Dynamic Mechanical Properties of Sisal Fiber

Reinforced Polyester Composites Fabricated

by Resin Transfer Molding

P.A. Sreekumar,1,2 Redouan Saiah,2 Jean Marc Saiter,2 Nathalie Leblanc,3 Kuruvilla Joseph,4
G. Unnikrishnan,1 Sabu Thomas5
1
National Institute of Technology Calicut, NIT Campus P O, Calicut, Kerala 673601, India

2
Laboratoire Polymères, Biopolymères et Membranes, Unité CNRS 6522, équipe LECAP,
Institut des Matériaux Rouen, Université de Rouen, Faculté des Sciences,
Avenue de L’université BP 12, Saint Etienne du Rouvray 76801, France

3
Laboratoire de Génie des Matériaux de l’Aliment (LGMA), Esitpa, Rue Grande, BP 607,
Val de Reuil Cedex 27 106, France

4
Department of Chemistry, St. Berchmans’ College, Changanacherry P O, Kottayam, Kerala 686101, India

5
School of Chemical Sciences, Mahatma Gandhi University, Priyadarshini Hills P O, Kottayam,
Kerala 686560, India

The dynamic mechanical properties of sisal fiber rein- INTRODUCTION

forced polyester composites fabricated by resin trans-
fer molding (RTM) were investigated as a function of
fiber content, frequency, and temperature. Investiga-
tion proved that at all temperature range the storage
modulus (E') value is maximum for the composites
having fiber loading of 40 vol%. The loss modulus (E00 )
and damping peaks (tan d) were lowered with increas-
ing fiber content. The height of the damping peaks
depends upon the fiber content and the fiber/matrix
adhesion. The extent of the reinforcement was esti-
mated from the experimental storage modulus, and it
has been found that the effect of reinforcement is max-
imum at 40 vol% fiber content. As the fiber content
increases the Tg from tan d curve showed a positive
shift. The loss modulus, storage modulus, and damp-
ing peaks were evaluated as a function of frequency.
The activation energy for the glass transition increases
upon the fiber content. Cole–Cole analysis was made
to understand the phase behavior of the fiber rein-
forced composites. Finally, attempts were made to
correlate the experimental dynamic properties with
theoretical predictions. POLYM. COMPOS., 30:768–775,
2009. ª 2008 Society of Plastics Engineers
Correspondence to: Sabu Thomas; e-mail: sabut@sancharnet.in or
sabut552001@yahoo.com
DOI 10.1002/pc.20611
Published online in Wiley InterScience (www.interscience.wiley.com).
C 2008 Society of Plastics Engineers
V composites [10, 11].
Natural fibers are one of the cheap and renewable
resources of materials. They have good mechanical prop-
erties, low density, low cost, renewability, and biodegrad-
ability. In recent years, tremendous progress has been
achieved in the usage of natural fibers as reinforcement
in polymer matrixes. It is interesting to note that the per-
formances of these natural fiber composites are found to
be good in polymer matrices [1–9]. Sisal fiber, which is
used for the manufacturing of handicraft materials, is rel-
atively inexpensive and abundantly available in southern
part of India. Its mechanical properties are found to be
better than the other natural fibers. Natural fiber compo-
sites have some disadvantages such as poor ageing resist-
ance, moisture absorption, etc. Now a days, the natural
fiber reinforced polymer composites are very commonly
used in automotive applications. So it is essential to
make detailed investigation regarding its performance.
Dynamic mechanical analysis can be used to study the
performance of material over a wide range of tempera-
tures. A dynamical mechanical test measures the response
of a material as it is deformed due to a sinusoidal or
other periodic stress. Thomas and coworkers done exten-
sive work on the viscoelastic properties of natural fiber

