Extraction of Fibers from Saccharum munja Grass

and Its Application in Composites

Girendra Pal Singh,1 Pallavi Vishwas Madiwale,1 Ramanand N Jagtap,2 Ravindra V Adivarekar1
1
Department of Fibres and Textile Processing Technology, Institute of Chemical Technology, Matunga,
Mumbai 400019, Maharashtra, India
2
Department of Polymer and Surface Coating Technology, Institute of Chemical Technology, Matunga,
Mumbai 400019, Maharashtra, India
Correspondence to: R. V. Adivarekar (E - mail: [email protected])

ABSTRACT: With growing environmental awareness, ecological concerns and new legislations, natural fiber-reinforced plastic compo-
sites have received increasing attention during the recent decades. The natural fiber composites have many advantages over traditional
glass fiber composites, including lower cost, lighter weight, environmental friendliness, and recyclability. This article reports the find-
ings of the studies done on a new fiber, hitherto unexplored, extracted from Saccharum munja grass. The extracted fibers were further
treated using sodium hydroxide to improve its performance in composites. Both treated and untreated fiber-reinforced composites
were prepared by hand lay-up process using unsaturated polyester resin. Mechanical properties and thermal behavior of the compo-
sites were evaluated. The improvement in properties was found for alkali-treated fiber composites. V C 2014 Wiley Periodicals, Inc. J. Appl.

Polym. Sci. 2014, 131, 40829.

KEYWORDS: cellulose and other wood products; composites; mechanical properties

Received 22 January 2014; accepted 6 April 2014

DOI: 10.1002/app.40829

INTRODUCTION matrix. The insufficient interface can be owing to the presence of

lignin and other covering matter on the natural fibers. This
Fiber composite materials such as glass fiber, carbon fiber, and
makes the fibers inaccessible for matrix bonding. The surface
aramid have been widely used in automotive, marine, aerospace,
modification of the fibers by chemical treatment is the solution
aircraft industries, and are now being used in structural and
worked on and is one of the largest areas of current research.
infrastructure application such as windmill, roof, bridge, girder,
railway sleepers, and floating river walkway.1 Because of their Different studies have been carried out on different fibers to
excellent tensile, toughness and thermal resistance properties, overcome the hurdle. Hemp, sisal, jute, and kapok natural fibers
and their hydrophobic nature, composite has variety of applica- were modified by using mercerization and acetylation and
tions. Various types of composites can be engineered according improved the performance of natural composites by promoting
to their applications. But limitations for the fibers in vogue are better fiber to resin bonding.3 The effect of alkali treatments on
their high cost, nonrecyclability or biodegradability, and supply the flexural properties of polyester matrix composite reinforced
chain management. These limitations forced researchers to pay with alfa fibers was studied and it was found that flexural
attention to more eco-friendly fibers. It was found that the use strength and flexural modulus improved by 23–57 MPa and
of natural fibers can overcome the limitations. from 1.16 to 3.04 GPa, respectively, for 10% of NaOH for 24-h
processed alfa fiber composite compared to the untreated fiber
Natural fibers provide numerous benefits such as low cost, light composite.2 Woven bamboo mat was treated with maleic anhy-
weight, high specific modulus, and no health hazards of compo- dride, benzoyl chloride, benzyl chloride, and flexural properties
sites reinforced with synthetic fibers such as glass, carbon, and of maleic anhydride-treated bamboo polyester composites were
aramid fibers. These advantages of natural fiber composites improved by nearly 50%. The tensile strength and modulus of
place the natural fiber composites among the high-performance benzoylated bamboo fiber polyester composite improved by 71
composites having economical and environmental advantages.2 and 118%, respectively.4
A hurdle in the use of natural fibers as reinforcement in compo- The variety of natural fibers and their availability depends on
sites is that it has insufficient interface quality with the polymer the richness of flora and fauna of the place. India is a country

C 2014 Wiley Periodicals, Inc.

