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COMPOSITES
SCIENCE AND
TECHNOLOGY
Composites Science and Technology 68 (2008) 631–638
www.elsevier.com/locate/compscitech

Effect of fiber surface treatment and fiber loading on the properties

of bagasse fiber–reinforced unsaturated polyester composites
V. Vilay a, M. Mariatti a,*
, R. Mat Taib a, Mitsugu Todo b

a
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Penang, Malaysia
b
Research Institute for Applied Mechanics, Kyushu University, Japan

Received 4 June 2007; received in revised form 7 September 2007; accepted 4 October 2007
Available online 23 October 2007

Abstract

Bagasse fiber is a residue of a sugarcane milling process. In this research, bagasse fiber has been used as reinforcing component for
unsaturated polyester resin (USP) to open up further possibilities in waste management. The chemical treatments using sodium hydrox-
ide (NaOH) and acrylic acid (AA) were carried out to modify the fiber properties. The effect of different fiber treatment and the fiber
content on the composite properties were investigated. At different fiber loadings, AA treated fiber composites shows better mechanical
properties compared to those of NaOH treated fiber composites. SEM investigations show that the surface modifications improve the
fiber–matrix interaction. Moreover, the storage modulus of dynamic mechanical analysis (DMA) indicated that NaOH and AA treated
fibers based composites enhance the storage modulus of the composites. From water absorption study, it was observed that the treated
fiber composites show lower water absorption properties compared to those of untreated fiber based composites.
 2007 Elsevier Ltd. All rights reserved.

Keywords: A. Polymer–matrix composites (PMCs); A. Fibers; B. Strength; B. Mechanical properties

1. Introduction
Fiber–reinforced plastic composites have played a dom-
inant role for a long time in a variety of applications for
their high specific strength and modulus. The manufacture,
use and removal of traditional fiber–reinforced plastic, usu-
ally made of glass, carbon or aramid fibers–reinforced ther-
moplastic and thermoset resins are considered critically
because of environmental problems. Recently, there has
been an increasing interest in the biodegradable plastic
composites using natural fiber reinforcement [1–4]. Natural
fibers have the advantages of biodegradability of low cost
and low density. If the low density of the natural fibers is
taken into consideration, then its specific stiffness and
strength are comparable to the respective quantities of
glass fibers. Some of the potential applications of natural
fiber reinforced composites include door and instrument
*
Corresponding author. Tel.: +60 4 5995262; fax: +60 4 5941011.
E-mail address: mariatti@eng.usm.my (M. Mariatti).
panels, package trays, glove boxes, arm rest and seat back
[1]. However, their high level of moisture absorption, poor
wettability by non-polar plastics, and insufficient adhesion
between untreated fibers and the polymer–matrix can lead
to debonding with age [3–5]. The careful choice of the fiber
and matrix pair, the fabrication method and manufactur-
ing procedures, the final application envisaged and the fiber
surface treatment is increasing the applications of natural
fiber reinforced composites [6,7].
Many investigations have been made on the potential of
the natural fibers such as flax, kenaf and jute reinforce-
ments for plastic materials [1–5]. Amongst those, bagasse
fibers are getting acceptance from many researchers and
it can be used as an alternative reinforcement in composite
materials. Bagasse is the residue left after the crushing of
sugar cane for juice extraction. Previous recast on bagasse
has suggested many value-added industrial products to
cater the needs in automotive, agriculture and other indus-
trial sectors [8]. Very few studies on the bagasse reinforced
thermosetting composites have been reported so far, hence

