.3–6 However, these composites suffer
from certain challenges as such incompatibility with
matrix, high sensitivity to moisture, low strength, etc.7,8
The water absorption of composites affects the mechani-
cal and viscoelastic properties that showed degradation
effects of water molecules on composites.9–11 Hence, it
becomes quintessential to address the aforementioned
challenges by altering the structure of the fiber so that
reduction in moisture content could be achieved and
hence high thermo-mechanical have sustained. Hybridi-
zation is another probable approach to improvise the
moisture uptake and hence achieve high mechanical and
viscoelastic properties of the natural fiber-reinforced
composites.
The hybridization process involves including two or
more than two types of natural fiber in a matrix.12 The
hybrid polymeric composites have been revealed to be
superior in properties to the nonhybrid composites.13,14
The hybridization effect has a positive effect on the
thermo-mechanical properties of the resulting compos-
ites. Moreover, the sensitivity associated with the mois-
ture uptake is also reduced. Hybridization with two or
more natural fibers is more environmentally stable in
comparison to the hybridization with the synthetic coun-
terpart. An array of research studies has been carried out
on mechanical properties as well as water absorption
capability of hybrid composites. Sanjay et al.15 studied
the mechanical properties of kenaf, jute, and glass fiber-
reinforced polymeric composites and the study revealed
high mechanical properties as a result of hybridization
with high strength fiber. The mechanical properties and
water absorption behavior of fiber-reinforced composites
from kenaf/jute/hemp and kenaf/pineapple were studied
by Maslinda et al.16 and Feng et al.17 The study reported
enhancement in mechanical properties as well as the
water uptake of the proposed composite system. Yet
another study conducted on hybridization effect by Sekar
et al.18 and Hamdan et al.,19 where effects of water
absorption of natural fiber epoxy composite on mechani-
cal properties were studied. The results revealed
improved mechanical properties and reduced water
absorption effects in comparison to the nonhybrid epoxy
composites derived from a single fiber. The water absorp-
tion behavior for banana- and sisal-reinforced hybrid
polymeric composites was investigated by Badyankal
et al.20 It was reported that the hybrid composites com-
prising 10 wt% banana and 30% sisal has the minimum
water absorption capacity. An investigation into water
uptake of kenaf- and pineapple-reinforced polymeric
composites was carried out by Feng et al.21 The superior-
ity of hybrid composites consisting the kenaf and pineap-
ple in 25:75 was revealed over the nonhybrid kenaf-based
polymeric composites. Ganesh et al.22 investigated the
water uptake behavior for Areca-sheath and palm leaf
sheath fiber-reinforced polymeric composites. The hybrid
composites made from skin layers of areca sheath and
core layer of palm leaf sheath fibers were revealed to
exhibit minimum water uptake characteristics in compar-
ison to the other considered configurations. The water
absorption behavior for Aloe vera, flax, and barium sul-
fate hybrid composites was examined by Arulmurugan
et al.23 The addition of barium sulfate on the hybrid poly-
meric composites was revealed to have a positive effect
on their water uptake behavior. Chandramohan et al.24
investigated the water absorption behavior for jute/Aloe
vera hybrid natural fiber polymeric composites and supe-
riority of the hybrid composites was revealed over the
nonhybrid composites.
Dynamic mechanical behavior is the essential param-
eters to measure the viscoelastic properties of the fiber-
SAHA ET AL.
reinforced polymer composites (FRPC). Duc et al.25
investigated the viscoelastic properties and compared
these damping properties with several fiber- (carbon,
glass, and flax fiber) reinforced composites. The results
showed that adding unidirectional flax fiber to the poly-
mer enhances the damping and loss factor of the devel-
oped composites. Cheour et al.26 studied the effects of
water uptake on damping and revealed that loss modulus
and damping factor of FRPC increases with an increase in
immersion time. Berges et al.27 reported that water aging
has a diverse effect on storage modulus and significant dec-
rement in the storage modulus is observed up to the satu-
rated points. Wang et al.28,29 reported the mechanical and
viscoelastic properties under hygrothermal aging and the
transfer process of water molecules with the Fickiam diffu-
sion model was discussed. The results showed that the dif-
fusion coefficient increased with water uptake and elevated
water temperature.
From the aforementioned literature survey, it is evi-
dent that several studies have been performed on the
investigation of water absorption behavior for natural
fiber-based hybrid composites. However, the effects of
hygrothermal aging and water uptake on mechanical
properties, thermal properties, and damping behavior
remain an open and emerging field for researchers where
very little work has been done so far. Hence, the present
study provides a novel contribution to the scientific com-
munity by investigating the effect of water absorption
behavior on the thermo-mechanical properties of hemp/
flax-reinforced epoxy composites.
2 | MATERIALS AND METHODS
2.1 | Materials
Materials have been selected based on their superior
properties. In the present work, Epoxy LY-556 and curing
agent hardener HY-951 are used as matrix material. It is
a thermosetting polymer which has bonding properties
with fibers with easy to cure at room temperature. Epoxy
resin and hardener were mixed in a ratio of 10:1 at room
temperature (as per the recommendation of the polymer
manufacturing company). Epoxy resin LY-556 was cho-
sen because the density of the resin is much closer to that
of the employed fiber densities. This allows for better
bonding between the selected fibers and the epoxy resin.
The chemical name of the selected epoxy resin is
diglycidal ether of bisphenolA and that for the hardener
is triethylenetetramine.
Hemp fiber and Flax fiber have been selected as rein-
forcing materials. Hemp fiber has a better crystallinity
index that results in better insulating properties and
3
thermal conductivity.30,31 Flax fiber has been selected
because of its superior mechanical properties and water
absorption capacity that allows for higher energy absorp-
tion capacity.32,33 Hemp fiber has been sourced from
Vruksha Composites & Services, Andhra Pradesh, India.
Hemp fiber is extracted from the bust of the hemp tree.
The scientific name of the hemp tree is Cannabis sativa.
Flax fiber is imported from Go Green Product, Chennai
India and is extracted from the basting of flax tree. The
scientific name of the flax tree is Linum usitatissimum.
Properties of fibers and epoxy34 are depicted in Table 1.
2.2 | Fiber processing
The selected fibers are cut to the desired length of 15–
20 cm for fabricating the composite specimens. The cut-
out fibers were soaked in water for 24 h, which can help
in eliminating the foreign impurities from the fiber. After
that, the soaked fibers are dried in an open atmosphere
for 24 h to remove moisture and other foul gases. After
drying in an open atmosphere, the fibers are further dried
inside an oven at 90
C for 6 h.35 The chemical composi-
tion of the hemp and flax fiber have been depicted in
Figure 1.
2.3 | Composite fabrication
The compression hand layup technique has been used to
fabricate the different composite specimen. During trial
experimentation, hemp and flax fiber-reinforced compos-
ites were fabricated separately with different weight frac-
tion of the respective fibers (10%, 20%, 30%, and 40%).
The fibers were distributed unidirectionally for the fabri-
cation of composite specimen. The fabricated composite
specimens were tested for their mechanical properties
that is, tensile and flexural properties. The experiment
results revealed that the composite specimens with a 30%
weight fraction of fiber had the highest mechanical prop-
erties. On the other hand, the composite specimens with
40% of fiber loading had the minimum mechanical prop-
erties of the considered compositions. A similar type of
decrement was reported by Komal et. al36 for banana
fiber and Feng et. al17 a Pineapple and Kenaf fiber.16
As a result of the findings from the trial experimenta-
tion runs, the hybrid composite specimens were fabri-
cated using a 30% weight fraction of fibers. The
composites specimens have been prepared with five dif-
ferent compositions of hemp and flax fiber. The composi-
tions and sample code are shown in Table 2. The
different weight fraction of flax/hemp (shown in Table 2)
is reinforced unidirectionally with epoxy resin and
 4

