Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

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Experimental study on dynamic mechanical properties of arecanut husk

fiber composite
Vishal C. Mathapati a,⇑, N. Muralidhar a, B.R. Tulasiram b, Muttana S. Balreddy b
a
Department of Civil Engineering, Sri Siddhartha Institute of Technology, Tumakuru 572105, Karnataka, India
b
Department of Civil Engineering, Siddaganga Institute of Technology, Tumakuru 572103, Karnataka, India

a r t i c l e i n f o a b s t r a c t

Article history: Natural fibers gain utility value by being used as reinforcing materials in the production of lightweight
Available online xxxx and inexpensive composites. Natural fibers possess considerable mechanical properties and will replace
the synthetic fiber used in applications of structural elements, such as construction materials, interior
Keywords: components, aerospace, automotive parts, and sports goods, packaging industries, and other industries.
Dynamic mechanical analysis It is necessary to investigate the viscoelastic behavior of polymer composite over increasing temperature
Arecanut husk fiber and frequency. The present investigation focuses on the dynamic behavior to evaluate the damping fac-
Alkali treatment
tor, elastic modulus and loss modulus of AHF reinforced epoxy composite using a DMA Q800 instrument
Potassium hydroxide
Multi-frequency
in double cantilever mode at heating rate of 3 °C per minute over ramping temperature from 28 °C to
125 °C with multi-frequency ranging from 1 to 10 Hz. The dynamic characteristics of AHF reinforced
epoxy composites are impacted by frequency and temperature. The modulus values increased as the
loading frequency increased, and the modulus values decreased as the temperature increased. Glass tran-
sition temperature was increased from 84 °C for untreated AHF composites to 91 °C for treated AHF com-
posites. Treated AHF composites show improved storage and loss modulus compared to untreated AHF
composites because of 6 % KOH treatment of AHF.
Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on Thermal Analysis and Energy Systems 2021.

1. Introduction modulus (E0 ), loss modulus (E00 ), glass transition temperature and
mechanical damping (tan d) values of the composite material [6].
Dynamic mechanical analysis (DMA) is commonly used Many investigations have shown that natural fibers can com-
methodology in material research, such as polymers and metals, pete with synthetic fibers to some extent. With some modifica-
but its applicability to natural fiber composites has yet to be com- tions, natural fiber-reinforced composites can replace synthetic
pletely explored. Natural fiber reinforced composite’s dynamic composites and plastics [7–9]. Sudhir Kumar et al. conducted
loading performance is as important as static loading performance mechanical and DMA tests on hybrid composite fabricated using
[1–3]. The dynamic characteristics of a composite material depend coir and bagasse fibers of different laying patterns and observed
on several parameters, such as modes of loading, matrix type and that the mechanical characteristics have better relationship with
content, fiber content, fiber orientation, fiber geometry, and ambi- dynamic properties. The author investigated the influence of
ent temperature [4,5]. The DMA approach grew more user-friendly frequency and temperature on E0 , tan d, and E00 values of the com-
as computer power rose, resulting in the instruments being used posites. The E0 values of the composites were significantly greater
for quality control and creating new materials. In most DMA inves- compared to plain epoxy novolac resin above transition tempera-
tigations, the stress is applied at a constant frequency, the ramping ture (Tg). The tri-layer composite, which was made with bagasse
temperature at a rate usually between 1 °C to 5 °C, and the strain is fiber for the skin and coir fiber for the core, had the maximum stiff-
maintained constant. This approach is used to examine the storage ness. [10]. The dynamic characteristics of composites depend on
several parameters such as fiber–matrix interfacial bonding, aspect
ratio of the fiber, fiber orientation and fiber dispersion in the
⇑ Corresponding author. matrix [11–15]. Geethamma et al. investigated the dynamic char-
E-mail address: [email protected] (V.C. Mathapati).
acteristics of natural rubber and its composites reinforced with coir

https://doi.org/10.1016/j.matpr.2022.04.494
2214-7853/Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on Thermal Analysis and Energy Systems 2021.

Please cite this article as: V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al., Experimental study on dynamic mechanical properties of arecanut husk fiber
composite, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2022.04.494
V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

