Materials and Design 37 (2012) 111–121

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Materials and Design

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Influence of fibre treatments on mechanical properties of short Sansevieria

cylindrica/polyester composites
V.S. Sreenivasan a,⇑, D. Ravindran b, V. Manikandan c, R. Narayanasamy d
a
Department of Mechanical Engineering, Dr. Sivanthi Aditanar College of Engineering, Tiruchendur 628 215, Tamil Nadu, India
b
Department of Mechanical Engineering, National Engineering College, Kovilpatti 628 503, Tamil Nadu, India
c
S. Veerasamy Chettiyar College of Engineering & Technology, Puliankudi 627 855, Tamil Nadu, India
d
Department of Production Engineering, National Institute of Technology, Tiruchirappalli 620 015, Tamil Nadu, India

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

Article history: In the present study, to improve the interfacial bond between Sansevieria cylindrica fibres (SCFs) and poly-
Received 25 November 2011 ester matrix, chemical surface treatments have been performed on the fibres. Treatments including alkali,
Accepted 3 January 2012 benzoyl peroxide, potassium permanganate and stearic acid were carried out to modify the fibre surface.
Available online 12 January 2012
Raw and each type of treated SCF samples were utilised separately for fabricating the composites. The
mechanical properties of composites prepared from the chemically treated SCFs are found to be much
Keywords: better than those of the untreated ones. Potassium-permanganate-treated S. cylindrica fibre/polyester
A. Polymer matrix composites
(PSCFP) composites showed optimum mechanical properties among the treated S. cylindrica fibre/polyes-
E. Mechanical
G. Scanning electron microscopy
ter (SCFP) composites. The surface morphologies of fracture surfaces of composites were recorded using
scanning electron microscopy (SEM). The SEM micrographs reveal that interfacial bonding between
potassium-permanganate-treated SCF (PSCF) and polyester matrix has significantly improved, suggesting
that better dispersion of PSCF into the matrix has occurred upon potassium permanganate treatment of
SCF.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction
The ecological concern has resulted in a renewed interest in
natural polymeric materials. Natural fibres such as flax, hemp, sisal
and jute are interesting, eco-friendly alternatives to the use of glass
fibres to reinforce polymer-based engineering composites [1,2].
The advantages of natural fibre composites include high specific
strength and modulus, low cost, light weight, recyclability, biode-
gradability, lack of health hazards and non-abrasive nature [3,4].
The excellent price–performance ratio and low weight of natural fi-
bres combined with their eco-friendliness are very important for
their acceptance in large volume engineering markets, such as
the automotive, aerospace and building industries [5–7].
Unfortunately, some drawbacks of natural fibre composites
such as poor wettability and incompatibility of fibres with some
polymeric matrices, and high moisture absorption of fibres, make
them undesirable for certain applications. The main problem often
encountered is the fibre–matrix adhesion problem due to the
incompatibility between the hydrophilic natural fibres and the
hydrophobic polymer matrix. This problem may be rectified by
⇑ Corresponding author. Mobile: +91 94865 66704; fax: +91 4639 243188.
E-mail addresses: vssreenivasan@ymail.com (V.S. Sreenivasan), rmkv1@rediff
mail.com (D. Ravindran), vaimanikandan@yahoo.com (V. Manikandan), narayan@
nitt.edu (R. Narayanasamy).
chemically treating the fibre surfaces before fabricating the com-
posites [4]. Chemical treatment of fibres is a common method of
cleaning and modifying the fibre surface in order to lower the sur-
face tension and enhance the interfacial adhesion between a natu-
ral fibre and a polymeric matrix [8].
Rong et al. [9] analysed the effect of fibre treatment on the
mechanical properties of unidirectional sisal-reinforced epoxy
composites. They also reported that (i) fibre strength and (ii) the
adhesion between the fibre bundles and the matrix were improved
by alkali treatment of sisal fibres. Cantero et al. [10] studied the
effects of fibre treatment on the mechanical behaviour of flax/poly-
propylene composites. They observed that flax fibre composites
exhibited superior mechanical properties when treated with
maleic anhydride than when treated with vinyl trimethoxy silane.
Sreenivasan et al. [3] investigated the mechanical properties of
randomly oriented short SCFP composites. They invented the crit-
ical fibre length and optimum fibre weight percent of 30 mm and
40%, respectively for raw short SCFP composites. They also deter-
mined that a weak interfacial bond existed between raw SCFs
and a polyester matrix. Despite this weak interfacial bonding, the
mechanical properties of raw SCFP composites compared well with
other natural fibre and synthetic (glass) fibre composites. When
the interfacial bond between SCFs and the polyester matrix is
improved by suitable chemical treatments, the resulting SCFP
composites will surely provide superior mechanical properties [3].