TABLE 1 Properties of epoxy and fibers16,32,34

Sl. No. Materials Properties Unit Value Standard

1 Epoxy LY-556 with hardener HY-951 Viscosity(at 25 C) mPa-s 12,000 As per technical data sheet
Visual inspection
ASTM D 638 type V
2 Density(at 25
C) g/cm3 1.15
3 Color — Clear, Pale Yellow
4 Tensile strength MPa 26 ± 3.5
5 Tensile modulus MPa 1.1 ± 0.6 ASTM D 638 type V
3
1 Hemp fiber Density g/cm 1.43 ± 0.0012 Helium pycnometer
2 Diameter μm 310–318 Stereo microscope
3 Length cm 15–16 Slide Calipash
4 Tensile strength MPa 550 ± 40 ASTM D3822-14
5 Tensile modulus GPa 7 ± 2.4 ASTM D3822-14
6 Elongation at brake % 1.6–1.8 ASTM D3822-14
3
1 Flax fiber Density g/cm 1.51 ± 0.0016 Helium pycnometer
2 Diameter μm 260–280 Stereo microscope
3 Length cm 15–16 Slide Calipash
4 Tensile strength MPa 800 ± 45 ASTM D3822-14
5 Tensile modulus GPa 10 ± 2.1 ASTM D3822-14
6 Elongation at brake % 1.2–1.3 ASTM D3822-14
SAHA ET AL.
SAHA ET AL. 5

FIGURE 1 Chemical composition of hemp fiber and flax fiber (in percentage) [Color figure can be viewed at wileyonlinelibrary.com]

TABLE 2 Sample code with fiber weight and volume fraction

Weight Volume
fraction of fraction of
fiber fiber
Sample Total weight fraction of Total volume fraction Total volume fraction
code Flax Hemp matrix (%) Flax Hemp of fiber (%) of matrix (%)
S0 0 0 100 0 0 0 100
S1 0 30 70 0 20.979 20.979 79.021
S2 10 20 70 6.667 13.986 20.653 79.347
S3 15 15 70 10 10.490 20.490 79.510
S4 20 10 70 13.333 6.993 20.326 79.674
S5 30 0 70 20 0 20 80

FIGURE 2 Fabrication method of developed composites plates [Color figure can be viewed at wileyonlinelibrary.com]
6 SAHA ET AL.
hardener solution (10:1). Mechanical stirring has been
used to properly stir the epoxy-hardener mixture. The
degasser ensures the reduction in bubble formation and
hence the defects that may arise due to improper mixing
process. The unidirectional flax/hemp fibers in desired
weight fraction were placed layer by layer on the lower
mold. The stirred and degassed matrix material was then
spread over the fiber layers with help of a roller. Roller also
aided to minimize the formation of voids that might have
arisen during the pouring process. Next, the upper mold
was placed over the lower mold containing the fibers and
matrix material. Suitable compression pressure was
maintained for 8 h at room temperature. The composite
plate bearing dimension 200 mm  200 mm  3.5 mm was
then removed from mold and post cured at 60
C for 3 h.
The cured composite plates were cut according to respective
ASTM standards as per the desired tests. The fabrication
methodology, as well as developed composite plates and
specimens, are shown in Figure 2.
3 | EXPERIMENTAL
CHARAC TERIZATION
3.1 | Physical characterization
Experimental and theoretical density has been measured of
all six types of the sample at the dry condition at room tem-
perature (23
C). Archimedes principle was used to measure
the experimental density of the composite as per ASTM D-
2734-70 (80 mm  30 mm  10 mm) standard specimen.37
To find out the experimental density, the water immersion
technique was adopted and Equation (1) was used:
mcðexpÞ
ρcðexpÞ ¼ , ð1Þ
vcðexpÞ
where ρc(exp) = experimental density of the composite, mc
(exp) = experimental mass of composite, and vc
(exp) = experimental volume of composite.
38
For calculation of theoretical density, RoM (Rule of
mixtures) for density measurement was used. RoM for
density measurement is shown in Equation (2).
ρcðtheoÞ ¼ ðvF  ρF Þ þ ðvH  ρH Þ þ ðvM  ρM Þ, ð2Þ
where vF, vH, and vM are the volume fraction of flax fiber,
hemp fiber, and matrix material, respectively. On the
other hand, ρF, ρH, and ρM are the densities of the flax
fiber, hemp fiber, and matrix material, respectively. To
measure the void content of the fabricated sample Equa-
tion (3) was used.
ρcðtheoÞ  ρcðexpÞ
Vc ¼  100, ð3Þ
ρcðtheoÞ
where Vc = void content of composite, ρc
(theo) = theoretical density of the composite, and ρc
(exp) = experimental density of the composite.
39
3.2 | Water absorption test
Natural fiber-reinforced composites are moisture sensitive
compared to their synthetic counterpart. From the applica-
tion point of view, it is very important to understand the
degree of water absorption for natural fiber-reinforced com-
posite. The water absorption experiment was carried out as
per ASTM D 570 (60 mm  60 mm  3 mm) standard.40
For the dry condition test, five samples of each group (S0, S1,
S2, S3, S4, and S5) were taken and dried at 40
C for 24 h.
Moreover, for the wet test, samples were submerged in dis-
tilled water for a different time interval (generally 24 h time
interval was taken for this test). After the completion of the
time interval, the specimens were taken out from the water.
The water on the surface of the sample was wiped out with
an absorbent lint-free cloth. The samples were then weighed
using a weighing machine having the precision of up to four
digits. Five samples of each group (S0, S1, S2, S3, S4, and S5)
were selected for water immersion and average reading was
taken for obtaining the percentage of water absorption. After
that, the specimens were immersed again in distilled water
for another 24 h and water absorption was obtained by the
difference in weight of the sample. This process was per-
formed continually until an increment in the weight of sam-
ples was revealed to be zero.
3.3 | Mechanical characterization
The fabricated composite specimens were characterized for
the mechanical properties. Tensile and flexural tests were
carried out on the samples under dry and wet conditions. For
the wet samples, the flexural and tensile tests were carried
out every 24 h of water immersion. With the continual pro-
cess of immersion of samples into the water, the wet samples
reached a saturation limit of water absorption. The samples
were then dried for 5 days at 40
C in an air oven.
The tensile tests were performed on a universal test-
ing machine (UTM), Instron 4201, with a load cell of
100 KN. The gripping capacity of the machine was
100 KN. The specimens were prepared with ASTM D-
638-3 (160 mm  14 mm  3.5 mm) standards.41 The
tests were performed on five specimens from each config-
uration at room temperature (25
C) with 50% of relative
humidity. The gauge length of the specimens was fixed to
SAHA ET AL.
60 mm and tests were conducted with a constant strain
rate of 1 mm/min.
The Flexural tests were performed on UTM, Instron
4201 with a support span of 50 mm, and a constant cross-
head speed of 1 mm/min. The specimens were prepared
with ASTM D-790-3 (130 mm  14 mm  3.5 mm) stan-
dard and five specimens of each configuration were
tested at room conditions.42
The mechanical properties such as strength, modulus,
strain, and maximum load at the break on the fabricated
composites were recorded.
3.4 | Conductivity test
Thermal Conductivity tests were performed for each dry and
wet sample. To perform a conductivity test, Unitherm Model
2022 was used. The test specimens were prepared to have
50 mm diameter and 4 mm thickness, that is, in accordance
with ASTM-E1530 standard.43 Specimens were placed
between two polished surfaces and pressure of 0.068 MPa
was applied on the top of the specimen. Thereafter, the heat
was generated with the help of power control from one side
of the test sample. The temperature on the other side of the
specimen was measured by employing a sensor. For one-
dimensional heat transfer, Equation (4) was used:
k  ΔT
q¼ , ð4Þ
L
2
where q stands for heat flux (W/m ), k is thermal conduc-
tivity (W/m-K), ΔT is temperature deference (K), and L is
the thickness (m) of the sample.
The thermal resistance of the composite sample is
given in Equation (5)
ΔT
R¼ , ð5Þ
q uted to the fact that during the fabrication of composites
Here R is the resistance (m2-K/W) between the hot and
cold surface.
By using Equations (4) and (5), one can write thermal
conductivity as Equation (6)
L specimens.
k¼ : ð6Þ
R The lumen within natural fibers acts as a void for the fab-
3.5 | Dynamic mechanical analysis
Dynamic mechanical analysis (DMA) is a mechanical
technique for measuring microscopic properties and
molecular arrangements with the influence of tempera-
ture. The dynamic mechanical properties of polymeric
7
materials are the function of frequency, temperature, and
time that measures the microscopic deformation gener-
ated from molecular rearrangements. Various properties
such as storage modulus (E´), viscous modulus (G´), and
damping factor (tanδ) have been examined during test-
ing. The samples were prepared with rectangular dimen-
sions (50 mm  13 mm  3 mm) as per ASTM D-5023
standard to characterize the viscoelastic properties of
composites and glass transition temperature (Tg).44 The
tests were performed at 1 Hz frequency under the tem-
perature range from room temperature to 200
C with a
heating rate of 3
C/min and strain amplitude of 0.1%.
3.6 | Scanning electron microscopy
Scanning electron microscopy (SEM) is the microstructure
and morphology analysis, wherein a high-energy beam of
the electron is passed with a raster scan pattern. SEM was
used to examine the morphological and fracture behavior
of the fabricated composite samples. This was done with
20–500 magnifications in a high vacuum at room tem-
perature. Since polymeric composite specimens are less
electrically conductive, the gold coating was done and
then analysis was performed with JSM-400 SEM machine.
4 | RESULTS A ND DISCUSSION
4.1 | Physical characterization
The experimental and theoretical densities of nonhybrid and
hybrid composite materials along with void content have
been determined using Archimedes principle and results are
presented in Table 3. It may be noted that the calculated the-
oretical density value of hybrid composite specimens is not
equal to the experimental density values. This may be attrib-
samples, some voids may arise. As observed from the tabula-
tion that the percentage of void contents increases with an
increase in the hemp fiber weight percentages. Natural fiber
composites with 30% hemp fiber have reported possessing
the highest void content. This may adversely affect the
mechanical and physical properties of the composite
ricated composite materials. Therefore, with the increase in
the fiber content, the void content of the fabricated compos-
ite specimens also increases. A similar trend of increment in
void content with fiber volume fraction has been observed by
other researchers.45
The composite specimen encompassing 30% flax
fibers has a relatively lower void content (Table 3). This
8 SAHA ET AL.