0266-3538/$ - see front matter  2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2007.10.005
632 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638
attempt has been made to study the properties of bagasse
fiber–reinforced unsaturated polyester (USP) composites.
In this work, the characterization of bagasse fiber and
bagasse filled USP were evaluated. Based from our previ-
ous work [9], the parameters for sodium hydroxide
(NaOH) and acrylic acid (AA) treatments on the bagasse
fibers were determined and vacuum bagging process was
carried out to fabricate the composite systems. The effect
of these two treatments and fiber content on the mechani-
cal, thermal and water absorption properties of untreated
and treated fiber based composites were studied.
2. Materials and methods
2.1. Materials
The bagasse was obtained from the local supplier, after
being processed to extract liquor. The fibers were soaked in
water for about two days, followed by drying at 80 C for
3 h. The fibers were then separated manually. Unsaturated
polyester P9509 obtained from Euro Chemo-Pharma Sdn.
Bhd. was used as matrix. Laboratory grade of methyl ethyl
ketone peroxide (55%) was used as hardener.
2.2. Chemical analysis
The chemical analysis carried out in Forestry Research
Institute of Malaysia (FRIM) using Technical Association
of Pulp and Paper Industry (TAPPI) standard [10].
2.3. Fiber treatments
The bagasse fibers were washed with water and dried in
an air oven for 72 h at 70 C. The dried fibers were desig-
nated as untreated fibers. The surface treatments using
NaOH and AA were then applied to the dried fibers.
2.3.1. Sodium hydroxide (NaOH) treatment
Bagasse fibers were soaked in 1% concentration of
NaOH solution for 3 h at room temperature [9]. Then the
fibers were washed several times to remove any NaOH
solution sticky to the fiber surface and the fibers were oven
dried at 70 C for 72 h [3].
2.3.2. Acrylic acid (AA) treatment
Bagasse fibers were immersed in NaOH solution for
30 min, and then soaked in 1% of acrylic acid (AA) solution
at room temperature for 1 h, then washing with distilled
water and dried in an oven for 72 h at the temperature of
70 C. According to Li et al. [1], this treatment method
showed good effects in improving the physical and mechan-
ical properties of flax fibers/polymer composites.
2.4. Composites preparation
In this study, 0, 10, 15 and 20 vol.% of treated and
untreated fibers were utilized in the preparation of the
composites. The bagasse fiber–USP composites were pre-
pared by vacuum bagging technique. The vacuum process
was carried out until the impregnation of the resin into
the fiber mat was completed, followed by curing process
in room temperature.
Formula (1) is utilized in the preparation of the
composites:
Wf
V f ¼ Wf
qf
ð1Þ
qf
þ Wqmm
where Wf is the weight of fiber, Wm is the weight of matrix,
Vf is the fiber volume faction and qm is the density of ma-
trix, qf is the density of fiber.
2.5. Testing
2.5.1. Mechanical properties
The tensile test method (ASTM D3822-01) was applied
to determine the tensile strength and Young’s modulus of
the fibers. Bagasse strand bundle were randomly chosen,
mounted and glued on a paper tab before measurement.
The testing was performed using Instron 3366 with the
sample gage length of 30 mm and crosshead speed of
5 mm/min. The tensile test and three-point flexural tests
of composites were carried out using Instron 3366 accord-
ing to the standard methods ASTM D3039 and ASTM
D790-98, respectively. The crosshead speed of the tensile
and flexural testings were set at 5 mm/min. The dimension
for tensile specimen is 60 mm long and 13 mm wide. The
span length:thickness ratio of the flexural sample is fixed
at 16:1. All the results were taken as the average value of
10 samples.
2.5.2. Water absorption of composites
The water absorption test using rectangular specimens
were cut with the dimensions of 30 · 28 mm (length · -
wide). The experiments were performed using test samples
unsealed on the sides (ASTM D570), in an attempt to rep-
licate the most aggressive in-use water absorption condi-
tion. The sample was oven dried at 50 C for 24 h to a
constant weight (M0). The specimens were then periodi-
cally taken out from tank; surface dried with absorbent
paper and weighed using an analytical balance with
0.1 mg precision (M1). The percentage weight gain at any
time t (percent water absorb, Mt), as the result of water
absorption was determined by using Eq. (2). The specimens
were immersed until saturated by averaged from four spec-
imens for each composite system.
M1  M0
M t ð%Þ ¼ ð2Þ
M0
where M0 is the dry initial weight, M1 is the weight after
immersion in water.
As pointed out by Fick’s law, the concentration gradient
is the driving force for diffusion and amount of the compo-
nent diffused is a function of time. In most cases, moisture
 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638
absorption processes often follow the prediction of Fick’s
law, where the mass of water absorbed increases linearly
with square root of time, and then gradually shows until
equilibrium plateau. The diffusion coefficient, D can be
determined from the following equation:
 2  2
h M2  M1
D¼p pffiffiffiffi pffiffiffiffi ð3Þ
4M m t2  t1
where Mm is the maximum moisture content, h is the thick-
ness of the sample, t1 and t2 are the selected points in the
initial linear portion and M2 and M1 are the respective
moisture content.
2.5.3. Dynamic mechanical analysis (DMA)
The dynamic mechanical properties of the resin and
composites were measured using a Mettler Toledo Model
DMA 861 under the flexural mode of testing. The dimen-
sions of the specimens were 50 mm · 13 mm · 4 mm. The
heating rate was set at 5 C/mm.
2.5.4. Scanning electron microscopy (SEM)
The field emission scanning electron microscopy
(FESEM) Leo Supra 35VP was used to identify the tensile
fracture morphology of the composite samples. The sample
surfaces were sputter coated with gold to avoid charging.
Fig. 1. SEM micrograph of the cross-section of: (a) untreated bagasse fiber, (b) NaOH treated fiber and (c) AA treated bagasse fiber (magnification 250·).
633
3. Results and discussions
3.1. Characterization of bagasse fiber
3.1.1. Chemical composition of fiber
The main chemical compositions of bagasse fibers
obtained from the chemical analysis are cellulose
(36.32%), hemicellulose (24.7%) and lignin (18.14%). In
general, the results obtained from the analysis are inaccor-
dance with the previous work [11]. However, it was realized
that the proportion of these components in a fiber depends
on the age, source of the fiber and the extraction conditions
used to obtain the fibers [8].
3.1.2. Morphology of bagasse fibers (treated and untreated
fibers)
Fig. 1 is the SEM micrograph of the cross-section of
untreated and treated bagasse fiber. Fig. 1a exhibits the cel-
lular structure of the fiber, which indicates the porous
structure. According to Reddy and Yang [8], in general
all natural cellulose fibers are multi cellular, where a bundle
of individual cells bound by natural polymers such as lignin
and pectin. The fiber used in this study refers to a bundle of
individual cell. The hollow cavity called lumen exists in unit
cell of the biofibers. The presence of the hollow lumen
634 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638