0261-3069/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2012.01.004
112 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121
In the present work, an attempt was made to strengthen the
interfacial bond between SCF and polyester matrix. Different
chemical treatments such as alkali, benzoyl peroxide, potassium
permanganate and stearic acid treatments were given to SCF. The
chemical and mechanical properties of the chemically treated SCFs
were measured and compared with untreated SCFs (USCFs). Sepa-
rate composite plates were prepared using each type of chemically
treated SCFs. The tensile, flexural, impact, hardness and water
absorption characteristics of these composites were analysed and
compared with untreated SCFP (USCFP) composites. Based upon
the mechanical properties, the optimum chemical treatment for
short SCFP composite was identified and reported. SEM micro-
graphs were utilised to describe the failure modes of composites.
2. Experimental details
2.1. Materials
SCFs were separated from Sansevieria cylindrica leaves, which
were collected from farms around the city of Tirunelveli, Tamil
Nadu, India, by a mechanical process called ‘‘decortication’’.
Sreenivasan et al. [11] described the decortication method used
for extracting SCF from its leaves. The chemicals used for the
modification of SCF surface such as sodium hydroxide, potassium
permanganate, benzoyl peroxide, acetone, stearic acid and ethyl
alcohol were of commercial grade. The matrix used for the investi-
gation was commercially available unsaturated polyester, with the
trade name Satyan polymer. Methyl ethyl ketone peroxide (MEKP)
and cobalt naphthenate were used as curing catalyst and accelera-
tor. The chemicals, matrix, catalyst and accelerator were supplied
by M/s. Raja Traders, Tirunelveli, Tamil Nadu, India. The properties
of raw SCF [11] and unsaturated polyester resin [3] have already
been reported elsewhere.
2.2. Fibre surface treatments
The raw SCFs were subjected to different surface treatments
with alkali, benzoyl peroxide, potassium permanganate and stearic
acid. SCFs were chopped into 30 mm (critical fibre length) length
[3] before giving the treatment.
2.2.1. Alkali-treated SCF (ASCF)
The SCFs were soaked in a stainless steel vessel containing 10%
sodium hydroxide solution for 1 h. The fibres were washed thor-
oughly with water to remove the excess of sodium hydroxide on
the fibres. Final washing was done with water containing a little
acetic acid. Fibres were dried in an air oven at 70 °C for 3 h [12].
2.2.2. Benzoyl-peroxide-treated SCF (BSCF)
The ASCFs were soaked in 6% benzoyl peroxide in acetone for
half an hour. The fibres were then decanted and dried in air for
24 h [13].
2.2.3. Potassium-permanganate-treated SCF (PSCF)
The ASCFs were soaked in 0.5% potassium permanganate in ace-
tone for half an hour. The fibres were then decanted and dried in
air for 24 h [12].
2.2.4. Stearic-acid-treated SCF (SSCF)
In all, 1% stearic acid was dissolved in ethyl alcohol. The solu-
tion was then added dropwise to the ASCFs placed in a stainless
steel vessel with continuous stirring. These fibres were then dried
in an air oven at 80 °C for 45 min [13].
All the chemical treatments and their reactions are schematised
in Fig. 1.
2.3. Characterisation of chemically treated SCFs
The chemical and mechanical properties of fibre influence the
mechanical behaviour of fibre reinforced composites. It is essential
to study the chemical and mechanical properties of chemically
treated SCFs.
2.3.1. Chemical analysis of the chemically treated SCFs
The goal of this analysis was to determine the content of lignin,
cellulose, hemicelluloses, wax and moisture of the treated SCFs
using conventional chemical and XRD analyses.
The determination of the lignin content in the treated SCFs was
carried out according to the Klason method [14]. The cellulose con-
tent in the chemically treated SCFs was measured according to
Kurshner and Hoffer’s method [15]. The determination of hemicel-
luloses in the chemically modified SCFs was carried out according
to standard NFT 12-008 [16]. The wax content in the treated SCFs
was determined following the method developed by Conrad [17].
The moisture content in the chemically treated SCFs was deter-
mined using the procedure followed by Sreenivasan et al. [11].
X-ray spectra (scan range (2h) = 10–80°; h = diffraction angle;
scan speed = 5.0 deg/min) of the treated SCFs were obtained with
a Rigaku X-ray diffractometer D/Max Ultima III with an X-ray tube
producing monochromatic Cu Ka radiation. The integrated intensi-
ties of the Bragg peaks in the spectra of the chemically treated SCFs
were identified, and their crystallinity indices were estimated.
2.3.2. Tensile behaviour of the chemically treated SCFs
The treated SCFs were tested in dry conditions under tensile
loading at a gauge length of 10 mm in an INSTRON universal testing
machine of type 5500 R according to the ASTM D 3379 standard
[18]. Pneumatic grips were used to clamp the fibre with a pressure
of 0.4 MPa. A 1.0 kN capacity load cell was used to measure the load.
The displacement of the fibre was measured by a short-stroke
transducer with a resolution of approximately 0.1 lm. The tensile
tests were conducted with a cross head speed of 0.1 mm/min.
The average strain rate was on the order of 0.6 s1. To account for