TABLE 3 Density and void content for developed composites

Theoretical Experimental Void

Sample Fiber percentage density(gm/cm3) density(gm/cm3) content (%)
S0 Neat epoxy 1.150 1.146 0.383
S1 30% hemp 1.222 1.165 4.614
S2 20% hemp +10% Flax 1.227 1.186 3.282
S3 15% hemp +15% Flax 1.229 1.194 2.838
S4 10% hemp +20% Flax 1.232 1.205 2.159
S5 30% flax 1.237 1.211 2.067

FIGURE 3 Comparisons of densities with void contents

could be attributed to the presence of a lower percentage
of the lumen in flax fibers in comparison to the hemp
fibers. Hence, the hybridization of flax fiber with hemp -
fiber-reinforced composite yielded lesser void content. A
similar trend was observed by other researchers.46 A
comparative analysis of the theoretical and experimental
densities with void contents of the fabricated composite
samples have been depicted in Figure 3.
4.2 | Water absorption results
Water absorption is a physical phenomenon for measur-
ing the water uptake by the composites during different
intervals of time. The moisture absorption of nonhybrid
and hybrid flax/hemp-reinforced polymer composite was
determined using the given Equation (7).
Wt  Wd
Ww ¼  100%,
Wd
where Ww = weight of water content, Wt = weight of
sample at time t, and Wd = weight of the dry specimen.
F I G U R E 4 Water absorption graph for the different sample at
room temperature (23
C)
Figure 4 shows the variation of water absorption per-
centage of the fabricated composites with immersion
time (t) at room temperature. For every composite config-
uration, five samples have been taken. From the results,
it is observed that the water absorption percentage of
sample S0 (sample of neat epoxy) is the least of the con-
sidered composite configurations. Other composite
configurations (S1, S2, S3, S4, and S5) show a higher per-
centage of water absorption compared to S0. For all the
considered composite configurations (S1, S2, S3, S4, and
S5), a similar trend in the percentage of water absorption
has been revealed with the immersion time in hours. The
percentage of water absorption is higher for initial
immersion times and then gradually becomes constant
after 264 h of immersion. A similar type of observation
was reported by Devireddy et al.39
ð7Þ
From the depiction in Figure 4, it is observed that the
highest water absorption has been observed for hemp
fiber (S1) and lowest for flax fiber (S5). On the other
hand, water absorption for hybrid composites (S2, S3,
SAHA ET AL. 9

and S4) has been observed to be intermediate between composite configurations, water absorption behavior can
these two composites. The presence of the cellulosic be modeled as Fick's second law. A similar type of n value
structure within the natural fibers is one of the major rea- is observed by Chandekar et al.51 and Feng et al.17
sons for water absorption. This may be attributed to the Assuming diffusion co-efficient constant along fiber
presence of the hydroxyl groups in the cellulosic struc- direction (x-direction), the 1D diffusion Equation (10).
ture that forms a hydrogen bond with the molecule of
water. Moreover, the lignin content also plays a very vital ∂C ∂2 C
¼D 2 , ð10Þ
role in the water absorption behavior of natural fiber- ∂t ∂x
reinforced composites. It has been observed that higher
lignin content leads to lower water absorption.47 Hence, where D = diffusion constant and C = concentration of
the different composite configurations (S1, S2, S3, S4, and diffusion substance.
S5) show a higher percentage of water absorption over Solving Equation (10) with appropriate boundary con-
the neat epoxy sample (S0).48 The water absorption dition, following Equation (11) can be obtained.52
behavior of hemp fiber-reinforced composites (S1) has


been revealed to be higher in comparison to flax fiber- Wt 8 X
∞
1 2 2 Dt
¼1 2 exp ð2n þ 1Þ π ,
reinforced composites (S5) because the cellulosic content W∞ π n¼0 ð2n þ 1Þ2 h2
in hemp fiber (68.4% by weight) is more in comparison to
ð11Þ
the flax fiber (51.43%). On the other hand, flax fiber has
higher lignin content (24.3% by weight) compared to
hemp fiber (3.7%). Also, the hybrid composite fabricated where h = half of the sheet thickness. Initially, Wt varies
with a more weight fraction of hemp fiber (S2) revealed linearly with time and hence Equation (11) can be writ-
more water absorption than the other hybrid composite ten as:
configurations (S3, S4, and S5).
rffiffiffiffiffi
At room temperature, the water absorption pattern Wt 4 Dt
¼ , ð12Þ
for natural fiber-reinforced composite follows Fickian W∞ h π
behavior where initially the water absorption is linear
and then approaches saturation after sufficient time of
immersion duration.49 By rearranging Equation (12), Equation (13) can be
The diffusion mechanics and kinetics in a material obtained and employed to determine the value of diffu-
can be analyzed by Equation (8). sion coefficient (D). D indicates the ability of water mole-
cules to penetrate a material
Wt
¼ kt n , ð8Þ
2
W∞ h ðW 2  W 1 Þ
D¼π pffiffiffiffi pffiffiffiffi , ð13Þ
4W ∞ ð t2  t1 Þ
where Wt = water absorption at time t, W∞ = water
absorption at saturation limit, time t is the immersion
time, and k and n are the coefficients. Therefore, Equa- where h = thickness of sample, W∞ = equilibrium mois-
tion (9) can be written as Equation (9) as follows: ture content, and ððpWffiffiffi
2 W 1Þ
pffiffiffi
t2  t1 Þ
is the slope of the initial part of
the graph of the moisture absorption curve.


Wt Table 4 shows the values of diffusion coefficient (D)
log ¼ logðkÞ þ nlogðt Þ, ð9Þ
W∞ for different composite configurations. Values of D are in
the range of 108 and a similar range of values for D have
Coefficients n and k can be found from the slope and been reported in other research studies.36,47 For the non-
intercept of the plot of log (Wt/W∞) vs. log (t) of water hybrid composite samples, hemp fiber-reinforced com-
absorption experiment data.50 Figure 5 shows Diffusion posite (S1) showed the highest diffusion coefficient and
mechanics with straight-line fitting for all types of com- hence maximum moisture absorption percentage. On the
posite samples. other hand, flax fiber-reinforced composite (S5) showed
When the value of n = 0.5 or less than that, it is said the lowest value of the diffusion coefficient and hence
to be Fickian diffusion behavior and when n = 1 or more, the lowest water intake capability. As such, the hybridi-
then the behavior is said to be anomalous diffusion. From zation of hemp and flax fiber reduced the water absorp-
Figure 5 it is seen that n is near about 0.5, so it is said to tion ability of the composite material and is reflected in
be Fickian diffusion. Therefore, for the considered the values of the diffusion coefficient.
10 SAHA ET AL.

