5th International & 26th All India Manufacturing Technology, Design and Research Conference (AIMTDR 2014) December

12th14th, 2014, IIT

Guwahati, Assam, India

DYNAMIC MECHANICAL AND THERMAL PROPERTIES OF

JUTE NANO FIBRE REINFORCED POLYMER COMPOSITE
K.T.B.Padal1*, S.Srikiran2, P. Surya Nagendra3
1*

Department Mechanical Engineering, Andhra University, Visakhapatnam, 530 003,

Email:[email protected]
2

Department of Mechanical Engineering, Kaushik College of Engineering,

Visakhapatnam, 530052, Email:[email protected]

Department of Marine Engineering, Andhra University, Visakhapatnam, 530003,

Email:[email protected]
ABSTRACT

A novel hybrid bio-composite is developed using bio-degradable Jute nanofibers reinforced in epoxy matrix.
Synthesis of the jute fibers was carried out using a high energy ball mill. The nanofibers used were of particle sizes
ranging from 10-30nm. The nano composites were processed using different weight percentages 0-5 wt. % of jute
nanofibers reinforced with epoxy polymer matrix by hand lay-up technique. The mechanical and thermal properties
of virgin (base) composite and nanocomposites (1-5wt.%) were compared using Dynamic Mechanical Analysis
(DMA), Thermo gravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC), DMA results revealed
that the storage modulus and loss modulus of these nano composites was improved, where as the mechanical loss
factor (tan delta) decreased. The nanocomposites were subjected to the heating cycle between 30C-600C to obtain
their thermal behavior and TGA measured test were conducted in the temperature range of 30C- 300C to identify
the thermal transition of the nanocomposites. The reinforcement of jute nanofibers in composite improves the
thermal stability. This enhancement of the stability and properties can be attributed to an improvement in the
interfacial adhesion and compatibility between the nanofibers and matrix.
Keywords: Jute nanofibers, epoxy resin, Dynamic mechanical analysis, Thermogravomentric analysis.

1 Introduction
The dispersion of nanosized fibres with in polymer
matrices can affect significantly their physical
properties. The main source of modification is due to
the interface macromolecular chains-nanofibre and to
the huge area of the nanofibres[1-6]. In nanocomposites
the physical properties of the interface become
dominant over the bulk properties of the polymer
matrices.
The addition of nanosized fibres to polymer matrix
typically enhances the thermal and thermo-oxidative
degradation of the polymer, the young modulus, and the
strength of the polymer matrix and affects the
crystallization process[7-10]. In most cases, the effect of
nanofibres consists in a rather modest increase of the
temperature at which the mass loss of the polymer is
highest. This parameter easily obtained by
thermogravemetric analysis (TGA) and Differential
scanning calorimetry (DSC) analysis can be considered

a fingerprint of the formation of a polymer nanofibre

interface.
The degradation of polymer composites may be
aggravated due to the interaction of a nanofibre with
polymer molecules in the presence of thermal energy
from working environments. These have been a
considerable amount of work on the thermal
degradation of polymers in nanocomposites[11-18].
Dynamic mechanical analysis is a thermal analysis
technique that measures the properties of materials as
they are deformed under periodic stress. In DMA a
variable sinusoidal stress is applied, and the resultant
sinusoidal strain is measured. If the material being
evaluated is purely elastic, the phase difference
between the stress and strain sine waves is 0 (i.e., they
are in phase). If the material is purely viscous, the
phase difference is 90. However, most real world
materials including polymers are viscoelastic and

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DYNAMIC MECHANICAL AND THERMAL PROPERTIES OF JUTE NANO FIBRE REINFORCED POLYMER COMPOSITE

exhibit a phase difference between those extremes

[18-25].
The nanocomposite system coatings can be
obtained by the traditional coatings technology, that is,
by filling with nanometric scale materials. Both
structural and functional properties of coatings can be
modified by filling with nanomaterials. The aim of the
work is to study the thermal degradation behavior,
viscoelastic properties of nanofibre reinforcement in
epoxy polymer matrix and to compare it with base
composite/nanofibre reinforced composites.