POLYMER COMPOSITES—-2009
 Joseph et al. [12] have done dynamic mechanical anal-
ysis of short sisal fiber reinforced polypropylene compo-
sites. Gassan and Bledzki [13] carried out the dynamic
mechanical analysis of jute/epoxy composites and ob-
served an improvement in the dynamic modulus with the
incorporation of treated jute fiber in epoxy resin. Ray
et al. [14] studied the dynamic mechanical and thermal
analysis of vinyl ester resin matrix composites reinforced
with untreated and alkali treated jute fibers. They reported
that for all composites the storage modulus E0 decreased
with increase in temperature. The glass transition temper-
ature (Tg) increased for all the reinforced composites on
account of the restricted mobility of resin molecules in
presence of fibers. It was further observed that the very
high tan d value of the resin decreased in the composite
indicating that the addition of fibers lowered the damping
capacity of the polymers. In a recent study, Pothan et al.
[15] carried out the dynamic mechanical study of banana/
glass fiber woven fabric reinforced polyester composites.
In the earlier studies, natural fiber reinforced compo-
sites were fabricated by conventional methods such as
compression molding, hand lay up, etc [16–19]. Resin
transfer molding (RTM) which bridges the gap between
compression and handlay up are being widely used in the
fabrication of high structure applications. Most research
works in RTM were concentrated in the area of flow front
visualization, modeling of void formation, numerical sim-
ulations of curing, etc, using synthetic fibers [20–22]. Lit-
erature survey shows that limited studies have been
reported on the properties of composites fabricated by
RTM [23–25]. The dynamic mechanical analysis could
give a better understanding of the quality of composite
materials such as fiber/matrix adhesion, damping behavior
elasticity, the effect of temperature, etc. A number of
studies above mentioned have been reported on the
dynamic mechanical behavior of synthetic fibers and natu-
ral fiber reinforced polymer composites fabricated by
compression molding.
In this study, we report the effect of fiber content on
the viscoelastic properties sisal fiber reinforced polyester
composites fabricated by RTM. Fiber incorporation
caused a change in the entire properties of the polyester
resin, especially in the nature of storage modulus, loss
modulus, and tan d. More insight into the fiber/matrix
TABLE 1. Properties of sisal fiber.
Diameter (lm) 100–300
Density (g cm23) 1.450
Cellulose (%) 65–78
Hemicellulose (%) 10–14
Pectin (%) 10
Lignin (%) 9.9
Waxes (%) 2
Elongation at break (%) 4–9
Tensile strength (MPa) 365 6 5.2
Young’s modulus (MPa) 12,250 6 6.8
DOI 10.1002/pc
TABLE 2. Properties of isophthalic polyester resin.
Appearance Pale yellow color
Viscosity (cps) 650
Density (g cm23) 1.15
Elongation at break (%) 4.8
Tensile strength (MPa) 39 6 1.8
Young’s modulus (MPa) 968 6 4.07
Flexural strength (MPa) 61 6 2.26
Flexural modulus (MPa) 2,461 6 2.22
interaction from fiber treatment could be obtained based
on the damping peaks. Scanning electron micrograph has
been made to understand the fiber surface morphology af-
ter fiber incorporation.
EXPERIMENTAL
Natural fiber, sisal, was obtained from Sheeba Fibers
and Handicrafts, Poovancode, Tamilnadu, India. Isopthalic
polyester resin was purchased from Makson Enterprises,
Kottayam, Kerala, India. Important characteristics of sisal
fiber and isophthalic polyester resin are given in Tables 1
[26] and 2.
Preparation of Composites
Sisal fiber reinforced isophthalic polyester resin was
fabricated by RTM. After drying of sisal fibers at 708C,
mats of uniform thickness were prepared from chopped
sisal fibers having fiber length of 30 mm. The mats were
put in the mold. The mold was closed and vacuum was
applied. Isophthalic polyester resin mixed with 1 wt%
cobalt napthanate and 1 wt% methyl ethyl ketone perox-
ide was injected into the mold at an optimum pressure of
1 kg cm22. The mold is kept closed until the curing
occurs. Then, it is demolded and the composite samples
are post cured in an air oven at 808C for 4 h.
Dynamic Mechanical Analysis
The dynamic mechanical behavior of sisal fiber rein-
forced composites prepared by RTM was studied by using
TAQ-800 DMA instrument. The experiment was per-
formed under flexural mode. The testing temperature
ranged from 25 to 2008C and the experiment was carried
out at frequencies 0.1, 1, 10, and 20 Hz at a heating rate
of 18C min21. The percentage of the error for the results
was less than 2%.
SEM Analysis
Scanning electron microscope of JEOL 5400, Tokyo,
Japan was used to study the fiber/matrix interaction and
the fracture mechanism in the composites.
POLYMER COMPOSITES—-2009 769