FIGURE 5 Diffusion mechanics fitted graph for all type of composite material

TABLE 4 Diffusion co-efficient for developed composites adverse effects of water absorption on their mechanical
properties have been observed. The tensile and flexural
Diffusion
Sample Fiber percentage co-efficient (D) (m2/s)
properties of all the composite samples (S1, S2, S3, S4,
and S5) have been revealed to be decreasing with increas-
S1 30% hemp 2.164  108
ing time interval of immersion in water. Moreover, the
S2 20% hemp +10% flax 2.132  108 decrement in the mechanical properties due to moisture
S3 15% hemp +15% flax 1.857  108 absorption is higher for composite samples having a more
S4 10% hemp +20% flax 1.383  108 weight fraction of hemp fiber in comparison to the com-
S5 30% flax 1.121  108 posite samples with a more weight fraction of flax fiber.
The absorption of water molecules will lead to a change
in the structure of the natural fibers, that is, swelling may
4.3 | Mechanical properties results occur. This may result in cracking of the matrix and
interfacial damage within the composite samples. The
To study the effect of water absorption on the mechanical interfacial damage may lead to deboning at the fiber-
properties, tensile and flexural tests were performed on matrix interface and therefore it adversely affects the
the dry sample as well as the wet sample. The wet condi- transformation of the stress from the matrix to the fiber.
tion tests were carried out by immersing the composite The water content may also reduce the reinforcing effect
samples into water for different time intervals (24, 48, of fiber, which results in the further decrement of
72……0.264 h) and then redrying the sample after mechanical and flexural properties.48 It has been revealed
reaching the saturation level of water absorption. The through the water absorption test results that hemp fibers
effects of water absorption on tensile and flexural proper- have more tendency to absorb water the flax fibers. As
ties of the fabricated composite samples with different such, the composite samples having a more weight frac-
time intervals have been shown in Figure 6 and Figure 7, tion of hemp fiber showed a higher reduction in the
respectively. mechanical properties in comparison to the composite
It has been observed that the effect of water absorp- samples with a more weight fraction of flax fibers.
tion on the tensile and flexural properties of the neat The maximum tensile strength and tensile modulus
epoxy samples (S0) is negligible. However, for fiber- are recorded for flax fiber-reinforced composite
reinforced composite samples (S1, S2, S3, S4, and S5), the (96.638 MPa) and (4.454 GPa), respectively, while the
SAHA ET AL. 11

FIGURE 6 Tensile properties (A) tensile strength and (B) tensile modulus of developed composites with different water immersion time

F I G U R E 7 Flexural properties (A) flexural strength and (B) flexural modulus of developed composites with different water
immersion time

minimum for hemp fiber-reinforced composite
(64.374 MPa) and (3.212 GPa), respectively, at dry condi-
tions. Similarly, at dry conditions, flexural strength
(143.912 MPa) and flexural modulus (12.015 GPa) are
maximum for flax-reinforced composites and minimum
for hemp fiber-reinforced composite (121.584 MPa) and
(10.264 GPa), respectively.
From the depiction in Figure 6 and Figure 7, it can be
observed that the tensile and flexural properties of the
composite specimens decreased rapidly initially and as
the time of water immersion increased, the rate of decre-
ment was lower. This may be because initially, the rate of
water absorption was higher for the composite specimens
which decreased their properties rapidly. However, with
the increase in the immersion time, the water absorption
rate was lower and was saturated finally, which resulted
in less decrement in mechanical properties.
After saturation conditions were reached, the com-
posite samples were re-dried at 40
C for 5 days and then
were tested for their mechanical properties. From the
results, it has been observed that the re-dried composite
samples were regaining their properties in comparison to
the wet saturated samples. At re-dried condition, flax
fiber-reinforced composite (S5) had regained the maxi-
mum number of mechanical properties while for hemp
fiber-reinforced composite (S1) the amount of the
regained properties was less. Therefore, it can be con-
cluded that the composites with a more weight fraction
12
of flax fibers not only had the less percentage of water
absorption but also had the potential ability to eradicate
water molecules at a higher rate at re-dried conditions in
comparison to the composites with higher weight frac-
tion of hemp fibers.
Figure 8 shows the comparative representation of the
tensile and flexural properties of all composite samples at
dry, saturated water submerged, and re-dry conditions. It
has been observed that the saturated water absorption
limit has the maximum reduction on tensile and flexural
properties compared to dry composite samples.
To understand the water aging effect, the percentage
of decrement in mechanical properties can be defined as
the aging index (AI). This can be determined by Equa-
tion (14) and the aging effect for all composite samples
have been tabulated in Table 5.


Ww
AI ¼ 1   100%,
Wd
where Ww = value of mechanical properties at wet condi-
tion or re-dried condition and Wd = value of mechanical
properties at dry condition.40
As can be observed from the tabulation in Table 5,
hemp fiber-reinforced composite showed the highest
aging index and flax fiber-reinforced composite showed
the lower aging index at both saturated wet and re-dried
conditions. This signifies that mechanical properties for
the flax fiber composites (S5) not only degraded to a
lesser extent but they were also able to regain their prop-
erties to a higher extent after the wet samples were dried.
The aging index for the hybrid composites (S2, S3, and
S4) showed a diminishing pattern with increased weight
fraction of flax fiber. Hence, the hybridization of flax
F I G U R E 8 Comparative representation (a) tensile properties (B) flexural properties of developed composites at dry, saturated water and
re-dried condition
SAHA ET AL.
fiber and hemp fiber can aid in reducing the moisture
absorption behavior percentage and aging index (AI).
This also implies that the balance in the moisture uptake
and mechanical strength of the composite can be
achieved by the hybridization process.
4.4 | Thermal conductivity results
Conductivity test has been performed at dry condition,
wet condition, and re-dried condition for all composite
samples. It has been revealed that at dry condition neat
epoxy specimen (S0) has the highest thermal conductivity
of 0.4 W/mK. However, as the percentage of fiber loading
increased, the thermal conductivity of the samples
decreased. The reason behind these decrements may be
attributed to the presence of a cylindrical air gap in terms
of the lumen in natural fiber. This air gap acts as resis-
ð14Þ
tance and thereby results in the decreased thermal con-
ductivity.53,54 Among all fiber-loaded composite samples,
the hemp fiber-reinforced composite (S1) showed the
highest thermal conductivity of 0.251 W/mK while flax
fiber-reinforced composite (S5) showed the lowest ther-
mal conductivity with the value of 0.199 W/mk. This is
because hemp fiber has a greater crystalline index com-
pared to flax fiber.31,55
From the results of the thermal conductivity test
under wet conditions, it could be observed that as the
immersion time of the composite in water is increased,
the thermal conductivity also increased. The thermal
conductivity of all the composite samples increased rap-
idly with a rapid increment of water absorption and as
the water absorption became saturated, the increment in
thermal conductivity also got saturated. Lumen and pores
SAHA ET AL. 13

TABLE 5 Aging index (AI) for mechanical properties of developed composites at the saturated and re-dried condition

AI for tensile AI for tensile AI for flexural AI for flexural

strength (%) modulus (%) strength (%) modulus (%)