fibers. The authors observe that as frequency increased E00 and tan d 2. Materials and methods
values were decreased, whereas E0 values increased in both com-
posites. The damping factor peak correlates to the glass transition 2.1. Experimentation
temperature. As frequency increases, the Tan d curve shift to a
higher temperature [12]. Joseph et al. examined dynamic charac- In the present research, the materials required to prepare AHF
teristics of composites fabricated using treated and untreated short reinforced composites are arecanut husk fiber, Epoxy resin (L-
sisal fiber reinforced with polypropylene. The effect of frequency, 12), Hardener (K-6), and potassium hydroxide (KOH) pellets. The
chemical treatments, fiber length, fiber loading and temperature arecanut husk required to extract AHF was collected from arecanut
were investigated. The author observed that with increase in fiber plantation. The epoxy resin and hardener were purchased from
loading, both the values of E0 and E00 were increased. The effect of Atul polymers, Bangalore. The KOH pellets were used to prepare
fiber length revealed that for maximum dynamic and loss modulus KOH solution for alkaline treatment of arecanut husk fibers.
is maximal for 2 mm fiber length. Chemically treated composites
have higher E0 and E00 values than untreated composites due to
2.2. Composite sample preparation
improved fiber – matrix interfacial adhesion [13]. Even slight
changes in fiber’s physical and chemical characteristics lead to sig-
The sun dried arecanut husk was soaked in water for about
nificant variations in composite’s overall dynamic mechanical
three days to loosen the fibers then fibers were manually extracted
characteristics [16]. Muralidhar et al. studied the impact of loading
[20]. The extracted arecanut husk fibers were sundried for three
and temperature on values of E0 , E00 and tan d of the composites fab-
days to reduce moisture content. The AHF was treated with 6 %
ricated using epoxy resin reinforced with NaOH treated arecanut
KOH solution for 6 hrs. The fibers were thoroughly cleaned to elim-
husk fiber (AHF). The author observed the increase in values of E0
inate the chemical traces present on the surface and cleaned AHF
with increase in loading frequency, decrement in variation of E0
was sundried for 24 hrs. To reduce the absorbed moisture content
values with increase in frequency and concluded viscoelastic
[17,20]. The AHF composite panels were fabricated with 20 % fiber
behavior of composite material is impacted by a lot of factors such
loading. The hand lay-up method is used to prepare AHF composite
as frequency, evaluating time, and temperature [17]. Patra et al.
panels [21]. A mild steel mold having dimensions of 320 mm
provided a brief introductory overview of DMA and studied several
length and 320 mm width is used to prepare the AHF reinforced
characteristics of materials using DMA, such as microstructure,
epoxy resin composites [20]. The composite panels were made
damping, phase transitions, and complicated interactions in the
by using arecanut husk fiber and epoxy resin with weight fraction.
composite matrix. With increasing loading frequency, the dynamic
The (L-12) epoxy resin and hardener (K-6) were mixed thoroughly
modulus values increased and also observed that modulus values
in a container in the ratio 10:1 until it became uniform at room
decrease as the temperature rises. As the frequency increases, the
temperature. Treated and untreated AHF reinforced epoxy com-
tan d curve broadens. This widening is particularly noticeable in
posites were fabricated. The composite panel surface was cleaned
composites with high fiber content [18]. Pothan et al. carried a
with acetone and marked to cut the specimens required to perform
study to examine the impact of loading frequency, fiber content
dynamic mechanical tests as per ASTM standards. Specimen sam-
and temperature on dynamic characteristics of composites fabri-
ple for DMA test is shown in Fig. 1 for both untreated (U1) and
cated using banana fiber. The composites prepared with 40 % fiber
treated (T1). The dimensions of specimen U1 is 50.28  9.79  4.
content were observed to have maximum storage modulus also
78 mm and T1 is 50.13  10.24  4.13 mm.
with higher fiber loading, the glass transition values increased
[19]. In the present study effect of alkali treatment, frequency
and temperature on E0 , E00 and tan d of KOH treated and untreated 2.3. Multi–frequency DMA experiments
AHF composites were investigated. Even though some researchers
studied dynamic characteristics of various natural fiber compos- The viscoelastic behavior of composites is investigated by using
ites, very limited study on the composites fabricated using KOH Dynamic Mechanical Analyzer. The DMA tests can be performed in
treated and untreated AHF and effect of potassium hydroxide various modes with different control parameters such as controlled
treatment on the dynamic characteristics of AHF composites. AHF force/strain rate, multi-frequency, creep-recovery, multi-stress/
composite samples were fabricated with 20 % fiber loading and strain, is of strain mode, and stress relaxation [18]. DMA is a pop-
DMA technique has been used to examine the E0 , E00 , tan d and Tg ular method for analysis and characterization of composites with
values of untreated and potassium hydroxide (KOH) treated AHF respect to temperature, time, and frequency or combination of
reinforced composites at a heating rate of 3 °C per minute over these parameters by applying sinusoidal stress of constant ampli-
ramping temperature from 28 °C to 125 °C with multi-frequency tude to a sample of known geometry and measures strain induced
ranging from 1 to 10 Hz. in the material [14,17]. The composite sample can be subjected to

Fig. 1. DMA test specimen samples for both untreated U1 and treated T1 of AHF.

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V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 2. Schematic diagram of DMA instrument and test sample top view and side view.