the variability of the natural fibres, 20 samples were tested from
each type of chemically treated SCFs, and the average value was re-
ported. All testing was conducted at ambient temperature (21 °C)
and a relative humidity of about 65%.
2.4. Composite fabrication
The compression moulding method was adopted for the fabri-
cation of composites. Untreated and chemically treated SCFs were
used separately for fabricating the composites. USCFs were cut into
30 mm (critical fibre length) length [3]. Chemically treated SCFs
such as ASCF, BSCF, PSCF and SSCF are already possessing 30 mm
length. 40% (optimum fibre weight percent) weight [3] of SCFs of
a specific category (USCF/ASCF/BSCF/PSCF/SSCF) was randomly
spread between two mild steel plates. Extreme care was taken to
obtain a uniform distribution of fibres. A load of 40 metric tons
was applied on the mild steel plates by hydraulic compression to
form a single sheet. This compressed sheet was placed in a mould
with a size of 300 mm  150 mm  3 mm. Then, 97.5% of unsatu-
rated polyester resin was mixed with 2% MEKP (catalyst) and
0.5% cobalt naphthenate (accelerator). The prepared matrix solu-
tion was degassed before pouring. The degassed matrix solution
was applied on the compressed sheet by using a brush, and air
bubbles were removed carefully with a grooved roller. The mould
was closed, and hydraulic pressure was applied until complete
closure. The closed mould was kept under pressure for 24 h. The
composites were fabricated in the form of a flat plate with a size
of 300 mm  150 mm  3 mm. Composite plates were prepared
separately from SCFs of each category such as USCF, ASCF, BSCF,
 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121
Fig. 1. The chemical treatments used on SCFs were as follows: (a) alkali, (b) benzoyl peroxide, (c) potassium permanganate and (d) stearic acid.
PSCF and SSCF with critical fibre length (30 mm) and optimum fi-
bre weight percent (40%).
2.5. Mechanical tests for composites
Test specimens were cut from the composite plates as per the
ASTM standard. Tensile testing was carried out in a FIE universal
testing machine UTE-40 with a 400-kN capacity with a gauge
length of 100 mm and a cross head speed of 1 mm/min, as per
ASTM D 638-01 [19]. The three-point flexural properties were
determined by an INSTRON universal testing machine 4301 with
a 5-metric ton capacity, a gauge length of 50 mm and a cross head
speed of 1 mm/min, according to ASTM D 790-00 [20]. The Izod im-
pact test was done on unnotched specimens with a KARL FRANK
GMBH 53568 impact testing machine with a pendellange of
390 mm. The impact test was carried out with an impact speed
of 3.46 m/s and an incident energy of 2.75 J according to ASTM D
6110-97 [21]. The hardness of the composites was measured using
a Rockwell hardness testing machine, according to ASTM D 785-98
[22]. A minimum of six samples were tested in each case, and the
average value is reported. All testing was conducted at ambient
temperature (21 °C) and a relative humidity of about 65%.
2.6. Scanning electron microscopy
Fractography of the failure surface of composite samples were
examined using a scanning electron microscope, JEOL model
6390. The fractured portions of the samples were cut, and the
SEM micrographs were taken. A uniform coating of platinum was
given to the samples in order to make the surface conducting,
and then they were examined under the above microscope. The
secondary electrons were used for imaging. The surface of the frac-
tured specimens under tensile and impact tests were examined at
different magnifications.
113
2.7. Water absorption test for composites
In order to measure the absorption characteristics of the com-
posites, rectangular specimens were prepared having dimensions
of 39 mm  10 mm  3 mm. The specimens were dried in an oven
at 105 °C, cooled in a desiccator using silica gel and immediately
weighed. A Denver Instron balance was used for weight measure-
ment. The dried and weighed specimens were immersed in
distilled water according to ASTM D 570-99 [23]. The water
absorption tests were carried out by immersing the specimens
for 2 h and 24 h in hot and cold water, respectively. After immer-
sion, the excess water on the surface of the specimens was wiped
up using a piece of soft cloth and the final weights of the specimens
were then taken. The increase in the weight of the specimens was
calculated using the following equation:
Final weight  Origial weight  100
Water absorption ð%Þ ¼
Original weight
ð1Þ
3. Results and discussion
3.1. Characterisation of chemically treated SCFs
3.1.1. Chemical analysis of the chemically treated SCFs
The chemical composition of the untreated and treated SCFs is
reported in Table 1. The chemical composition of the fibre influ-
ences its properties, and in many ways, the fibres themselves can
be considered fibrous composite materials [24]. Cellulose and
lignin contents in the natural fibres act as reinforcement and
matrix, respectively. Generally cellulose has four basic types. They
are cellulose I, II, III and IV. The physico-chemical and mechanical
properties of natural fibres depend on its cellulose type, because
each type of cellulose has its own cell geometry. As cellulose is
114 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121