2. Experimental Work
2.1 Materials
Nanofibres were extracted from natural fibre Jute
by mechanical milling and chemical treatment. The
structural morphology and size was analysed by
Scanning electron microscope(SEM) and X-ray
diffraction .
Epoxy, one of the most commonly used materials is
the base polymer material for the present work.
Bisphenol-A epoxy resin (DGEBA) along with a
Triethylene Tetramine hardner (HY956) was used for
the investigations. Glass fibre woven plain fabrics were
supplied by M/s Ecmas Pvt Limited, Visakhapatnam.
The average fibre area weight (FAW) of glass fibre was
410 g/m2.

2.2 Characterization of Nano fibres

X-Ray diffractometer (Phillips make X Pert Pro
Diffractometer model) analyzed the nanofibres of jute at
a scanning rate 4/min with Cu, K radiation at 45 kv
and 40mA. The size of the jute fibres were determined
by using Scherrer formulae. The Scanning Electronic
microscope (SEM) images of jute fibres and
microfibrils were taken with JEOL model Scanning
Electronic microscope. It is observed that the obtained
jute fibres are micro to nano scale at different milling
hours.

samples for investigating the thermal properties as per

ASTM standards.
2.3.1 Thermal analysis of nanofibre composites.
The thermogravemetric analysis (TGA) is
commonly employed in research and testing to
determine the characteristics of polymer nanofibre
composites. This analysis is used to study the
degradation temperatures, absorbed moisture content of
materials, the level of inorganic and organic
components in materials, decomposition points of
explosives and solvent residues. It is also often used to
estimate the corrosion kinetics in high temperature
oxidation. The specimens were heated from room
temperature to 600C at heating rate of 10 C /min. For
comparing the effect of different weight percentages (15 wt.%)of jute nanofibre composites were also oven
aged in hot air at various temperatures for 10 min.
Differential Scanning Calorimetry (DSC) of base
composite and nanofibre reinforced with different
weights were carried out by using Pyris Diamond DSC
model Perkin Elmer apparatus. The present
investigation 5-10 mg of samples at scanning rate of
20C/min and temperature of 30C-300C under
nitrogen atmosphere. Subsequently, the samples were
held at 300C for 5 min and then cooled from 300C to
30C at the rate of 20C/min. Corresponding melting
temperature; heat of fusion and crystallization
temperature were recorded.
In DMA the Jute nanofibre composites of different
weight percentages (base composite and with 1 to 5
wt.% JNF/epoxy composite) specimen samples were
prepared as rectangular bars of size 40x10x3 mm3 as per
ASTM standards .The specimens are subjected to the
three point bending test method as shown in Fig.1

2.3 Preparation of Jute nanofibre

composites
The Jute nanofibres with varying percentage weight
(1wt.% to 5wt.%) reinforced in epoxy resins to prepare
nanofibre composites by hand lay-up technique. The
composites were prepared by using glass fibre woven
mat and epoxy resin with 50 wt.% / 50 wt.% fraction.
The epoxy resin is reinforced with different weight
percentage of Jute nanofibre reinforcing (0, 1, 2, 3, 4
and 5 wt. %) was mixed by using a mechanical stirrer at
750 rpm for 30 minutes at room temperature. Then, for
each 100 gm of epoxy resin, 12% of curing agent TETA
was added to the mixture by weight and thoroughly
mixed until it became uniform. Finally, the composite
is allowed to fully cure at room temperature for 24
hours. The finished laminate was used to prepare

Fig.1. Three point Bending Test set up

3. Results and Discussion

3.1Differential scanning calorimetry:
DSC monitors heat effects associated with phase
transitions and chemical reactions as a function of