V

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with rich and abundant flora and fauna. There are various natu- were further dried in sun light for 7 days. The bundle of culms is
ral resources available which show potential use as reinforce- shown in Figure 1(b). This bundle was then beaten with a wooden
ment in composites. Grass is in plethora all over the country. hammer to convert culms into fibers. Thus, S. munja fibers (SMF)
There are various types of grasses available which have very were extracted from the grass. The bundle of fibers obtained from
good potential to use as reinforcement in composites. S. munja grass is shown in Figure 1(c).
Munja is one such grass which shows a very good potential to Treatment of Fibers
be used as reinforcement. It is commonly known as Kana or SMFs extracted from the grass were cut to a length of 200 mm
sarkanda or Munja. The botanical name of this grass is Saccha- and treated with 5% of sodium hydroxide for 2, 4, 6, and 8 h
rum m unja. It is distributed over North India and North West in water bath using material to a liquor ratio of 1 : 30 on
India and it is also found in Pakistan and Afghanistan. This weight basis at room temperature. Then they were washed
grass is found in arid areas and along river banks in India. The multiple times to remove soluble impurities and remaining
grass is tall, panicles silky, and greenish brown. The grass grows sodium hydroxide. After washing, treated fibers were neutralized
in excess and up to 7 feet in height. It is planted in field divid- with acetic acid and dried at room temperature for 48 h. After
ing area because it forms extensive root network that binds the drying, combing was carried out for unidirectional alignment of
soil/pebbles and prevents soil erosion from fields. This grass fibers. The difference in weight of the fibers before and after
cannot be used for cattle feed because the leaf blades can wound NaOH treatment was 22.8% for 8-h alkali-treated samples.
the cattle. It is used to make fire during winters or also used to Before fabrication of composite, fibers were dried in an oven at
make ropes, brooms, and huts. Overall, the grass does not have 105 C for 2 h. The complete removal of moisture from
any notable scale commercial application.5 fibers was confirmed by constant weight of the fibers. These
fibers were directly used for the fabrication of composites.
In this research, the fiber obtained from S. munja grass was
Tensile and thermal properties of the fibers were studied and
used as reinforcement. This grass has neither been used previ-
reported.
ously as textile fiber nor as reinforcement in the composite. In
our research study, a thriving attempt has been made to sepa- Composite Fabrication
rate fibrous material (S. munja fiber) from S. munja grass and A stainless steel mold of size 200 mm 3 150 mm 3 3 mm was
use of S. munja fiber as a reinforcing material in composites. prepared and the dried fibers were laid aligned unidirectional. In
Because of the newness/originality of the obtained fibers, the all, 10% of weight fraction of fibers was used to make composite
properties of fiber are studied prior to its application in com- sheet. In brief, 3% of cobalt accelerator and 1% of methyl ethyl
posite. It was found that S. munja has very good reinforcing ketone peroxide hardener were mixed with sufficient quantity of
properties. The composites formed seem to have potential to unsaturated polyester resin (UPR). This mixture was then poured
supplement common fiber-reinforced composites. into the mold. Plastic squeeze was used for uniform application.
A silicon roller was rolled to remove entrapped air from the
EXPERIMENTAL fibers. The mold was left for 24 h at room temperature for cur-
ing of composite. After 24 h, the unidirectional fiber-reinforced
Extraction of Fibers from S. munja Grass
composite sheet was separated from mold. Specimens for tensile,
As shown in Figure 1(a), S. munja grass is grown on the border of
flexural, and impact strength testing were cut on vertical cutting
fields to avoid soil erosion. This grass was obtained from a village
machine according to the required dimensions. In total, five
in East Rajasthan, India. The grasses were cut from bottom and
types of composites were made and characterized. For each type
left open in sun light for 15 days to dry at a climatic temperature
of composite, three batches of fiber samples were used.
of 35 C. The stem of the grass (known as sarkanda) was separated
from the leaves manually. The culms (outer covering of the stem) Fourier Transform Infrared Spectroscopy
were separated manually from the dried stems. The dried stem Fiber samples were grinded and converted into powder form.
can be used for making decorative items or furniture. Then culms This powder was mixed with KBr in the ratio of 1 : 9 without

Figure 1. Extraction of fibers from S. munja grass. (a) S. munja plant. (b) Bundle of culms of S. munja. (c) Fibers of S. munja.