Table 1
Chemical composition of the untreated and treated SCFs.

Fibres Cellulose (%) Hemicelluloses (%) Lignin (%) Wax (%) Moisture (%) References
USCF 79.7 ± 1.51 10.13 ± 1.55 3.8 ± 1.15 0.09 ± 0.01 6.08 ± 1.51 [11]
ASCF 80.82 ± 1.33 6.91 ± 1.51 4.11 ± 1.32 0.07 ± 0.01 8.09 ± 1.64 –
BSCF 82.37 ± 1.23 8.33 ± 1.63 6.99 ± 1.64 0.06 ± 0.01 2.25 ± 1.32 –
PSCF 86.19 ± 1.55 2.99 ± 0.91 6.33 ± 1.19 0.03 ± 0.01 4.46 ± 1.24 –
SSCF 81.28 ± 1.19 3.65 ± 1.42 5.69 ± 1.33 0.05 ± 0.01 9.33 ± 1.46 –

the strongest (reinforcement) material in natural fibres, cellulose

content has an important influence on the mechanical properties
of natural fibres [25]. In general, fibre strength increases with
increasing cellulose content. As shown in Table 1, the USCFs con-
tained 79.7 ± 1.51% cellulose. From Table 1, it is also noted that
all the chemical treatments used in this research increased the
content of cellulose in SCFs, with the PSCFs possessing the highest
cellulose content of 86.19 ± 1.55%.
USCFs were composed of 10.13 ± 1.55% hemicelluloses. The
chemical treatments decreased the content of hemicelluloses in
SCFs. PSCFs had the lowest hemicelluloses content of 2.99 ± 0.91%.
The removal of hemicelluloses during chemical treatments affects
the tensile properties of natural fibres. When the hemicelluloses
are removed, the interfibrillar region in the natural fibre is likely to
be less dense and less rigid, and thereby makes the fibrils more capa-
ble of rearranging themselves along the direction of tensile deforma-
tion. When natural fibres are stretched, such rearrangements
amongst the fibrils would result in better load sharing by them
and hence result in higher tensile stress development in the fibre.
The lignin content influences the structure, morphology, tensile
strength and flexural rigidity of natural fibres [24]. When the nat-
ural fibres possess high lignin content, then it will have high tensile
strength and flexural rigidity. But the tensile strength of lignin is
less than that of cellulose. USCFs included 3.8 ± 1.15% lignin. From
Table 1, it is evident that the chemical treatments increased the
content of lignin in SCFs. The lignification was found to increase
the strength of the fibres [26]. BSCFs possessed the highest lignin
content of 6.99 ± 1.64%.
The wax content in the fibres affected the interfacial bond be-
tween the fibres and matrix during composite formation [11].
USCFs contained 0.09 ± 0.01% wax. The chemical treatments de-
creased the content of wax in SCFs, and PSCFs had the lowest
wax content at 0.03 ± 0.01%. USCFs contained 6.08 ± 1.51% mois-
ture. From Table 1, it is observed that the chemical treatments
increased the content of moisture in SCFs except in potassium per-
manganate and benzoyl peroxide treatments. BSCFs and SSCFs pos-
sessed the lowest and highest moisture content at 2.25 ± 1.32% and
9.33 ± 1.46%, respectively.