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5th International & 26th All India Manufacturing Technology, Design and Research Conference (AIMTDR 2014) December 12th14th, 2014, IIT
Guwahati, Assam, India

temperature. Crystallization is a typical exothermic

process and melting a typical endothermic process. DSC
curves are used to obtain thermal information such as
the glass transition temperature, crystallization
temperature and melt temperature.
The DSC curves of base composite and 1 wt.% to 5
wt.% jute nanofibre reinforced composites were
compared in the temperature range of 30C to 300C to
determine the thermal transitions as shown in the Fig.
2. It can be seen that the glass transition temperature of
the nanocomposites did not change significantly due to
the addition of nano jute fibres, however the addition of
jute nanofibres did affect the crystallization behavior of
the polymer composite.

Fig.2. Comparision DSC curves of base composite

and nanofibre reinforced composites
The crystallization began at a higher temperature
71C for pure epoxy composite where as for all jute
nanofibre reinforced composites 72C to 75C. The
addition of nano jute fibres increased the crystallization
temperature Tc by up to 1C- 4C compared to the pure
epoxy composites. This result indicates that the
nucleating effect of jute nanofibres composites was
strengthened. The jute nanofibres played the role of
nucleating agent and facilitated crystallization. This is
due to stronger interaction between nano jute fibre
surface and chains. The nucleating effect of jute
nanofibre could also explain the increase of
crystallinity. The nano scale dispersion of the filler and
its orientation in the matrix are among these factors. All
the hybrid composites had a higher melting temperature
compared to pure epoxy composites.

3.2 Thermogravimetric analysis

The thermal degradation behaviour of pure epoxy
composite and Jute nanofibre reinforced polymer
composites with 1-5wt.% Jute nanofibre loading has
been employing by TGA curves as shown in figure. A
sudden drop in the mass of the sample indicates the
thermal degradation of the materials, however adding
the jute nanofibre in the matrix increased the

degradation temperature onset of the composites and

also increased the decomposition temperature.
From Fig.3, it is evident that the thermal
degradation of base composite is started at 344.2C and
100 % degradation was noticed at 560C. However with
the incorporation of jute nanofibres, there was
substantial enhancement in the thermal stability of the
nanocomposites with an initial degradation temperature
at 370C and final decomposition at 583C. This
indicates that a significant increase in the jute nanofibre
content of fibre reinforced composite play an important
role in controlling its rate of thermal degradation. The
major source of thermal stability improvement may be
due to the fact that a highly cross linked multilayer
epoxy matrix which produces additional intermolecular
bonding between fibre and matrix allowing more
thermal energy distributed over these bonds within the
interface

Fig.3. Comparision TGA curves of base composite

and nanofibre reinforced composites

3.3 Dynamic Mechanical analysis

DMA results of Jute nanofibre reinforcement with
pure epoxy Polymer composite. The influence of
percentage weight of 1% to 5% nanofibre reinforcement
has been studied using a Dynamic Mechanical Analysis.
The base composite and nanofibre composite samples
were subjected to dynamic mechanical analysis in order
to understand the nanofibre interaction in the composite
with the increase in percentage weight (1-5wt.%)
nanofibre. DMA results show that the changes in a
composite material, i.e storage modulus, loss modulus
and tan delta with increasing temperature may be able to
reveal a great deal about its thermal transition.
3.3.1 Storage Modulus
The Jute nanofibre composites with different
weight percentages were tested by the three point
bending method and the storage modulus comparison
graphs were shown in Fig.4. It is observed that the
nanocomposites show a slighty higher storage modulus
with the addition of nanofibres compared to pure epoxy

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DYNAMIC MECHANICAL AND THERMAL PROPERTIES OF JUTE NANO FIBRE REINFORCED POLYMER COMPOSITE

composites. The storage modulus of all the composite

samples dropped drastically between 65C 80C which
was their glass transition region. The glass transition
temperature of pure composite has been found to be
65C, whereas the transition temperature of Jute
nanofibre composites were at 70C 75C.
The storage modulus of Jute nanofibre
reinforced composite increases with an increased fibre
content in the glassy as well as rubbery region. This
observation is most likely related to the interaction
between the hydroxyl group of epoxy and hydroxyl
groups that are known to exist on damaged sites on the
Jute nanofibre surface or as a result of atomic scale
defects formed along Jute nanofibre composites. The
increase in glass transition also suggests that the degree
of interaction between the polymer chains and the
surface of the Jute nanofibre increase.