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drying and pellets were prepared. The Fourier transform infra-

red spectroscopy (FTIR) spectra of the untreated and the alkali-
treated samples were recorded in the region of 3750–700cm21on
a Shimadzu 8400S FT-IR instrument with 32 scans in each case
at a resolution of 4 cm21.
Mechanical Testing
Tensile, flexural, and izod impact tests were carried out accord-
ing to the ASTM Standard. For each test and type of composite,
five specimens were tested and the average values are reported.
Tensile tests were conducted according to ASTM D 638 using a
Universal Testing Machine (Lloyd LR) at a crosshead speed of 5
mm/min. Flexural tests were carried out according to ASTM D
790 using the same testing machine mentioned above at a cross-
head speed of 2 mm/min. Izod impact tests of notched samples
were conducted according to ASTM D 256 using a Tinius Olsen
Impact Tester (model 104) which has metallic hammer. Tensile Figure 3. FTIR spectra of untreated and treated SMFs.
strength of fibers was measured according ISO 5079 method on
Tinius Universal Testing Machine at a crosshead speed of alkali-treated fibers can be seen in this figure. As it is observed,
30 mm/min. after alkali treatment tensile strength of the fiber was increased
up to 16% after 8-h alkali treatment in comparison with
Scanning Electron Microscopy
untreated fiber. After NaOH treatment, impurities and some
The interfacial bonding between SMFs and UPR matrix in man-
part of hemicelluloses and lignin were removed, which increase
ufactured composites was examined using a scanning electron
the strength of fiber.
microscope (SEM) (model JEM 5400). Fibers samples were
mounted on the metallic stub and coated with gold ions for 6 Fourier Transform Infrared Spectroscopy. The spectra of
min and thickness of gold coating was approximately 10 Å. The untreated SMFs and alkali-treated SMFs are shown in Figure 3.
accelerating power in the SEM was kept in the range of 3 kV. The untreated SMF shows a peak at 1740 cm21 assigned to
Thermogravimetric Analysis C@O, which disappeared when the fibers were treated with the
Thermogravimetric analysis (TGA) of fiber samples and com- NaOH aqueous solution. The observation shows the removal of
posite sample was done with Shimadzu 8400S and the degrada- hemicelluloses by alkali treatment. The vibrational peak around
tion of the sample with respect to temperature was studied. The 2900 cm21, belonging to the CAH stretching vibration in cellu-
experiment was done by using 8 g of samples from 30 to 500 C lose and hemicelluloses, decreased after NaOH treatment. It
with a heating rate of 20 C/min for fiber sample and 10 C/min indicates that part of the hemicelluloses was removed.6 Further-
for composite sample. The nitrogen gas was used as purge gas. more, the peak around 1633 cm21 for CAO assigned to the
ester and ether crosslink between cellulose and lignin, or cellu-
RESULTS AND DISCUSSION lose and hemicelluloses, disappeared during NaOH treatment.
This is owing to the removal of acid, lignin, and other fiber
Characterization of SMF
constituents.7 Though these groups attached through lignin
SMFs are characterized for tensile and thermal properties. The
contents are removed, their presence in the cellulose structure
surface characteristic of the fibers is also reported to study the
of fiber shows some intensity around that region.
effect of alkali treatment on the fiber surface.