FIG. 1. Storage modulus versus temperature curves of untreated sisal
fiber reinforced polyester composites.
RESULTS AND DISCUSSION
Effect of Fiber Loading
The storage modulus–temperature curve obtained dur-
ing dynamic mechanical test gives valuable insight into
the stiffness of a material as a function of temperature.
Storage modulus is a measure of the maximum energy
stored in the material during one cycle of oscillation. Fig-
ure 1 shows the variation of storage modulus (E0 ) of neat
polyester and various composites having different fiber
content as a function of temperature. Incorporation of
fibers causes a variation in storage modulus of compo-
sites. As the fiber content is increased, the storage modu-
lus value also increased till the composite having a fiber
loading of 40 vol% after that the value is decreased. In
the glassy region the fiber filled composites shows a
greater value as compared to cured polyester. The storage
modulus value for the composites varies as follows: Poly-
ester \ R20 \ R30 \ R40 [ R50. The composites hav-
ing a fiber loading of 40 vol% shows 19% greater value
when compared with composite having fiber content of
20 vol%. As temperature increased the decrease in modu-
lus value becomes lower due to incorporation of fiber. At
a temperature of 1208C, i.e. after the glass transition tem-
perature the storage modulus value decreases dramatically
but it follows the same order: Polyester \ R20 \ R30 \
R40 [ R50. The increase in storage modulus is due to
reinforcement imparted by fiber allowing stress transfer
from matrix to stronger fibers. At higher fiber loading,
there is a strong tendency for fiber–fiber interaction. This
leads to poor wetting of fibers and fiber dispersion. As a
consequence, the effective aspect ratio is reduced. Besides
in the case of composites fabricated by RTM, void con-
tent is very less because the mold is subjected to vacuum
and the resin is injected into it with an optimum pressure
in this process. The resin moves forward by pushing the
air content if any were left in the mold and the size of
770 POLYMER COMPOSITES—-2009
the entrapped air decreases due to the hydrostatic pres-
sure. The low void content is the main reason for the
increase in mechanical properties of composites fabricated
by RTM. Our earlier studies on the comparison of me-
chanical properties of composites fabricated by RTM and
compression molding indicated that RTM technique out-
performed the compression molding techniques in term of
mechanical properties and void content [26].
It can be seen that neat polyester shows a dramatic
decrease in E0 above the glass transition temperature. It is
interesting to note that the lowering of the modulus on
passing through the glass transition temperature is compa-
ratively less for sisal fiber reinforced composites as com-
pared to neat polyester resin. This can be attributed to the
combination of the hydrodynamic effects of the fibers em-
bedded in a viscoelastic medium and to the mechanical
restraint introduced by the fiber at the high concentra-
tions, which reduce the mobility and deformability of the
matrix. Other authors have also reported similar observa-
tions [27]. In principle, E0 is obviously influenced by fiber
stiffness and fibers have greater effect on the modulus
above Tg than below it.
The effectiveness of fillers on the moduli of the com-
posites can be represented by a coefficient, C [28] which
is given by:

C ¼ ðE0g =E0r Þcomp ðE0g =E0r Þresin ð1Þ
where E0g and E0r are the storage modulus values in the
glassy and rubbery region, respectively. The lower
the value of the constant C, greater is the effectiveness of
the filler. The measured E0 values at 30 and 1208C were
used as E0g and E0r , respectively. The values obtained for
different fiber loading is given in the Table 3. The lowest
value of C is obtained for the composites having fiber
loading of 40 vol% indicating the effective stress transfer
in the composites. The value increases to 0.20 at 50 vol%
of fiber because of poor dispersion and wettability at high
fiber loading.
Table 4 shows the variation of normalized storage
modulus of sisal fiber reinforced at different temperatures
40, 60, 90, and 1208C. It is noticeable that at lower fiber
loading i.e at 20 vol% and at lower temperature, the value
of normalized storage modulus is lower due to the poor
stress transfer and when the temperature increases the
modulus value also increases. Relative change in the
modulus is less pronounced at lower temperature, but at
higher temperature the presence of fiber and fiber/matrix
TABLE 3. The value of the constant C.
Materials C
R20 0.21
R30 0.16
R40 0.15
R50 0.20
DOI 10.1002/pc
TABLE 4. Variation of storage modulus (E0 ) and normalized storage TABLE 5. Tg of untreated sisal fiber reinforced polyester composites.
modulus of sisal/polyester composites with fibre loading at 40, 60, 90
and 1208C. Materials Glass transition temperature Tg (8C)