Sample Saturated Re-dry Saturated Re-dry Saturated Re-dry Saturated Re-dry

code wet sample sample wet sample sample wet sample sample wet sample sample
S0 3.29 0.76 5.00 1.27 5.77 2.54 9.13 4.78
S1 47.09 41.37 52.68 38.97 48.75 42.60 55.00 38.69
S2 40.99 31.69 51.77 36.51 46.02 37.02 53.72 35.69
S3 38.15 25.93 50.24 31.66 43.17 31.61 52.96 33.26
S4 36.84 21.67 47.26 25.38 40.98 26.91 49.15 25.87
S5 34.12 16.53 44.57 11.82 37.26 19.60 45.85 16.14

contents are present in these natural fibers that absorb

the water and the cylindrical air gap is filled with water.
The conductivity of water is greater than air, therefore,
with the increase in the moisture content, the composite
samples showed higher thermal conductivity compared
to thermal conductivity under dry conditions.56 Figure 9
shows the thermal conductivity of all the composite sam-
ples at the different immersion time in the water.
The maximum increment in thermal conductivity
(228%) has been observed for hemp-reinforced composite
(S1) for saturated water samples in comparison to the dry
samples. On the other hand, the lowest increment in
thermal conductivity (140%) has been observed for flax-
reinforced composite (S5). A comparative analysis of the
thermal conductivity results for all the composite samples
under dry, saturated, and re-dried conditions have been
presented in Figure 10. For the re-dried samples, it is
seen that the thermal conductivity of all composite sam- F I G U R E 9 Thermal conductivity of developed composites with
ples is low compared to saturated condition but it is different immersion time
higher than the thermal conductivity under dry condi-
tions. This implies that after re-drying the composite
samples, some amount of water is still present in the measures the elastic response of the polymeric compos-
lumen structure of the natural fiber, which acts as a ther- ites under the per cycle of oscillation represents the stiff-
mal conductor in the composite samples. ness of the material which is a function of temperature.58
The loss modulus also called the viscous modulus, is used
to characterize the viscous response of the polymeric
4.5 | DMA results material and measures the energy dissipation rate in the
form of heat per loading cycle. The loss factor also
DMA is a characterization technique to find out the vis- referred to as damping factor, is the ratio of loss modulus
coelastic properties of the materials. DMA is used to to storage modulus. The Tg is the temperature where the
reveal the molecular mobility behavior of the polymeric materials change their region from a glassy state to a rub-
composites' materials.57 There are three different regions bery state and is measured at that temperature where the
that are present in DMA: glass region, glass transition values loss modulus or loss factor are maximum.59 Vari-
region, and rubbery region. The storage modulus attends ous viscoelastic properties such as storage modulus (E'),
maximum value in the glassy region, the loss modulus loss modulus (G'), and loss factor (tanδ) were investigated
and damping factor are maximum in the glass transition for the fabricated composites under the influence of the
region and the rubbery region, and the viscoelastic prop- temperature and frequency. The current study investi-
erties have the lowest value. The storage modulus gated various viscoelastic properties of the flax and
14
F I G U R E 1 0 Comparative thermal conductivity of developed
composites under dry, saturated, and re-dried conditions
hemp-reinforced polymer composites under dry, wet,
and re-dried conditions. The results have been obtained
for temperature varying from 24
C to 200
C and at a con-
stant frequency of 1 Hz. For wet condition, the compos-
ites samples were immersed in the distilled water at
room temperature for different time intervals (0–264 h).
The storage modulus of the different composite samples
(S0, S1, S2, S3, S4, and S5) under dry condition has been
shown in Figure 11(A). The results show that the storage
modulus is higher for all the composite samples at room
temperature because the molecules of the matrix and fibers
are packed closely. However, as the temperature increases,
the storage modulus suddenly drops down because, with
the increase in temperature, the close packing between the
molecules becomes weak and also there is a decrement in
the stiffness of the fibers.60 The hybrid composite sample
(S3) exhibited maximum storage modulus (7.8 GPa) due to
the better interlocking bond between matrix and fibers that
provided better stress transfer at interfaces of the composite
sample. On the other hand, the neat epoxy sample (S0) had
the lowest value of storage modulus (1.675 GPa). For the
other composite samples, the following order was revealed
for the storage modulus: S1 < S5 < S2 < S4.56 The flax
fiber-reinforced polymer composite (S1) had higher storage
modulus (4.25 GPa) in comparison to the hemp fiber com-
posite (3.33 GPa) (S5). This may be attributed to the fact
that flax fibers have lower moisture absorption capacity and
high energy capacity rate.32,61 The storage modulus values
for other hybrid composites (S2 and S4) were recorded to be
4.87 GPa and 5.45 GPa, respectively. The results revealed
that hybrid composites (S2, S3, and S4) had higher values of
storage modulus than the single fiber-reinforced polymer
composites (S1 and S5).
SAHA ET AL.
The loss modulus of the different composite samples
under dry conditions is shown in Figure 11(B). As the
temperature increased from the glassy region to the glass
transition region, the loss modulus had the highest value
and then dropped drastically in the rubbery region with
further increase in the temperature. The highest value of
loss modulus, as well as the Tg, have been revealed in the
glass transition region. The hybrid composites with equal
weight fractions of flax and hemp (S3) exhibited the
highest value of loss modulus (1.396 GPa) at the highest
Tg (102
C). On the other hand, the neat epoxy sample
(S0) had the lowest loss modulus (0.215 GPa) with the
lowest Tg (71C
). This may be attributed to the fact that
natural fibers are elastic in comparison to the polymeric
matrix that increases the heat dissipation rate at higher
temperature.62 Moreover, the high energy absorption
capacity of the fibers is another reason for the higher loss
modulus. The loss modulus values for the other
composite samples followed the following order:
S1 < S5 < S2 < S4. The results, therefore reveal that the
hybrid composites (S2, S3, and S4) had higher values of
loss modulus in comparison to the single fiber-reinforced
composites (S1 and S5). The loss modulus for other
hybrid composites (S2 and S4) have been revealed to be
0.775 GPa and 0.891GPa at Tg of 86
C and 91
C, respec-
tively. Hence, the composite sample with a higher weight
fraction of flax fiber (S4) had the highest loss modulus
(S4). This is because flax fibers are more flexible and have
more energy absorption rate than hemp fibers.
The damping factor (tanδ) also known as loss factor is
defined by the ratio of loss modulus to storage modulus.
The loss factor curve depends on the adhesion between
matrix and reinforcement materials that in turn depend
on temperature.59 Figure 11(C) shows the loss factor
curve, which is similar to the loss modulus curve.
Figure 12 shows the comparison of storage modulus
and loss modulus for all the composite samples at dry,
saturated wet, and re-dried conditions. As results show,
all the composite samples have lower values of storage
modulus in wet condition in comparison to dry condi-
tion. The moisture content has adverse effects on the
storage modulus as the presence of water molecules dis-
turbs the molecular bond of the composites. Therefore,
the molecular chains are enlarged and also there is
enhanced mobility of the molecules, which decreases the
stiffness of the materials.63 The decrements in storage
modulus are 7%, 30%, 18%, 12%, 13%, and 8% for S0, S1,
S2, S3, S4, S5, and S6, respectively. Since, hemp fiber
exhibited a high moisture absorption rate, the highest
decrement in the storage modulus was observed for hemp
fiber composites (S1).
On other hand, the values of the loss modulus of com-
posite samples under wet condition have been revealed
SAHA ET AL. 15

F I G U R E 1 1 Dynamic mechanical analysis (DMA) properties (a) storage modulus (B) loss modulus and (C) damping factor of developed
composites with variations in temperature

to be higher than that of the composite samples under

dry conditions. This is because the loss modulus
depends mainly on the viscoelastic damping character-
istics of the fiber and matrix. Higher values of loss
modulus indicate higher damping and poor adhesion
of interface, which also results in decreased Tg.64 The
water molecules increase the mobility of the chain seg-
ments, thereby increasing the viscosity of the mate-
rials. Moreover, with the increase in water content,
debonding on the interface area of fiber and epoxy
takes place and hence the mismatch of moisture expan-
sion co-efferent between fibers and matrix causes
higher dissipation of energy.57 The increment in loss
modulus values were revealed to be 5%, 19%, 11%, 8%,
6%, and 4% for S0, S1, S2, S3, S4, S5, and S6, respec-
tively. On the other hand, the decrement in Tg has F I G U R E 1 2 Comparative studies of Dynamic mechanical
been revealed to be in the range of 3
C–6
C. analysis (DMA) properties at dry, saturated, and re-dried conditions
16 SAHA ET AL.