3.1.1.1. XRD analysis of the chemically treated SCFs. Fig. 2 displays

the X-ray spectra for the untreated and treated SCFs. From Fig. 2,
it is observed that all of the spectra contained two peaks that are
particularly well defined for natural fibres. The presence of these
diffraction peaks indicates that the untreated and treated SCFs
were semi-crystalline. According to several authors [27,28], the
two peaks situated at 2h = 15.4° and 2h = 22.5° can be attributed
to cellulose I and IV, both of which exhibit a monoclinic structure
[27–29]. The two peaks in all of the spectra (Fig. 2) are attributed to
the (2 0 0) and (1 1 0) crystallographic planes [27,30,31]. The crys-
tallinity index (CI) was estimated using the following expression
[32]:
Fig. 2. X-ray spectra of the untreated and treated SCFs.
H22:5  H18:5
CI ¼ ð2Þ
H22:5
where H22.5 is the height of the peak at 2h = 22.5°. This is due to the H18.5 is the diffracted intensity at 2h = 18.5° and is attributed to
contribution of both the amorphous and the crystalline fractions. the amorphous fraction [31,33]. The CIs of the untreated and treated
 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121
SCFs calculated using Eq. (2) are presented in Table 2. Compara-
tively, USCFs had the lowest CI of 60 ± 2% (Table 2). From Table 2,
it is noted that all the chemical treatments used in this research in-
creased the CI of SCFs, possibly because of an increased removal of
the fibre amorphous constituents during the treatments. PSCFs had
the highest CI of 82 ± 2% (Table 2). This result suggests that the crys-
tallites of PSCFs were more ordered than those of USCFs, ASCFs,
BSCFs and SSCFs. Zafeiropoules et al. [34] reported that acetylation
increased the CI of flax fibres. However, Marcovich et al. [35]
showed that the treatment of wood flour with maleic anhydride
led to a reduction of CI.
An estimate of crystallite size (CS) was performed using Scher-
rer’s formula [32]:
Kk
CS ¼
b cos h
where K = 0.89 is Scherrer’s constant, b is the peak’s full-width at
half-maximum and k is the wavelength of the radiation
[27,29,36]. The CSs of the untreated and treated SCFs computed
using Eq. (3) are reported in Table 2. The CS of USCFs was the lowest
at 86 ± 1 nm (Table 2). From Table 2, it is also clear that all the
chemical treatments used in this research increased the CS of SCFs.
PSCFs possessed the highest CS of 93 ± 2 nm (Table 2). This large
crystallite size of PSCFs reduced their chemical reactivity and water
absorption capacity [11].
3.1.2. Tensile behaviour of the chemically treated SCFs
Table 3 presents the tensile properties of the untreated and
treated SCFs. The effects of chemical treatment on the properties
of natural fibres depend on the type and concentration of the
chemical solution as well as the temperature and time of treatment
[9]. The chemical treatments used in this research led to an
improvement of tensile strength and strain to failure up to 24%
and 77%, respectively, but a decrease in Young’s modulus (Table
3). Compared with untreated fibres, the tensile strength was found
to be higher for all of the treated fibres. This result tends to show
that the chemical treatments reinforced the fibres. Moreover, the
fact that some substances were removed during the chemical
treatments led to an increase in the ratio of cellulose in the mate-
rial. This increased cellulose content improved the mechanical
properties of the fibres. It is interesting that PSCF showed a much
more significant increase in tensile strength (Table 3) because of
the increased quantity of cellulose (Table 1).
By comparing the Young’s modulus values of raw fibres with
the treated ones, it appears that the chemical treatments used in
this work reduced the stiffness of fibres (Table 3). This decrease
can be explained by considering that hemicelluloses, waxes, gums
and cementing materials that ensure cohesion between cellulose
microfibrils [8] are partially eliminated by the chemical treat-
ments. The partial removal of hemicelluloses, waxes and cement-
ing materials decreases the resistance of cellulose microfibrils to
stretching [9]. Thus, a decrease in the Young’s modulus was re-
corded in all the chemical treatments (Table 3) in comparison with
USCFs. From Table 3, it is also noted that all the chemical treat-
ments resulted in greater extensibility. This result suggests that
Table 2
Summary of XRD analysis of the untreated and treated SCFs.
Fibres CI (%) CS (nm) References
USCF 60 ± 2 86 ± 1 [11]
ASCF 62 ± 1 87 ± 1 – (iv) PSCFP composites and (v) SSCF/polyester (SSCFP) composites
BSCF 66 ± 1 89 ± 1 – are shown in Fig. 5a–e, respectively. From Fig. 5, it is evident that
PSCF 82 ± 2 93 ± 2 –
SSCF 73 ± 2 91 ± 2 –
115
SCFs become relatively ductile after the removal of some hemicel-
luloses, waxes and cementing materials.
Our results are in agreement with Bessadok et al. [37], who ana-
lysed the tensile performance of chemically treated agave fibres.
They also found that when compared with raw agave fibres, trea-
ted agave fibres increased in tensile strength and breaking strain
but decreased in tensile modulus.
3.2. Characterisation of chemically treated SCFP composites
3.2.1. Tensile properties
The dispersion and interfacial adhesion between the hydropho-
bic matrix and hydrophilic filler are the critical factors in determin-
ing the mechanical properties of composites. In the present study,
surface modification of the SCF was carried out to achieve better
ð3Þ
mechanical properties of composites and the results were com-
pared with those of the untreated ones. The effect of fibre treat-
ments on the tensile stress–strain behaviour of short SCFP
composites is shown in Fig. 3. It was found that the stress–strain
curve of cured pure polyester resin is similar to that of brittle
materials. The behaviour is elastic in nature. However, the addition
of fibres makes the matrix ductile, which is evident from the high
elongation at break value of all the short SCFP composites. The
stress value was found to increase non-linearly with strain in un-
treated and treated short SCFP composites. In addition the trans-
verse failure corresponding to the first cracking in the tensile
curve was recorded by USCFP composites (Fig. 3). This transverse
failure problem is no longer detectable in the stress–strain behav-
iour of treated short SCFP composites (Fig. 3), which helps to en-
hance the stability of the composites.
Fig. 4 represents the effect of fibre treatments on the tensile
properties of short SCFP composites. The tensile strength of cured
pure polyester resin is 33 MPa. Due to the incorporation of raw
SCFs into polyester matrix, the tensile strength of USCFP composite
is increased to 75.75 MPa. From Fig. 4, it is observed that the ten-
sile strength of treated SCFP composites is greater than that of
USCFP composites, due to the intrinsically increased strength of
treated SCFs. Among the treated SCFP composites, the maximum
tensile strength is recorded by PSCFP composites, manifesting the
existence of good interfacial bond between PSCFs and polyester
matrix.
From Fig. 4, it is clear that the extensibility of treated SCFP com-
posites is higher than that of USCFP composites, because of the in-
crease in extensibility of treated SCFs. The maximum extensibility
is registered by PSCFP composites (Fig. 4), as PSCFs have maximum
extensibility among the treated SCFs. The Young’s modulus of
cured pure polyester resin is 1 GPa (Fig. 4). Since the untreated
and treated SCFs have higher modulus than polyester matrix,
incorporation of untreated and treated SCFs into the matrix, has
improved the stiffness of untreated and treated SCFP composites.
As a result, Young’s modulus of the untreated and treated SCFP
composites is higher than cured pure polyester resin. From Fig. 4,
it is also noted that the treated SCFP composites have higher mod-
ulus than USCFP composites. Usually crystallites possess higher
modulus compared to amorphous substances [38]. When SCF is
subjected to different chemical treatments, crystallisation of SCF
surface dominates over its bulk nature, giving higher modulus of
treated SCFP composites. The maximum Young’s modulus is dis-
played by PSCFP composites (Fig. 4), as PSCFs have maximum CI
and CS among the treated SCFs (as shown in Table 2).
The tensile fractograph of (i) USCFP composites, (ii) ASCF/poly-
ester (ASCFP) composites, (iii) BSCF/polyester (BSCFP) composites,
all the short SCFP composites except PSCFP composites, failed in
the same fracture mechanism under tensile loading. It is also clear
116 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121

Table 3
Tensile properties of the untreated and treated SCFs.