decreases bulk density of the fiber and acts as acoustic and
thermal insulators. The NaOH and AA treatments (Fig. 1b
and c) revealed a compressed cellular structure. In other
words, the treatment destroyed the cellular structure of
the bagasse fiber, hence reduced the void content of the
fiber.
3.1.3. Tensile properties of bagasse fiber
From the tensile test results (Table 1), it is observed that
the treatment improves the tensile properties of the fibers.
All treated fibers have higher tensile strength, modulus
and elongation at break than those of untreated fibers, with
obvious higher properties shown in AA treated fibers.
3.2. Properties of bagasse fiber–polyester composites
The most important factor to obtain a good fiber rein-
forced composites is the adhesion between matrix polymers
or the fiber and interphase properties. Due to the presence
of hydroxyl group in natural fibers, the moisture absorp-
tion is high which leads to poor wettability and weak inter-
facial bonding between fibers and hydrophobic matrices.
Therefore, in order to develop composites with better
mechanical properties, it is necessary to impart hydropho-
bicity to the fibers by suitable chemical treatments [4]. The
Table 1
The average tensile properties of untreated and treated bagasse fibers
Fibers Tensile strain at Average tensile
break (%) strength (MPa)
Untreated 4.03 ± 2.41 96.24 ± 29.95
fiber
NaOH 5.84 ± 2.64 156.88 ± 45.46
treated
fiber
AA treated 5.59 ± 3.44 229.01 ± 35.56
fiber
surface modification of bagasse would not only decrease
the moisture absorption, but would improve the wettability
of fiber and matrix at interphase region hence subsequently
improve the mechanical properties of the composites.
Figs. 2 and 3 show the effect of treated and untreated
bagasse content at 0, 10, 15 and 20 vol.% on tensile and
flexural properties of the composites, respectively. The ten-
sile and flexural properties of the resin at 0 vol.% of fiber
are used as control. It is observed that the use of treated
bagasse fiber from 10 to 20 vol.% improved the tensile
and flexural properties of the polyester composites. The
superior mechanical properties of AA and NaOH treated
bagasse based composites as compared to untreated
bagasse based composites are attributed to the fact that
treatment improves the fiber surface adhesives characteris-
tics by fibrillation process [12].
Fig. 4 compares the SEM micrographs of untreated,
NaOH and AA treated fibers. The SEM micrograph of
untreated fiber (a) showed the presence of waxy substances
on the untreated fiber surface. According to Mohanty [13],
such waxy substance contributed to ineffective fiber–matrix
bonding and poor surface wet out. Micrographs (b) and (c)
indicate that the chemical treatments smoothed the fiber
surface especially using NaOH treatment. The NaOH trea-
ted fiber surface appears clean and smooth with little sur-
face debris and overgrowths compared with AA treated
fiber. According to Cao et al. [14], the fibers in the
untreated fibers were packed together but got split after
Average tensile the treatments. The phenomenon is called as fibrillation,
modulus (GPa) which breaks the untreated fiber bundle down into smaller
6.42 ± 1.16 ones by dissolution of the hemicellulose. The fibrillation is
reported to increase the effective surface area available for
7.13 ± 0.99
contact with the matrix [3], and hence the interfacial was
improved.
8.09 ± 1.43 Fig. 5 shows the fracture photomicrographs of the spec-
imen subjected to tensile loads. It can be seen in Fig. 5a for