Normalized storage modulus Polyester 85

Storage modulus (MPa) (MPa) R20 86
R30 94
Material 408C 608C 908C 1208C 408C 608C 908C 1208C
R40 97
R50 92
Polyester 3,217 2,686 1,073 78 1 1 1 1
R20 3,081 2,414 1,273 581 0.95 0.89 1.18 7.44
R30 3,656 3,066 1,882 846 1.13 1.14 1.75 10.84
R40 3,798 3,264 2,162 858 1.18 1.21 2.01 11.0
R50 3,451 2,737 1,425 663 1.07 1.01 1.32 8.5
incorporation of fiber in polyester matrix increased the Tg
values of the composites and is maximum for the compo-
sites having a fiber loading of 40 vol% which have higher
fiber–matrix interaction.
interaction restricts the polymer flow. This restriction is Mechanical damping term (tan d) is the ratio of the
maximum for the composites having a fiber loading of loss modulus to storage modulus and is related to the
40 vol% which shows the maximum interaction with the degree of molecular mobility in the polymer material.
polymer matrix. At higher fiber content (50 vol%), the Figure 3 shows the variation of tan d of neat polyester
modulus value decreases due to fiber entanglement and resin and various composites having different fiber con-
poor fiber wettability. tent as a function of temperature. It is clear that the tan d
Figure 2 shows the variation of loss modulus (E00 ) of value is greater for the neat polyester resin. It is evident
neat polyester and various composites having different from the Table 6 that with the addition of the tan d value
fiber content as a function of temperature. Loss modulus decreases dramatically. As the fiber content increased the
is the measure of energy dissipated or lost as heat per peak of tan d moves towards higher temperature. The
cycle of sinusoidal deformation, when different systems are shift is maximum for the composite having fiber loading
compared at the same strain amplitude. They are more sen- of 40 vol% which also showed highest storage modulus
sitive to molecular motions. Here the addition of fiber values. It is interesting to note that for 50 vol% fiber
decreases the peak height and an increase in the peak composites the tan d does not show any shift to the high
width [29]. The modulus value increases with fiber con- temperature side. This is due to the fact that at high fiber
tent and is maximum at glass transition temperature. The loaded composites, poor fiber dispersion occurs and more-
difference in the physical state of the matrix surrounding over due to fiber entanglement and fiber–fiber interaction,
the fibers contributes to broadening of the loss modulus the fiber/matrix adhesion becomes poor. In turn, this will
curve. The width of the relaxation spectrum expresses the affect the damping nature of the composite. From the
diversity of chain segments and is expected to be higher Fig. 4a and b which represents the SEM of the composite
in three-dimensional polymers than in linear polymers having fiber loading of 20 and 40 vol%, it is clear that
[29]. The glass transition temperature obtained from the the adhesion between fiber and matrix is better for the
loss modulus curve is given in the Table 5. It is clear that composite having fiber loading of 40 vol%.

FIG. 2. Loss modulus versus temperature curves of untreated sisal fiber FIG. 3. Tan d versus temperature curves of untreated sisal fiber
reinforced polyester composites. reinforced polyester composites.

DOI 10.1002/pc POLYMER COMPOSITES—-2009 771

TABLE 6. Shift of Tg and tan d peakmax value of untreated sisal fiber
reinforced polyester composites.