Fibres Tensile strength (MPa) Young’s modulus (GPa) Strain to failure (%) References
USCF 656.72 ± 46 5.96 ± 5.5 11.03 ± 1.4 [11]
ASCF 721.82 ± 55 5.45 ± 3.6 13.24 ± 1.2 –
BSCF 766.19 ± 37 4.98 ± 2.5 15.37 ± 1.5 –
PSCF 811.73 ± 24 4.16 ± 2.8 19.51 ± 1.3 –
SSCF 793.28 ± 23 4.58 ± 2.4 17.33 ± 1.4 –

From Fig. 5d, it is noted that the wetting of PSCFs by the poly-
160
Cured pure polyester resin
ester resin was good due to the existence of minimum quantity
140 USCF/polyester composites of hemicelluloses and wax contents (refer Table 1) in the surface
ASCF/polyester composites of PSCFs. When the PSCFP composites were subjected to tensile
120 BSCF/polyester composites
Tensile Stress (MPa)

load, the cracks were initiated from the fibre–matrix interface

PSCF/polyester composites
100 SSCF/polyester composites
80
60
40
20
0 the ultimate tensile strength of PSCFs. From Fig. 5d, it is transpar-
0 2 4 6 8 10
Tensile strain (%)
Fig. 3. Effect of fibre treatments on the tensile stress–strain behaviour of short SCFP
composites.
that wetting of USCFs (Fig. 5a), ASCFs (Fig. 5b), BSCFs (Fig. 5c) and
SSCFs (Fig. 5e) by the polyester resin was very poor due to the pres-
ence of hemicelluloses and wax contents in the surface of USCFs,
ASCFs, BSCFs and SSCFs. Sreekumar et al. [39] reported that the
wax, hemicelluloses and pectin contents in the surface of natural
fibres prevented the wetting of fibre with matrix. When the tensile
load was applied on short USCFP/ASCFP/BSCFP/SSCFP composites,
fibres were debonded from the matrix. Consecutively, the fibres
were pulled out from the matrix, and then matrix and fibres were
fractured by the tensile force. In short USCFP/ASCFP/BSCFP/SSCFP
composites, fibre fracture was very small, and the predominant
failure mechanism was fibre pull-out. The voids were created on
the failure surface of composites due to fibre pull-out.
due to the heterogeneous connection. Then the cracks were prop-
agated along the matrix, as the tensile strength of matrix is lower
[3] than that of PSCFs. After that the adjacent fibres in the failure
plane of PSCFP composites were interconnected by the cracks.
After the complete fracture of the matrix in the failure plane of
PSCFP composites, the applied tensile load was totally carried by
PSCFs. Later the PSCFs were fractured in the failure plane of the
PSCFP composites, when the applied tensile load was greater than
12 14 ent that fibre/matrix debonding and fibre pull-out were hard to oc-
cur in PSCFP composites due to the existence of good interfacial
bond between PSCFs and polyester matrix. In short PSCFP compos-
ites, matrix and fibre fractures were the predominant failure
mechanisms.
Our results are in accordance with the findings of Varga et al.
[40]. They analysed about improving the tensile properties of
glass-fibre-reinforced polyester composites by the modification
of fibre surface. It was revealed that the tensile strength and exten-
sibility of polyalkenyl-poly-maleic-anhydride-ester-amide treated
glass fibre composites were improved by 38.9% and 25%, respec-
tively, than untreated glass fibre composites.
3.2.2. Flexural properties
The effect of fibre treatments on the flexural stress–strain
behaviour of short SCFP composites is presented in Fig. 6. As the
upper and lower surface of the specimen under three-point bend-
ing load are subjected to bending stress (compression and tension)
and the axisymmetric plane is subjected to shear stress, there are

160

141.91
140

120 Cured pure polyester resin

USCF/polyester composites
ASCF/polyester composites
100
BSCF/polyester composites
86.19 84.21
82.32 PSCF/polyester composites
80 75.75
SSCF/polyester composites

60

40 33

20
11.51 10 11.02 11.05 11.1 12.33 11.03
7.77 7.91 8 7.93
1.5
0
Tensile strength (MPa) Elongation at break (%) Young's modulus ( x 10-1 GPa)

Fig. 4. Effect of fibre treatments on the tensile properties of short SCFP composites.
 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121
Fig. 5. Tensile fractograph of (a) USCFP composites, (b) ASCFP composites, (c) BSCFP
composites, (d) PSCFP composites and (e) SSCFP composites.
117
160
140
Flexural stress (MPa)
120
100
80
60 Cured pure polyester resin
USCFP composites
40 ASCFP composites
BSCFP composites
20 PSCFP composites
SSCFP composites
0
0 2 4 6 8 10 12 14 16
Flexural strain (%)
Fig. 6. Effect of fibre treatments on the flexural stress–strain behaviour of short
SCFP composites.
two failure modes in materials: flexural and shear failure. The
specimen fails when the bending or the shear stress reaches the
corresponding critical value. Usually, the force–deflection curve
obtained by three-point bending is able to reveal the modes of fail-
ure [41]. That is: when the specimen fails so abruptly that the
curve is practically linear, it can be attributed to flexural failure
mode. When the specimen fails in the way that the slope of the
force–deflection curve decreases gradually to zero, shear failure
takes place. The appearance of a curve shown between these two
forms can be considered a result of mixed failure mode [42].
According to this criterion, it is clear that the contribution of flex-
ural deformation plays the leading role in untreated and treated
short SCFP composites (Fig. 6). From Fig. 6, it is noted that the un-
treated and treated SCFs introduce a plasticising effect on the brit-
tle polyester matrix. Thus, the untreated and treated short SCFP
composites have higher toughness. Due to the high extensibility
of SCFs, the untreated and treated SCFs can withstand the stress
applied and will prevent catastrophic failure of the untreated and
treated short SCFP composites.
Fig. 7 displays the effect of fibre treatments on the flexural prop-
erties of short SCFP composites. Treated SCFP composites are found
to show higher flexural strength and modulus compared to USCFP
composites, indicating that the chemical treatments performed on
SCFs improve stress transfer from the matrix to the fibre. Compar-
atively, the maximum flexural strength and modulus were regis-
tered by PSCFP composites (Fig. 7), manifesting that the existence
of good interfacial bond between PSCFs and polyester matrix. Our
findings are in agreement with Aziz and Ansell [43]. They studied
the flexural properties of untreated and alkali treated kenaf fibre
polyester composites. It was shown that the flexural strength and
modulus of alkali treated kenaf fibre polyester composites were
greater than that of untreated kenaf fibre polyester composites.
3.2.3. Impact strength
Impact resistance is the ability of a material to resist breaking
under a shock loading or the ability to resist the fracture under
stress applied at high speed [44]. The impact strength of compos-
ites is governed mainly by two factors: first, the capability of the
filler to absorb energy that can stop crack propagation and second,
poor interfacial bonding which induces micro-spaces between the
filler and the matrix, resulting in easy crack propagation [45,46].
The effect of fibre treatments on the impact strength of short SCFP
composites is demonstrated in Fig. 8. There is no significant change
in impact strength for ASCFP, BSCFP and SSCFP composites when
compared with USCFP composites, due to the existence of poor
118 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121