A comparative analysis of the storage modulus and
loss modulus was also investigated for all the compos-
ite samples after they were re-dried at 40
C for 5 days.
The results showed that there was an insignificant
increment in the storage modulus and insignificant
decrement in the loss modulus for all the re-dried com-
posite samples over the composite samples under wet
conditions.
A comparative analysis of the results obtained for the
studied composites with that of the other prominent
research works has been depicted in Table 6.
4.6 | Morphology analysis of composite
The morphological behavior of developed nonhybrid and
hybrid composites has been analyzed at dry and saturated
conditions using SEM. The microstructures of nonhybrid
(S0 and S5) at fracture have been shown in Figure 13(A),
(B), respectively, and the morphology of hybrid compos-
ites (S2, S3, and S5) has been shown in Figure 13(C),(D)
at tensile and flexural loading conditions.
Through the analysis, it was revealed that failures
to the composite specimen occurred due to fiber pull-
out, fiber breakage, fiber-matrix debonding, cluster
effects, fiber delamination, and crushing. A weaker
interfacial bonding with the epoxy matrix has been rev-
ealed for the hemp fiber composite and hence lower
stiffness and strength in comparison to the flax poly-
meric composites. Also, the presence of water within
the microstructure of composites had adverse effects
on their mechanical properties due to poor bonding
and lower load transfer to the matrix. Similar adverse
effects of the presence of water on the properties have
also been reported by Yorseng et al.74 The hybrid com-
posites (S2, S3, and S4) showed excellent interlocking
between fibers and matrix that may be evidenced to
significant load transfer, improved energy-dissipating
capacity, and enhanced mechanical as well viscoelastic
properties.17 Overall, all the developed composites
showed brittle catastrophic failure without the occur-
rence of plastic deformation and breakage of fiber indi-
cates better adhesive bonding between fibers and epoxy
matrix.

TABLE 6 A comparative analysis with the past research studies

Tensile Tensile Flexural Flexural Water

strength modulus strength modulus absorption
References Fibers Matrix (MPa) (GPa) (MPa) (GPa) (%)
Thiagamani Hemp SR Greenpoxy 30.76 1.095 — — 11.86
et al.65 Sisal 56
Senthilkumar Hemp SR green poxy 33.30 2.893 60.56 2.860 —
et al.66 Sisal 56
Chaudhary Jute Epoxy resin 43.32 1.64 86.6 1.78 —
et al.67 Flax
Hemp
Kishnasamy Aloe Epoxy resin 46.41 — 134.28 — 4.48%
et al.68 vera
Flax
Hemp
Ashraf et al.69 Flax Epoxamite 241.2 13.2 140.8 3.84 —
Glass 100 epoxy
Hongguang Flax Epoxy 231.43 5.68 426.53 15.76 —
Wang et al.70 Glass
Lalta Prasad Hemp Polyester 74.61 — 18.35 — 2.43%
et al.71 Nettle
Ng Lin Feng Kenaf Polypropylene 21.36 3.83 52.98 2.75 5.14%
et al.17 PALF
Sumesh et al72 PALF 36.75 68.97
Flax
Venkateshwaran Banana Epoxy LY-556 18.66 0.682 59.687 9.13 23.47%
et al.73 Sisal
Present work Hemp Epoxy LY-556 84.67 4.4 134.663 11.413 5.06%
Flax
SAHA ET AL. 17

FIGURE 13 Scanning electron microscopy (SEM) morphological images of developed composites

sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
5 | S T ATI S T I C AL AN A LY S I S O F 1 XN
SD ¼ ðx i  x Þ2 , ð16Þ
TESTED DATA ðN  1 Þ i

Many factors can affect the tested result of the developed

composites, such as manufacturing process, distribution
of fibers, fiber direction, fiber-matrix bonding, matrix-
hardener mixture, storage of the samples, experiment
temperature, experiment technique, design of test ring,
etc.75 The statistical scatter, which is mathematically
known as the coefficient of variation (CV), SD and mean
values have been obtained from the experimental results
and tabulated in respective results data. To find out the
mean value, SD, and CV, Equations (1) (2), and (3) have
been used.76
The mean value of property x will be,
x1 þ x2 þ x3 þ … þ xN
x ¼ , ð15Þ
N weight gain behavior, the maximum CV value is observed
where n is the numbers of samples. The standard devia-
tion was determined using (16):
where i varied from 1 to N, and the coefficient of vari-
ation (CV) has been found by using:


SD
CV ¼  100 %, ð17Þ
x
Tables S1–S7 (in the supplementary document) depict
the statistical analysis results for void content, water
absorption behavior, tensile strength, tensile modulus,
flexural strength, flexural modulus, and conductivity of
the developed composites respectively.
The maximum scatters for void content have been
observed for the S3 composite (6.64%). For water absorption
for S4 composite (8.714%) after 96 h of water submerging.
On other hand, tensile strength, tensile modulus, flexural
strength, flexural modulus, and conductivity, the maximum
18
CV values are observed as 9.983%, 10.759%, 13.714%,
12.404%, and 10.909%, respectively. Thus, it can be concluded
that for all developed composites specimens, the maximum
scatters values are recorded less than 15%, which is well
accepted for composite design and developments.77,78
6 | C ON C L U S I ON
This study aimed to investigate the water absorption
behavior and effects of water absorption on mechanical,
thermal, and dynamic mechanical properties of flax/
hemp-reinforced nonhybrid and hybrid composite with
different weight fraction of fibers (whereas total weight
fraction of fiber remains constant to 30%). As per the
results obtained, the following conclusion can be drawn:
• The maximum water absorption capacity has been
observed for hemp fiber-reinforced composite (S1) and
the minimum was reported for flax fiber-reinforced
composite (S5). It is due to the presence of a greater
percentage of cellulose and a lower percentage of lig-
nin contents in hemp fiber over the flax fibers. The
hybridization of hemp fibers with flax fibers resulted
in lower water absorption capacity over the hemp
fiber-reinforced composites. Following decrements in
the percentage of water absorption capacity have been
observed for S2, S3 and, S4 over S1, respectively:
10.61%, 19.29%, and 32.34%.
• Under dry conditions, following observations have
been revealed: tensile strength is maximum for S5
(96.63 MPa) while the minimum for S1 (64.37). The
hybridization of hemp fibers with flax fibers showed
better results. Following enhancement in tensile
strength have been recorded for S2, S3, and S4 over S1
13.10%, 22.38%, and 31.57%, respectively. The percent-
age increments in tensile modulus have been revealed
to be 14.13%, 18.06%, and 25.65%, respectively, for S2,
S3, and S4 over S1. Flexural strength of S2, S3, and S4
showed the following percentage enhancement over
S1: 2.53%, 5.10%, and 10.91%, respectively. Flexural
modulus of S2, S3, and S4 showed increments of
5.36%, 8.19%, and 11.26%, respectively over S1. The
thermal conductivity at dry conditions is recorded
maximum for S0 (0.41 W/mK) and the addition of fiber
showed a decrement in thermal conductivity values (S1 to
S5). At dry condition, S1 has the highest conductivity
(0.251 W/mK) while the lowest for S5 (0.199 W/mK).
There were the following decrements in the thermal con-
ductivity of S2, S3 and S4 over S1: 8.13%, 16.89%, and
18.25%, respectively. The dynamic mechanical properties
(storage modulus and loss modulus) at dry condition were
recorded to be maximum for S3 composites (7.8GPa and
SAHA ET AL.
1.396GPa) with Tg of 102
C while the minimum for S1
(3.33 GPa and 0.465 GPa), respectively. The hybridization
of flax/hemp fiber-reinforced composites have better inter-
locking bonding and greater interfacial load-bearing
capacity where the influence of temperature and fre-
quency may less affect the molecular chain of closed bond
structure.
• Water absorption resulted in the decrement in mechani-
cal properties with a higher water absorption rate
resulting in more decrement in the mechanical proper-
ties of the fabricated composites. Maximum decrement
in the tensile strength, tensile modulus, flexural strength,
and flexural modulus was observed for S1, that is, by 47.
27%, 54.87%, 52.01%, and 55%, respectively, under the
saturated condition. Hybridization of hemp fibers with
flax fibers resulted in lower decrements in mechanical
properties. Tensile strengths for S2, S3, and S4 decreased
by 41.85%, 38.23%, and 36.79%, respectively, and tensile
modulus showed the following decrements for S2, S3,
and S4, respectively: 53.27%, 51.79%, and 47.99%. For
flexural strength and flexural modulus following decre-
ments have been observed for S2, S3, and S4, respectively:
47.84%, 44.06%, 37.16% and 53.75%, 52.79% and 49.03%.
However, an increment in thermal conductivity at satu-
ration condition was revealed for the fabricated compos-
ites. It was revealed to be maximum for S1 (225.66%).
The percentage increments in thermal conductivity for
S2, S3, and S4 have been revealed to be 204.54%, 155.38%,
and 103.35%, respectively. The storage modulus values
for S1, S2, S3, and S4 showed the following decrements at
saturations 30%, 18%, 12%, and 13%, while following
increments in the loss modulus were recorded for S1, S2,
S3, and S4, respectively: 19%, 11%, 8%, and 6%. The water
contents in composites increase the molecular chain and
mobility. The increments in mobility increase the viscosity
and also enhances the free motion, which results in the
decrement in storage modulus and increments in loss
modulus of developed composites at saturated conditions.
• Under the re-dried condition, the developed compos-
ites were able to regain their mechanical properties to
a maximum extent.
Overall, the hybridization of flax and hemp fiber-
reinforced composites has been revealed to be advanta-
geous as the addition of flax fiber in hemp fiber-
reinforced composites have decreased the water absorp-
tion rate and increased the mechanical and viscoelastic
properties of developed hybrid composites.
ACKNOWLEDGMENTS
The authors would like to acknowledge CIF, IIT
Guwahati and ACMS, IIT Kanpur for providing the test
facilities.
SAHA ET AL.
ORCID
Abir Saha https://orcid.org/0000-0002-2909-7788
Santosh Kumar https://orcid.org/0000-0002-1831-8805
Divya Zindani https://orcid.org/0000-0002-9941-593X
R EF E RE N C E S
[1] M. Habibi, L. Laperrière, H. M. Hassanabadi, Compos. Struct.
2018, 186, 175. https://doi.org/10.1016/j.compstruct.2017.
12.024
[2] S. M. Sultana, M. Hasan, S. M. Hasan, M. J. Hossain, N.
Nafsin, Polym. Compos. 2017, 38, 1259. https://doi.org/10.
1002/pc.23690
[3] V. P. Arthanarieswaran, A. Kumaravel, M. Kathirselvam,
Mater. Des. 2014, 64, 194. https://doi.org/10.1016/j.matdes.
2014.07.058
[4] I. N. Hidayah, D. N. Syuhada, H. A. Khalil, Z. A. Ishak, M.
Mariatti, Mater. Des. 2019, 171, 107710. https://doi.org/10.
1016/j.matdes.2019.107710
[5] V. Paul, K. Kanny, G. G. Redhi, Compos. Part A Appl. Sci.
Manuf. 2015, 68, 90. https://doi.org/10.1016/j.compositesa.
2014.08.032
[6] M. P. Dicker, P. F. Duckworth, A. B. Baker, G. Francois, M. K.
Hazzard, P. M. Weaver, Compos. Part A Appl. Sci. Manuf.
2014, 56, 280. https://doi.org/10.1016/j.compositesa.2013.
10.014
[7] D. B. Dittenber, H. V. GangaRao, Compos. Part A Appl. Sci.
Manuf. 2012, 43, 1419. https://doi.org/10.1016/j.compositesa.
2011.11.019
[8] S. Nimanpure, S. A. Hashmi, R. Kumar, H. N. Bhargaw, R.
Kumar, P. Nair, A. Naik, Polym. Compos. 2019, 40, 664.
https://doi.org/10.1002/pc.24706
[9] A. Perrier, F. Touchard, L. Chocinski-Arnault, D. Mellier,
Polym. Test. 2017, 57, 17. https://doi.org/10.1016/j.
polymertesting.2016.10.035
[10] Y. Shen, J. Zhong, S. Cai, H. Ma, Z. Qu, Y. Guo, Y. E. Li, Mate-
rials 2019, 12, 453. https://doi.org/10.3390/ma12030453
[11] M. M. Lu, A. W. Van Vuure, Compos. Part A Appl. Sci. Manuf.
2019, 123, 301. https://doi.org/10.1016/j.compositesa.2019.
05.029
[12] N. L. Feng, S. D. Malingam, K. Subramaniam, M. Z. Selamat,
M. B. Ali, O. Bapokutty, Def. Sci. and Technol. Tech. Bull. 2020,
13, 117.
[13] Y. Karaduman, L. Onal, A. Rawal, Polym. Compos. 2015, 36,
2167. https://doi.org/10.1002/pc.23127
[14] L. F. Ng, D. Sivakumar, K. A. Zakaria, O. Bapokutty,
Pertanika. J. Sci. 2017, 25, 1.
[15] M. R. Sanjay, B. Yogesha, J. Ind. Text. 2018, 47, 1830. https://
doi.org/10.1177/1528083717710713
[16] A. B. Maslinda, M. A. Majid, M. J. Ridzuan, M. Afendi, A. G.
Gibson, Compos. Struct. 2017, 167, 227. https://doi.org/10.
1016/j.compstruct.2017.02.023
[17] N. L. Feng, S. D. Malingam, C. W. Ping, Int. Rev. Mech. Eng.