Shift in glass transition

Materials Peakmax temperature Tg (8C)

Polyester 0.56 0
R20 0.21 3
R30 0.17 8
R40 0.15 11
R50 0.19 4

Effect of Frequency
Dynamic mechanical properties such as storage modu-
lus, damping peak, and loss modulus is affected by the
change in frequency. Figure 5a shows the variation of the
storage modulus as a function of frequency for the fiber
reinforced composites having a fiber loading of 40 vol%.
If a material is subjected to a constant stress its elastic
modulus is expected to decrease due to the molecular
rearrangement to minimize the localized stress. Here, as
the frequency increases there is an increase in storage

FIG. 5. (a) Effect of frequency on E0 of sisal fiber reinforced polyester

composites having fiber content of 40 vol%. (b) Effect of frequency on
E00 of sisal fiber reinforced polyester composites having fiber content of
40 vol%. (c) Effect of frequency on tan d of sisal fiber reinforced poly-
ester composites having a fibre content of 40 vol%.

modulus, otherwise modulus measurement over a short

time results in higher value and measurement taken over
a long period results in lower value. The effect of
FIG. 4. (a,b) SEM of the composites having 20 and 40 vol% fiber con- frequency on the loss modulus for the fiber reinforced
tent, respectively. composites having a fiber loading of 40 vol% is given in

772 POLYMER COMPOSITES—-2009 DOI 10.1002/pc

TABLE 7. Activation energy value of untreated sisal fiber reinforced
polyester composites.

Materials Activation energy (kJ/mol)

Polyester 296
R20 308
R30 323
R40 340
R50 271

Fig. 5b. As the frequency increased, the peak of the loss

modulus shifted towards higher temperature as well as
decreases the peak height also. The tan d value shows a
variation as the frequency changes since the viscoelastic
nature of the composites depends upon the fiber content,
fiber–matrix adhesion, frequency, and temperature. Figure FIG. 6. Cole–Cole plot for the untreated sisal fiber reinforced polyester
5c gives us a clear vision regarding the variation of tan d composites having various fiber content.
values as a function of frequency for the fiber reinforced
composites having a fiber content of 40 vol%. In this tan to be indicative of the nature of the system. Homogeneous
d peak is found to shift at higher temperature when the polymeric systems are reported to show a semicircle dia-
frequency is varied form 0.1 to 20 Hz. Higher tan d val- gram [32]. The Cole–Cole plot was drawn by plotting log
ues are found for measurement made at 10 Hz. Pothan of loss modulus (E00 ) against log of storage modulus (E0 ).
et al. [29] observed similar trend for the banana fiber rein- Figure 6 represents the Cole–Cole plot for sisal fiber rein-
forced polyester composite fabricated by compression forced composites having varying fiber content. In this
molding. figure the Cole–Cole plot are imperfect semicirlces. It is
The change in the vibrational frequency causes the due to the presence of heterogeneously dispersed fibers in
glass transition temperature to rise and the amplitude of the matrix.
the damping peak to increases. The shift of the transition
temperature allows one to calculate the apparent activa-
tion energy of the relaxation process for each of the sam- Theoretical Modeling of Viscoelastic Properties
ples assuming a linear equation of the type [30]. Thoeretical Prediction of Dynamic Modulus. The
storage modulus of the sisal fiber reinforced polyester
log f ¼ log f0 þ H=2:303RT ð2Þ
composite with varying fiber content was calculated theo-
Where f0 is an experimental constant, f and T are the retically using the equation proposed by Einstein [33]
measuring frequency and the temperature for the disper-
sion peak, respectively, R is a gas constant, and H is the Ec ¼ Em ð1 þ Vf Þ ð3Þ
activation energy. Activation energy of the different com- where Ec is the storage modulus of the composite; Em,
posite samples was calculated from the Arrhenius rela- the modulus of the matrix; and Vf, the volume fraction of
tionships. These values indirectly represent the filler–
matrix interaction and the values are given in Table 7.
We can see that activation energy values of the compo-
sites with 40 vol% fiber loading are the maximum which
have good fiber/matrix adhesion.
The magnitude of polarization within a material is rep-
resented by the dielectric constant, which can be repre-
sented by the Debye and Onsagar equations [31]. The sin-
gle relaxation peaks are inadequate to describe the visco-
elastic response of polymers. Cole–Cole is a particular
treatment of dielectric relaxation data obtained by plotting
E00 against E0 , each point corresponding to one frequency.
Structural changes taking place in crosslinked polymers
after fiber addition to polymeric matrices can be studied
using the Cole–Cole method. Here, the dynamic mechani-
cal properties when examined as a function of tempera-
ture and frequency are represented on the Cole–Cole com- FIG. 7. Experimental and theoretical storage modulus values of sisal/
plex plane. The nature of the Cole–Cole plot is reported polyester composites having a fiber content of 40 vol% at 308C.