Fig.4 Comparsion of Storage Modulus vs

Temperature of base/ Jute nanofibre Composites
The storage modulus increases in the presence of
the Jute nanofibre which could be concluded as a
combined effect of the nanofibres embedded in a
viscoelastic matrix and the mechanical limitations. At
high concentrations the fibre reduces the mobility and
deformation of matrix, and in this case, the stress can be
transferred from the epoxy matrix to the Jute nanofibre
reinforcement.

3.3.2 Loss Modulus

The loss modulus value which reflects the amount
of viscous dissipation in the composites revealed some
interesting behaviour. The loss modulus is a function of
temperature (E") for both the pure epoxy and 1 to 5
wt.% of Jute nanofibre composites.

Fig.5 Comparsion of Loss modulus curves of base/

Jute nanofibre composites
Fig.5. shows the comparison between the loss
modulus vs temperature plots of the base/nanofibre
composite samples. The Tg of the Jute nanofibre
composites are slightly shifted to a higher temperature
with a broader range of the transition region than the
pure epoxy composite sample. As the loss factors are
sensitive to molecular motions it could mean that the
mobility of the polymer molecular chains decreases as
the chains were hindered by the nanofibre reinforcement
leading to shift of Tg. Good adhesion of Jute nanofibre
with the surrounding polymer matrix would additionally
benefit the dynamic modulus by hindering the
molecular motion to some extent. The loss modulus
increases with an increase in the percentage of Jute
nanofibre. This may be due to energy losses caused by
the rearrangements of the molecules and Jute nanofibre
as well as the internal friction between the Jute
nanofibre and the epoxy polymer matrix.

3.3.3 Tan Delta

The peak of the tan curve is a popular
measurement point for the Tg and it is usually easier to
isolate than to determine the onset of the drop in the
storage modulus. The tan verses temperature curve
can be used to determine much more about a system
than just its Tg. The width of the tan peak can indicate
how homogeneous a system. A system has very broad
peaks which are generally composed of different
polymer chain lengths or structures which gives rise to a
boarder temperature range, that initiate significant
viscous chain motions for the various components. On
the other hand, systems with narrow peaks generally
have a more narrow distribution of chain types and
molecular weights. The height or amplitude of the tan
curve is directly related to a materials ability to dissipate
energy through segmental motion. Systems with higher
tan peaks have higher ratios of energy absorbing
viscous motions and are therefore generally tougher
systems than those with low tan amplitudes.

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5th International & 26th All India Manufacturing Technology, Design and Research Conference (AIMTDR 2014) December 12th14th, 2014, IIT
Guwahati, Assam, India

damping). The DMA study indicates that the increased

modulus, together with the positive shift in tan delta
peak position, is attributed to the physical interaction
between the polymer and nanofibres that restrict the
segmental mobility of the polymer chains in the vicinity
of the Jute nanofibres.
Acknowledgement:
We acknowledge Naval Science and Technological
Laboratory, Visakhapatnam for providing Lab. facilities
for conducting a few experiments.

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Fig.6 Comparsion curves of Tan delta for base/ Jute
nanofibre composites
From Fig.6 it is noticed that the intensity of tan
peak decreased with an increase in Jute nanofibre
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The maximum damping parameter was observed as
0.220 of 5 wt% JNF composite and its improvement is
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might be due to the decrement of the mobility of
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which led to a reduction of height and sharpness of the
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4. Conclusions
The thermal properties of epoxy polymer filled with
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