160
150.82

140 136.77
127.41

120

102.55 Cured pure polyester resin

100 USCFP composites
ASCFP composites
83.85
BSCFP composites
80
PSCFP composites
SSCFP composites
60

40.6
40

20 14.19 13.5
10.5 11.73 12.81 8.7 9.9 11 10
6 8
1.5
0
Flexuralstrength (MPa) Flexuralstrain (%) Flexuralmodulus (x10-1 GPa)

Fig. 7. Effect of fibre treatments on the flexural properties of short SCFP composites.

25 fibres can also be seen in the impact fractographs of USCFP

Cured pure polyester resin 23.41
USCFP composites
(Fig. 9a), ASCFP (Fig. 9b), BSCFP (Fig. 9c) and SSCFP (Fig. 9e) com-
ASCFP composites posites. Fig. 9d exhibits the existence of good interfacial bond be-
20
Impact strength (J/cm2)

BSCFP composites
PSCFP composites
SSCFP composites
15
9.45 9.55 10
10
5 very low.
0
0.4
Type of composite
Fig. 8. Effect of fibre treatments on the impact strength of short SCFP composites.
interfacial bonding between ASCFs/BSCFs/SSCFs and polyester
matrix. Poor interfacial bonding induces micro-spaces at the
fibre–matrix interface. These micro-spaces cause micro-cracks
when impact occurs. Micro-cracks result in crack propagation
under impact load. So a negligible change in the impact strength
of the composites is recorded.
The impact strength of PSCFP composites are found to be higher
(Fig. 8) than that of other treated SCFP composites, indicating that
better interfacial bonding between PSCFs and the matrix has oc-
curred upon chemical treatment. As a result, PSCFP composites
are capable of absorbing higher amount of energy to stop crack
propagation, compared to other treated SCFP composites. The
experimental impact strength observations are supported by
impact fractographs (Fig. 9). The impact fractograph of (i) USCFP
composites, (ii) ASCFP composites, (iii) BSCFP composites, (iv)
PSCFP composites and (v) SSCFP composites are shown in
Fig. 9a–e, respectively. From Fig. 9, it is evident that the untreated
and treated SCFP composites failed in their tensile fracture mech-
anism under impact load too.
It is also noted that poor interaction is existing between USCFs
(Fig. 9a)/ASCFs (Fig. 9b)/BSCFs (Fig. 9c)/SSCFs (Fig. 9e) and polyes-
ter matrix. It is evident from the figure that the untreated and trea-
ted SCFs except PSCFs, were easily pulled out from the matrix
during impact failure. When the applied impact stress exceeded
the strength of USCF/ASCF/BSCF/SSCF, then the fibres were frac-
tured. The fibre/matrix debonding, matrix fracture and fractured
tween PSCFs and polyester matrix. The impact fractograph of
PSCFP composites are encroached by fibre and matrix fractures.
But very few amount of fibre pull-out and fibre/matrix debonding
can also be seen in the impact fractograph of PSCFP composites
9.75 (Fig. 9d), due to the nature of sudden high speed impact load. Com-
pared to other treated SCFP composites, the amount of fibre pull-
out and fibre/matrix debonding recorded in PSCFP composites is
Our impact results are in accordance with Rahman et al. [47].
They investigated the charpy impact strength of untreated and
benzene diazonium salt treated abaca/polypropylene composites.
It is revealed that the impact strength of treated abaca/polypropyl-
ene composites is higher than that of untreated abaca/polypropyl-
ene composites.
3.2.4. Hardness
Hardness of a particular sample refers to its stiffness or resis-
tance of being broken to have its shape changed permanently
when load is applied to it. It is an indication of the composite to re-
sist crack propagation when subjected to a sudden impact. Hard-
ness of a composite depends on the distribution of the filler into
the matrix [46,48]. Usually, the presence of a more flexible matrix
causes the resultant composites to exhibit lower hardness [46]. As
shown in Fig. 10, incorporation of both treated and untreated SCFs
into the polyester matrix has reduced the flexibility of the matrix
resulting in more rigid composites. The hardness of treated SCFP
composites is greater than that of USCFP composites. The PSCFP
composites seem to have much better hardness compared to other
treated SCFP composites. This could be due to the better dispersion
of PSCFs into the matrix with minimisation of voids, stronger inter-
facial adhesion between the matrix and PSCF, and surface crystal-
lization (Maximum CI and CS of PSCFs among the treated SCFs (As
shown in the Table 2)) upon potassium permanganate treatment of
SCF.
Our outcomes are in concurrence with Islam et al. [49]. They
analysed the Rockwell hardness of untreated and benzene diazo-
nium salt treated coir/polypropylene composites. It was exhibited
that the hardness of treated coir/polypropylene composites was
greater than that of untreated coir/polypropylene composites.
 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121 119