Fig. 4. DMA testing of samples for treated T1 specimens.

Fig. 3. DMA testing of samples for untreated U1 specimens.

carried out on both specimens U1 and T1. The schematic diagram

controlled strain or a controlled stress [1]. In this study multi- of the instrument, test sample top view and side view are given
frequency mode is used to investigate stress/strain variations with in Fig. 2. The AHF composite specimens were subjected to dynamic
respect to frequency (1 Hz–10 Hz) while amplitude of oscillation loading by double cantilever mode using a DMA Q800 instrument.
remains constant over ramping temperature ranging from 28 °C This technique is used to determine elastic modulus E0 , E00 and Tan
to 125 °C at a heating rate of 3 °C per minute. The DMA test was d and comparing the same among the untreated and treated AHF
performed on untreated and treated AHF composite specimens in composites used in this study. And the DMA test setup is shown
accordance with ASTM-D4065 standards [22]. The DMA test was in Fig. 3 and Fig. 4 respectively.
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V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

3. Results and discussion The untreated and treated AHF composite sample storage mod-
ulus variation with temperature as a function of frequency ranging
3.1. Storage modulus (E0 ) from 1 Hz to 10 Hz is given in Fig. 5 and Fig. 6, respectively.
The untreated and treated AHF composite specimen storage
The storage modulus indicates the capacity of the material to modulus is 2.44 GPa and 2.61 GPa respectively for loading fre-
store and release energy during the cyclic loading and unloading quency of 1 Hz at 28 °C. The storage modulus has been increased
process. It is sometimes referred to as the elastic modulus. The by 6.97 % for the treated AHF composite specimen. It is obvious
storage modulus (E0 ) is generally used for determining elastic prop- that the values of the storage module increase with the alkaline
erties of the material [1,17]. The variation of storage modulus with treatment. The 6 % KOH treated fiber composite showed the max-
temperature obtained from the DMA test may be used to deter- imum value of the elastic modulus with alkaline treatment.
mine the stiffness of the material. Because it depends on several Untreated and treated AHF composites are able to retain their elas-
parameters such as fiber–matrix interfacial interaction, degree of tic properties up to a temperature of 70 °C, and later it transforms
cross linking, and molecular weight [19]. to viscous material, thereafter it shows a decrease in storage

Fig. 5. Storage modulus variation of untreated AHF composite with change in temperature and multi-frequency (1–10 Hz).

Fig. 6. Storage modulus variation of treated AHF composite with change in temperature and multi-frequency (1–10 Hz).

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V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

exhibit considerable variations. The interface region experiences

molecular rearrangement as frequency increases, resulting in an
increase in modulus values. Storage modulus measurements taken
over at high frequency yield higher results, whereas measurements
taken over low frequency give lower results. This is because the
material goes through molecular rearrangements in order to
reduce localised stresses.

3.2. Loss modulus (E00 )

The loss modulus of a material is a measure of its viscous

response that indicates energy lost as heat or dissipated during a
single cycle load of sinusoidal deformation. The Loss modulus is
used in determining the viscous properties of a polymer-based
material hence, it is also known as viscous modulus [17]. It
depends on phase lag between stress curve and strain curve. The
untreated and treated AHF composite sample loss modulus varia-
tion with temperature as a function of frequency ranging from
Fig. 7. Loss modulus variation of untreated AHF composite with change in 1 Hz to 10 Hz is given in Fig. 7 and Fig. 8 respectively.
temperature and multi-frequency (1–10 Hz). The loss modulus of untreated and treated AHF composite spec-
imen was found to be 314.7 MPa and 317.1 MPa for loading fre-
quency of 1 Hz. It can be observed that the peak of loss modulus
modulus. Up to 70 °C, the storage modulus remained consistent shifts to higher value with alkali treatment. The sudden increase
indicating the persistence of a good fiber–matrix interaction. For in loss modulus observed due to energy dissipation as a result of
both untreated and treated AHF composite samples, the storage intermolecular frictional forces. The peak of the loss modulus cor-
modulus reduces as the temperature increases from 28 °C to relates to the Tg. The material’s stored energy dissipates suddenly
125 °C, and the rate of reduction is not constant over the temper- at the glass transition zone resulting in a quick increase in loss
ature range. The storage modulus significantly reduced between modulus and reduction in storage modulus. The loss modulus of
70 °C and 80 °C, and these temperature value may be correlated untreated AHF composite suddenly increased at 70 °C, showing
to the glass transition state of the AHF composite. It can also be that the material’s behavior had transitioned from elastic to vis-
observed that storage modulus increases with increase in fre- cous. However, in the case of treated AHF composite, a sudden
quency, however there aren’t many significant changes for storage increase in loss modulus was observed at 78 °C. It may also con-
modulus values due to ramping temperature in both treated and clude that the KOH treatment increased the Tg of the composite.
untreated conditions when the frequency is increased from 1 to According to some authors, at temperature below Tg, peak values
10 Hz; beyond this frequency range, the storage modulus may of the loss modulus reduce as fiber content increases, whereas

Fig. 8. Loss modulus variation of treated AHF composite with change in temperature and multi-frequency (1–10 Hz).