DOI 10.1002/pc POLYMER COMPOSITES—-2009 773

the fiber in the composite. The modification Einstein
equation was done by several authors like Guth [34]
Ec ¼ Em ð1 þ 2:5Vf þ 14:1Vf2 Þ
The experimental and theoretical storage modulus of
sisal/polyester composites at 308C for different loadings
are given in Fig. 7. In this as the fiber content increases
all the curves shows an increasing trend. But the experi-
mental value shows an increase up to a fiber content of
40 vol% and decreases slightly. On comparison, experi-
mental values shows more resemblance with the Einstein
equation rather than Guth equation The deviation from
theoretical curve is due to the interaction between sisal
and polyester. It also increases with increase in fiber load-
ing as the number of reacting sites increases with increase
in fiber loading.
Theoretical Prediction of Damping Factor. In indus-
trial point of view, the damping behavior study of compo-
sites are very important and their predictive methods will
be beneficial for the polymer technologists. Rigid fillers
and fibers usually decreases the damping and is evident
from Fig. 3. The nature of tan d to a certain extent can be
predicted by rule of mixture equation [35].
tan dc ¼ Vf tan df þ Vm tan dm
In the case of rigid fillers first term can be neglected and
the equation becomes [36]
tan dc ¼ Vm tan dm
where the subscripts c and m represents composite and
matrix, Vm is the volume fraction of the matrix. In case
of composites, when additional constraint imposing on the
matrix can further reduce damping value. So, the above
equation can be modified by introducing the stiffness
term. The modification is based on the assumption that
FIG. 8. Experimental and theoretical tan d values of sisal/polyester
composites having a fiber content of 40 vol% at 308C.
774 POLYMER COMPOSITES—-2009
matrix in presence of fiber offers a stiffness equivalent to
the minimum elastic modulus of the composites. Then,
the equation becomes:
ð4Þ
tan dc ¼ Vm ðEm =Ec Þ tan dm ð7Þ
where the Em and Ec represents the storage modulus of
the matrix and composite.
Figure 8 represents the comparison of experimental and
theoretical values of tan d against different fiber loading at
0.1 Hz and at 308C. The value of experimental is not in
agreement with the theoretical prediction. The deviation is
due to the fact that both equation neglects the localized con-
straints imposed by the fibers on the matrix deformation
and also due to the heterogeneous nature of the composite.
CONCLUSIONS
The study on the dynamic mechanical behavior of
short sisal fiber reinforced polyester composites fabricated
by RTM revealed that the nature of composite depends
on the fiber content. The storage modulus showed a maxi-
mum for the composite having a fiber content of 40 vol%
which showed lower C value. The loss modulus curve
broadened as the fiber content increased when compared
with polyester. The tan d value is lower for the composite
having a fiber content of 40 vol% which reveals that bet-
ð5Þ ter adhesion is found between the fiber and matrix. The
SEM of the composite having fiber loading of 20 and
40 vol% supports the abovementioned. As the fiber con-
tent increased, the Tg value shows a positive deviation,
ð6Þ i.e. a shift towards higher temperature. Studies revealed
that frequency variation also affects the dynamic mechan-
ical properties. The Cole–Cole plots were imperfect semi-
cirlces which indicate the heterogeneous nature of the
composites. In theoretical modeling of the storage modu-
lus and damping factor, the experimental value shows
deviation due to the fiber/matrix interaction and heteroge-
nous nature. Finally, it is important to mention that good
fiber/matrix interaction could be obtained for the compo-
sites fabricated by RTM.
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