2017, 11, 61. https://doi.org/10.1002/pc.25451
[18] S. Sekar, S. S. Kumar, S. Vigneshwaran, J. Nat. Fibers 2020, 1,
11. https://doi.org/10.1080/15440478.2020.1788487
[19] M. H. M. Hamdan, J. P. Siregar, T. Cionita, J. Jaafar, A.
Efriyohadi, R. Junid, A. Kholil, Int. J. Adv. Manuf. Tech 2019,
104, 1075. https://doi.org/10.1007/s00170-019-03976-9
19
[20] P. V. Badyankal, T. S. Manjunatha, G. B. Vaggar, K. C.
Praveen, Mater. Today 2021, 35, 383. https://doi.org/10.1016/j.
matpr.2020.02.695
[21] N. L. Feng, S. D. Malingam, C. W. Ping, N. Razali, Polym.
Compos. 2020, 41. https://doi.org/10.1002/pc.25451
[22] S. Ganesh, Y. Gunda, S. R. J. Mohan, V. Raghunathan, J. D. J.
Dhilip, J. Nat. Fibers. 2020, 18, 1. https://doi.org/10.1080/
15440478.2020.1787921
[23] M. Arulmurugan, A. S. Selvakumar, K. Prabu, G.
Rajamurugan, Bull. Mater. Sci. 2020, 43, 1. https://doi.org/10.
1007/s12034-019-2018-7
[24] D. Chandramohan, T. Sathish, S. D. Kumar, M. Sudhakar, AIP
Conf. Proc. 2020, 2283, 020084. https://doi.org/10.1063/5.
0024976
[25] F. Duc, P. E. Bourban, C. J. G. Plummer, J.-A. E. Månson,
Compos. Part A Appl. Sci. Manuf. 2014, 64, 115. https://doi.
org/10.1016/j.compositesa.2014.04.016
[26] K. Cheour, M. Assarar, D. Scida, R. Ayad, X. -L. E. Gong,
Compos. Struct. 2016, 152, 259. https://doi.org/10.1016/j.
compstruct.2016.05.045
[27] M. Berges, R. Léger, V. Placet, V. Person, S. Corn, X. Gabrion,
J. Rousseau, E. Ramasso, P. Ienny, S. Fontaine, Compos. Part
A Appl. Sci. Manuf. 2016, 88, 165. https://doi.org/10.1016/j.
compositesa.2016.05.029
[28] X. Wang, M. Petru, Materials 2019, 12, 2376. https://doi.org/
10.3390/ma12152376
[29] W. Wang, X. Guo, D. Zhao, L. Liu, R. Zhang, J. Yu, Polymer
2020, 12, 782. https://doi.org/10.3390/polym12040782
[30] L. Y. Mwaikambo, M. P. Ansell, J. Appl. Polym. 2002, 84, 2222.
https://doi.org/10.1002/app.10460
[31] S. Vaitkus, R. Karpavičiutė, S. Vėjelis, L. Lek
unaitė, Key. Eng.
Mater. 2014, 604, 285.
[32] M. L. Loong, D. Cree, J. Polym. Environ. 2018, 26, 224. https://
doi.org/10.1007/s10924-017-0943-3
[33] C. Audibert, A. S. Andreani, E. Lainé, J. C. Grandidier, Compos.
Struct. 2018, 195, 126. https://doi.org/10.1016/j.compstruct.2018.
04.061
[34] A. Saha, S. Kumar, A. Kumar, J. Poly. Res. 2021, 28, 66.
https://doi.org/10.1007/s10965-021-02435-y
[35] A. Mishra, S. Ghosh, Fuel 2019, 236, 544. https://doi.org/10.
1016/j.fuel.2018.09.024
[36] U. K. Komal, M. K. Lila, I. Singh, Compos. B Eng. 2020, 180,
107535. https://doi.org/10.1016/j.compositesb.2019.107535
[37] ASTM Standard D 2734-70. Standard test method for void con-
tent of reinforced plastics. American society for testing and
materials. 1985.
[38] A. V. Rajulu, K. N. Chary, G. R. Reddy, Y. Z. Meng, J. Reinf. Plast.
Compos. 2004, 23, 127. https://doi.org/10.1177/0731684404029326
[39] S. B. Devireddy, S. Biswas, J. Reinf. Plast. Compos. 2016, 35,
1157. https://doi.org/10.1177/0731684416642877
[40] ASTM D 570-98. Standard test method for water absorption of
plastics 2005.
[41] ASTM Standard D638, Standard Test Method for Tensile Prop-
erties of Plastics, ASTM International, West Conshohocken
(PA) 2010.
[42] ASTM Standard D790, Standard Test Methods for Flexural
Properties of Unreinforced and Reinforced Plastics and Electri-
cal Insulating Materials, ASTM International, West Con-
shohocken (PA) 2010.
20
[43] Standard AS. Standard Test Method for Evaluating the Resis-
tance to Thermal Transmission of Materials by the Guarded
Heat Flow Meter Technique. Designation: E1530–11. 2011.
[44] ASTM D5023-99 Standard Test Method for measuring the
dynamic mechanical properties of plastics using three-point
bending.
[45] A. Satapathy, A. K. Jha, S. Mantry, S. K. Singh, A. Patnaik, J.
Reinf. Plast. 2010, 29, 2869. https://doi.org/10.1177/
0731684409341757
[46] M. Jawaid, H. A. Khalil, A. Hassan, E. Abdallah, Bioresources
2012, 7, 2344.
[47] M. Z. Khan, S. K. Srivastava, M. K. Gupta, J. Reinf. Plast. 2018,
37, 1435. https://doi.org/10.1177/0731684418799528
[48] Y. Sudiana, M. Z. Selamat, S. N. Sahadan, S. D. Malingam, N.
Mohamad, Proceed. Mech. Eng. Res. 2017, 2017, 410. https://
doi.org/10.11113/jt.v80.10774
[49] Z. N. Azwa, B. F. Yousif, A. C. Manalo, W. Karunasena, Mater.
Des. 2013, 47, 424. https://doi.org/10.1016/j.matdes.2012.
11.025
[50] S. Ramakrishnan, K. Krishnamurthy, R. Rajasekar, G.
Rajeshkumar, J. Ind. Text. 2019, 49, 597. https://doi.org/10.
1177/1528083718792915
[51] H. Chandekar, V. Chaudhari, S. Waigaonkar, A. Mascarenhas,
Polym. Compos. 2020, 41, 1447. https://doi.org/10.1002/pc.
25468
[52] G. S. Springer, C. H. Shen, Michigan Univ. ann. Arbor. Dept.
of Mechanical Engineering; 1978.
[53] N. Saba, P. M. Tahir, M. Jawaid, Polymers 2014, 6, 2247.
https://doi.org/10.3390/polym6082247
[54] H. N. Dhakal, Z. Y. Zhang, M. O. W. Richardson, Compos. Sci.
Technol. 2007, 67, 1674. https://doi.org/10.1016/j.compscitech.
2006.06.019
[55] M. S. Kumar, S. Kumar, D. Pranesh, C. Naveen, AIP Conf.
Proc. 2019, 2200, 02009. https://doi.org/10.1063/1.5141264
[56] Z. Javanbakht, W. Hall, A. Öchsner, Mater. Perform. 2018, 92,
507. https://doi.org/10.1007/978-3-319-79005-3_32
[57] Z. Wang, G. Xian, X. L. Zhao, Constr. Build. Mater. 2018, 161,
634. https://doi.org/10.1016/j.conbuildmat.2017.11.171
[58] C. A. Pandian, H. S. Jailani, Polym. Bull. 2018, 75, 1997.
[59] N. Saba, M. Jawaid, O. Y. Alothman, M. T. Paridah, Constr.
Build. Mater. 2016, 106, 149. https://doi.org/10.1016/j.
conbuildmat.2015.12.075
[60] V. Chaudhary, P. K. Bajpai, S. Maheshwari, Fiber. Polym.
2018, 19, 403. https://doi.org/10.1007/s12221-018-7759-6
[61] M. Rajesh, P. Jeyaraj, N. Rajini, Nanoclay. Reinf. Polym. Com-
pos. 2016, 281, 1. https://doi.org/10.1007/978-981-10-0950-1_12
[62] M. K. Gupta, P. I. Mech. Eng. L-J. Mat. 2018, 232, 743. https://
doi.org/10.1177/1464420716646398
[63] A. Le Duigou, P. Davies, C. Baley, Polym. Degrad. Stabil. 2009,
94, 1151. https://doi.org/10.1016/j.polymdegradstab.2009.
03.025
[64] T. Yilmaz, T. Sinmazcelik, J. Mater. Sci. 2010, 45, 399. https://
doi.org/10.1007/s10853-009-3954-1
SAHA ET AL.
[65] S. M. Thiagamani, S. Krishnasamy, C. Muthukumar, J.
Tengsuthiwat, R. Nagarajan, S. Siengchin, S. O. Ismail, Int. J.
Biol. Macromol. 2019, 140, 637. https://doi.org/10.1016/j.
ijbiomac.2019.08.166
[66] K. Senthilkumar, T. Ungtrakul, M. Chandrasekar, T. S.
Kumar, N. Rajini, S. Siengchin, H. Pulikkalparambil, J.
Parameswaranpillai, N. Ayrilmis, J. Polym. Environ. 2021, 29,
624. https://doi.org/10.1007/s10924-020-01904-7
[67] V. Chaudhary, P. K. Bajpai, S. Maheshwari, J. Nat. Fibers.
2018, 15, 80. https://doi.org/10.1080/15440478.2017.1320260
[68] P. Krishnasamy, G. Rajamurugan, S. Aravindraj, P. E.
Sudhagar, J. Nat. Fibers. 2020, 7, 1. https://doi.org/10.1080/
15440478.2020.1835782
[69] W. Ashraf, M. R. Ishak, M. Y. Zuhri, N. Yidris, A. M. Ya'acob,
Int. J. Polym. Sci. 2021, 2021, 1. https://doi.org/10.1155/2021/
8855952
[70] H. Wang, L. Yang, H. Wu, Polym. Compos. 2021, 42, 714.
https://doi.org/10.1002/pc.25860
[71] L. Prasad, A. Kumain, R. V. Patel, A. Yadav, J. Winczek, J.
Nat. Fibers. 2020, 19, 1. https://doi.org/10.1080/15440478.2020.
1821284
[72] K. R. Sumesh, K. Kanthavel, V. Kavimani, Int. J. Biol.
Macromol. 2020, 150, 775. https://doi.org/10.1016/j.ijbiomac.
2020.02.118
[73] N. Venkateshwaran, A. ElayaPerumal, A. Alavudeen, M.
Thiruchitrambalam, Mater. Des. 2011, 32, 4017. https://doi.
org/10.1016/j.matdes.2011.03.002
[74] K. Yorseng, S. M. Rangappa, H. Pulikkalparambil, S. Siengchin,
J. Parameswaranpillai, Constr. Build. Mater. 2020, 235, 117464.
https://doi.org/10.1016/j.conbuildmat.2019.117464
[75] A. I. Selmy, M. A. Abd El-baky, D. A. Hegazy, J. Thermoplast.
Compos. Mater. 2019, 32, 267. https://doi.org/10.1177/
0892705717751022
[76] M. A. Abd El-baky, Fibers Polym. 2017, 18, 2417. https://doi.
org/10.1007/s12221-017-7682-x
[77] M. A. Attia, M. A. A. El-Baky, M. A. Hassan, T. A. Sebaey, E.
Mahdi, Polym. Compos. 2017, 39, 2245. https://doi.org/10.
1002/pc.24597
[78] M. Megahed, D. E. Tobbala, M. A. El-baky, Polym. Compos.
2020, 42, 271. https://doi.org/10.1002/pc.25823
SU PP O R TI N G I N F O RMA TI O N
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