120
Cured pure polyester resin USCFP composites
ASCFP composites BSCFP composites
PSCFP composites SSCFP composites
100 96
91 93 92
86

Hardness (Rockwell)
80
64
60

40

20

0
Type of composite

Fig. 10. Effect of fibre treatments on the hardness of short SCFP composites.

3.2.5. Water absorption characteristics

Water absorption behaviour of the SCFP composites in cold and
hot water immersion is shown in Fig. 11. Cold water was not ab-
sorbed by cured pure polyester resin. From Fig. 11, it is noted that
the hot water absorption of cured pure polyester resin is also neg-
ligible due to the absence of water absorbing elements in it. Com-
paratively, the maximum quantity of water both in cold and hot
state was absorbed by USCFP composites due to the presence of
micro voids. Yang and coworkers [50,51] reported that raw natural
fibre polymer composites show remarkable water absorption due
to the presence of micro voids. It has been reported that water
absorption can significantly be minimised if the filler is thoroughly
encapsulated by the matrix [52].
Chemically treated SCFP composites showed lower water
absorption tendency compared to those prepared with USCF. This
observation suggests that the hydrophilic nature of SCF has sub-
stantially decreased upon its chemical treatment with alkali, ben-
zoyl peroxide, potassium permanganate and stearic acid. This can
be described as the decrease in the number of hydroxyl groups
in the cellulose moiety during various chemical treatments. PSCFP
composites show minimum water absorption (Fig. 11) compared
to other treated SCFP composites. It can be attributed that due to
the favourable interaction between PSCFs and polyester matrix,
voids in the composites have largely minimised, showing lower
water absorption tendency of the PSCFP composites. As the maxi-
mum CS (93±2 nm) of PSCFs (Refer Table 2) reduces its water
absorption capacity, the water absorption nature of PSCFP compos-
ites also decreases.

60
Cured pure polyester resin
USCFP composites 51.11
50 ASCFP composites
BSCFP composites
PSCFP composites
Water absorption (%)

SSCFP composites
40

30 28.24

20
14.45
11.81
10.77
10 6.85
8.5
7.43 6.63
5.14

0 0.4
0
Cold water aabsorption Hot water absorption

Fig. 9. Impact fractograph of (a) USCFP composites, (b) ASCFP composites, (c) BSCFP Fig. 11. Effect of fibre treatments on the water absorption behaviour of short SCFP
composites, (d) PSCFP composites and (e) SSCFP composites. composites.
120 V.S. Sreenivasan et al. / Materials and Design 37 (2012) 111–121
Our findings are similar to the results of Rahman et al. [47].
They studied the water absorption behaviour of untreated and
benzene diazonium salt treated abaca/polypropylene composites.
It was identified that the water absorption of treated abaca/poly-
propylene composites was lower than that of untreated abaca/
polypropylene composites.
4. Conclusions
The following conclusions were drawn from the test results.
1. The mechanical properties of treated SCFP composites were
found to be greater than that of USCFP composites.
2. PSCFP composites possessed the maximum tensile strength and
modulus of around 142 MPa and 1.2 GPa, respectively among
the other treated SCFP composites. PSCFP composites yielded
the maximum flexural strength, flexural modulus, impact
strength and hardness, when compared with other treated SCFP
composites.
3. SEM analysis showed that the interaction between the USCFs/
ASCFs/BSCFs/SSCFs and polyester matrix is poor. The tensile
and impact fractographs of USCFP, ASCFP, BSCFP and SSCFP
composites showed that fibre/matrix debonding, fibre pull-
out, matrix fracture and fibre fracture occurred under tensile
and impact loading. It is also revealed from the tensile and
impact fractographs of PSCFP composites that the wetting of
PSCFs by the polyester resin was good. Matrix and fibre frac-
tures were predominant failure mechanisms in short PSCFP
composites under tensile and impact loading.
4. Comparatively the maximum quantity of water both in cold and
hot state was absorbed by USCFP composites. The chemical
treatments used in this research decrease the water absorption
tendency of SCFP composites. PSCFP composites showed mini-
mum water absorption when compared with other treated SCFP
composites.
5. Due to the existence of good interfacial bond between PSCFs
and polyester matrix, PSCFP composites provide superior
mechanical properties. From this research, it is revealed that
potassium permanganate treatment is the ideal chemical treat-
ment for SCFs to obtain optimum mechanical properties from
SCFP composites.
Acknowledgement
The authors thank the management of Dr. Sivanthi Aditanar
College of Engineering, Tiruchendur 628 215, Tamil Nadu, India,
for providing necessary assistance to carry out this research.
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