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V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

sample Tan d variation with temperature as a function of fre-

quency ranging from 1 Hz to 10 Hz is given in Fig. 9 and
Fig. 10 respectively.
The tan curve peak shifts to higher values as frequency
increases and also to higher temperature. Hence, with the
increase in frequency, there is an apparent shift towards higher
glass transition temperatures. The tan d value of 6 % KOH treated
AHF composite was observed to be lower than that of untreated
AHF composite. Because of improved bonding, treated AHF com-
posite has a low tan d value due to strong and rigid interfacial
bonding between fiber and matrix which decreases molecular
mobility in the interfacial zone. As a result, molecular mobility
was significantly hampered and resulting in low damping proper-
ties. The lower peak value indicates good interfacial adhesion. The
tan-delta curve peak was shifted to a higher temperature after
the KOH treatment. This illustrates the effectiveness of KOH
treatment on composite that increases the glass transition
temperature.

Fig. 9. Tan-delta variation of untreated AHF composite with change in temperature

and multi-frequency (1–10 Hz). 3.4. Scanning electron microscope (SEM) analysis

SEM is an excellent technique to investigate the surface mor-

phology of epoxy composites reinforced with untreated and
treated AHF. Fig. 11a and Fig. 11b shows the SEM micrographs
modulus values increase as fiber content increases above Tg. [19]. of untreated and alkali-treated AHF composites. After treat-
The peak of the loss modulus curve which correlates to Tg, shifts to ments, components such as pectin, lignin, and others were
a higher temperature as frequency increases. removed from the raw AHF and also treated fibers were
observed to have comparatively rough surface. The removal of
3.3. Damping factor (Tan d) hemicelluloses, pectin, and lignin were attributed to the surface
morphologies of treated AHF. The SEM analysis micrographs
The damping factor is the ratio of the loss modulus to the stor- of composite surface of untreated AHF composite shows poor
age modulus. It is also known as Tan-delta, which is used to fiber – matrix interfacial bonding. Micrographs indicated fiber
determine glass transition temperature (Tg) of composite material pull out, debonding, fiber breakage and delamination. The
[23]. In a polymeric structure, the damping properties of the cracks were observed and cracks initiated from the fiber surface
material maintain the equilibrium between the elastic and vis- and propagated into the epoxy matrix in treated AHF compos-
cous phases. The storage and loss modulus are both affected by ites and also much less fiber pull out were observed indicating
the test specimen geometry, while the tan-d is a constant that the better interfacial adhesion between fiber and matrix due to
is unaffected by it. The untreated and treated AHF composite treatment.

Fig. 10. Tan-delta variation of treated AHF composite with change in temperature and multi-frequency (1–10 Hz).

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V.C. Mathapati, N. Muralidhar, B.R. Tulasiram et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 11. SEM micrographs a. untreated AHF composite surface b. treated AHF composite surface.

4. Conclusion Project administration. B.R. Tulasiram: Methodology,

Investigation, Writing – original draft. Muttana S. Balreddy:
Dynamic properties of epoxy composites reinforced with KOH Conceptualization, Methodology, Validation, Resources, Writing –
treated and untreated AHF were studied by using DMA with mul- review & editing.
tifrequency over ramping temperature. From the results of this
study treated AHF composites show improved storage modulus Declaration of Competing Interest
and loss modulus values as compared with untreated AHF compos-
ites. The storage modulus has been increased by 6.97 % for the trea- The authors declare that they have no known competing finan-
ted AHF composite specimen. cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
 The values of storage modulus of untreated and treated AHF
composites are 2.44 GPa and 2.61 GPa respectively for loading
Acknowledgement
frequency of 1 Hz at room temperature.
 The storage modulus increases with increasing loading fre-
We would like to thank Department of Civil Engineering, Sri Sid-
quency, and AHF composite samples exhibit improved elastic
dhartha Institute of Technology, (SSIT) for the support during the
characteristics at higher loading frequencies.
research work.
 The values of loss modulus of untreated and treated AHF com-
The authors declare no conflict of interests in the preparation of
posites are found to be 314.7 MPa and 317.1 MPa respectively
this article.
for loading frequency of 1 Hz at room temperature.
 The peak of loss modulus shifts to higher value due to KOH
treatment. The sudden increase in loss modulus observed due References
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