a Untreated fiber composites b Untreated fiber composites

NaOH treated fiber composites NaOH treated fiber composites
AA treated fiber composites 5500 AA treated fiber composites
37
Polyester Polyester
Tensile Modulus (MPa)
Tensile Strength (MPa)

4500
33

3500
29

25 2500

21 1500

17 500
0 10 15 20 0 10 15 20
Fiber loading (%) Fiber loading (%)

Fig. 2. The (a) tensile strength and (b) tensile modulus of treated and untreated fiber composites at different fiber loadings. Unfilled polyester resin is used
as a control.
 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638 635

a Untreated fiber composites b 7500 Untreated fiber composites

NaOH treated fiber composites NaOH treaed fiber composites
80 AA treated fiber composites AA treaed fiber composites
Polyester

Flexural Modulus (MPa)

Flexural Strength (MPa) Polyester 6500
70
5500
60
4500
50

3500
40

30 2500

20 1500
0 10 15 20 0 10 15 20
Fiber loading (%) Fiber loading (%)

Fig. 3. (a) Flexural strength and (b) flexural modulus of treated and untreated fiber composites at different fiber loadings.

Fig. 4. SEM micrographs of fiber surface of: (a) untreated fiber (500· magnification), (b) NaOH treated fiber (500· magnification) and (c) AA treated
fiber (300· magnification).

Fig. 5. SEM photomicrographs of tensile fracture surface of: (a) untreated fiber based composites; (b) NaOH fiber based composites and (c) AA fiber
based composites at 80· magnification.
636 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638

untreated bagasse fiber based composites, the phenomenon
of pull-out fibers occurred in greater extent than those of
treated fiber based composites. It could be observed that
in NaOH treated based composites (shown in Fig. 5b),
the fibers are still embedded in the resin together with some
cavities left by pulled-out fibers. It is interesting to note
that there is little evidence of fiber pulled-out in the AA
treated fibers based composites, which indirectly indicating
better adhesion exists at the interphase.
Fig. 6 shows the dynamic storage modulus (E 0 ) and tan
delta (d) for polyester resin and 20 vol.% of untreated,
NaOH and AA treated fiber based composites, plotted
against temperature. From the DMA curves, the E 0 values
fall steeply around the glass transition temperature (Tg) of
the resins. The E 0 values were higher for treated fiber based
composites compared with those of untreated fiber com-
posites and unfilled resin. For example at 35 C, the E 0 of
polyester resin is about 1800 MPa. By incorporation of
untreated fibers, the E 0 value increasing up to 2750 MPa.
While the NaOH and AA treated fiber composites exhibit
higher E 0 values such as 2900 MPa and 2780 MPa, respec-
tively. These results indicate that the fiber modified by AA
and NaOH treatments exhibited better compatibility with
the polyester resin than the untreated fibers. This is in
accordance with the explanation by Aziz et al. [15] where
higher E 0 value of treated kenaf–polyester composite is
due to greater interfacial adhesion and bond strength
between resin and fiber. From the DMA curves, incorpora-
tion of treated fibers imparts stiffness to the composite
material, the similar trend was observed in the static flex-
ural modulus shown in Fig. 3. From the plot of tan d in
Fig. 6b, it is observed that for the AA treated fiber based

a Resin 20 vol.% Untreated fiber composites

20 vol.% NaOH treated fiber composites 20 vol.% AA treated fiber composites

4500

4000
Storage Modulus (MPa)

3500

3000

2500

2000

1500

1000

500

0
32 52 72 92 112 132 152 172 192
Temperature (°C)

b 20 vol.% AA treated fiber composites

20 vol.% NaOH treated fiber composites
20 vol.% untreated fiber composites
Resin
0.9

0.8

0.7

0.6
Tan delta

0.5

0.4

0.3

0.2

0.1

0
30 50 70 90 110 130 150 170
Temperature (°C)

Fig. 6. (a) Dynamic storage modulus and (b) tan d for resin (as control), 20 vol.% of untreated and treated fiber based composites.
 V. Vilay et al. / Composites Science and Technology 68 (2008) 631–638 637

composites the tan d peak, assigned as the glass transition Table 2

of polyester, slightly shifted to higher temperature. Accord- The water absorption behavior of polyester and 20 vol.% of treated and
untreated fiber composites
ing to Nishino et al. [16], this phenomenon is due to a
strong interaction between the treated bagasse fiber and Specimens D (·1011) m2 s1 Tm (h) Mm (%)
the polymer resin, which decreases the polymer chain Polyester 1.39 720 4.48
mobility. Similarly, report by Aziz et al. [17] indicates that Untreated fiber composite 91.8 720 12.18
NaOH treated fiber composite 1.34 720 8.08
the incorporation of stiff fibers reduces the tan d peak by AA treated fiber composites 1.58 720 7.09
restricting the movement of polymer molecule.
Typically absorption curves showing weight gain as a
function of exposure time in water at room temperature With better adhesion between matrix and fibers, the velocity
for polyester and composites are shown in Fig. 7. In all of the diffusional processes decreases since there are less
cases, the water absorption process is sharp at the begin- gaps in the interfacial region. According to Li et al. [1],
ning and leveled of for some length of time where it chemical treatments of natural fibers can reduce the hydro-
approaches to equilibrium. It is considered that the change xyl group in the cell wall of natural fibers, thus decreasing
of weight gain for all samples is a typical Fickian diffusion the water absorption of the composites. The Mm values of
behavior. The composites show lower water absorption untreated fiber composites are higher compared to treated
than polyester resin. It is apparent that the acrylic acid fiber composites. Poor adhesion between fiber and matrix
and NaOH treatments of bagasse fibers reduced the water can cause increasing value of Mm [19]. The saturation time
uptake of the composite system. As shown, chemical treat- (Tm) is insignificantly influenced by the treatment of fibers.
ment can reduce the hydroxyl group in the cell wall of the
natural fiber molecule, thus decreasing the water absorp- 4. Conclusions
tion of the composites. The result of water uptake however
is in accordance with previous work by Fraga et al. [18] on
their study on jute–fiber unsaturated polyester composites. • Addition of higher amount of fiber results in higher ten-
However, it should be reiterated that water absorption in a sile and flexural properties of the bagasse fiber–rein-
fibrous composites is dependent on temperature, fiber forced polyester composites.
loading, orientation, permeability of fiber, surface protec- • Higher tensile and flexural properties were obtained for
tion, area of the exposed surfaces, diffusivity, etc [19]. treated fiber composites compared to those of untreated
According to Das et al. [20], initially, water saturates the fiber based composites, with significant trend shown by
cell wall of the bagasse fiber, and next, water occupies void AA treated fiber based composites.
spaces. • Chemical treatments via NaOH and AA decreased the
Table 2 summarizes the diffusion coefficient (D), time water absorption of composites, and increased the stor-
needed reach saturation time (Tm) and moisture content at age modulus and Tg of the composites.
saturation level (Mm) of the variables. From the D values
of the composite samples, it was found that the NaOH
and AA treated fiber polyester composites has better resis- Acknowledgements
tance towards water absorption than those of untreated
fiber composites. Untreated fiber polyester composites show The work was funded by AUN/SEED-Net and JICA.
the highest D values. Higher D value might also indicate The authors greatly acknowledged the support from Uni-
higher void content in the system where void generates more versiti Sains Malaysia.
pathways for water to start diffusing into the composite.
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