Tensile Properties. The tensile properties of SMFs obtained are Scanning Electron Microscopy. Figure 4(a) shows the SEM
shown in Figure 2. A comparison of untreated SMFs with micrograph of untreated SMFs. The impurities were clearly
observed on the surface of untreated fiber. The modification of
fiber by sodium hydroxide (NaOH) effectively removed the
impurities from the fiber surface. Figure 4(b–d) shows the SEM
micrograph of the surfaces of alkali-treated SMFs for different
time periods. It was found that the treated fiber surfaces are
cleaner than untreated fibers.8 Figure 4(e) shows the SEM
micrograph of 8-h-treated SMFs that presented the cleanest
fiber surface. It was observed that almost all impurities have
been removed from the fiber surface. The increase of soaking
time in NaOH showed more clean and rough surface of the
fiber.

Thermogravimetric Analysis. The fiber degradation process

was divided into four stages: moisture evaporation, hemicellulo-
Figure 2. Effect of NaOH treatment on tensile strength (kgf) of fibers. ses degradation, cellulose degradation, and lignin decomposition.

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Figure 4. SEM image of SMFs. (a) Untreated SMFs. (b) Two-hour alkali-treated SMFs. (c) Four-hour treated SMFs. (d). Six-hour alkali-treated SMFs.
(e) Eight-hour alkali-treated SMFs.

Moisture is present in the fiber in two forms: free water and The crystalline structure contains strong intramolecular and
linked water. Free water is generally attached on the fiber surface intermolecular hydrogen bonds which requires higher energies to
and evaporates at lower temperature (25–150 C). However, the be broken down.10 The decomposition of hemicelluloses is at
linked water forms chemical bonds with the hydroxyl groups about 200 C.The thermal decomposition of lignin took place
present in hemicelluloses and lignin, and evaporates at higher over a broader temperature range (150–450 C) than the cellulose
temperatures.9 After the removal of free water, in the temperature and hemicelluloses. During heating, lignin formed aromatic
range of 150–500 C, the degradation process begins in the cellu- hydrocarbons, hydroxyl, and phenolic compounds. All these com-
lose, hemicellulose, and lignin constituents. The different degra- ponents contained AOH groups which became unstable at higher
dation stages during the thermal degradation of fiber are shown temperatures. These unstable groups underwent further reactions
in Figure 5(a,b). It can be observed that the cellulose decomposi-
among themselves which resulted in structural rearrangements
tion process (weight loss) was very mild until around 250 C.
owing to radical–radical interactions.11 It was found that thermal
Then, a sharp and large weight loss occurred at about 350 C. In
the temperature range of 250–350 C, the cellulose was entirely degradation temperature (weight loss, 50%) of untreated SMFs
decomposed owing to the breaking down of its molecular struc- was 310.25 C and for alkali-treated (5% NaOH for 8 h) SMFs it
ture. This was owing to the fact that most of the cellulose struc- was increased to 340.28 C. Alkali-treated fibers showed higher
ture was crystalline, which is strong and resistant to hydrolysis. decomposition temperature compared to the untreated fibers.

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Figure 6. Effect on NaOH treatment on tensile strength of SMF/UPR

composites.

that alkali treatment time of 6 h gives good and optimum

results.
The improvement in tensile strength of SMF composites was
owing to the removal of impurities because of alkali treatment.
Alkali treatment leads to fibrillation which causes the breaking
down of the fiber bundle into smaller fibers which results in
decrease in fiber diameter and thereby increases the aspect ratio.
Therefore, the development of a rough surface topography and
enhancement in aspect ratio offers better fiber–matrix interface
adhesion and an increase in mechanical properties.12
Results of tensile modulus are shown in Figure 7. Modulus of
untreated SMF composites was found to be 2663 MPa. After
the treatment time of 8 h, tensile modulus of SMFs was 3836.2
MPa which shows improvement in modulus of alkali-treated
SMF composite. The increase in tensile modulus is 44%. The
Figure 5. (a) TGA of SMFs. (b) Differential TGA of SMFs.
increase in tensile modulus shows that the stiffness of the com-
posite is increasing with the use of fibers as reinforcement. UPR
For the main fiber decomposition region (250–350 C), the alkali- with SMFs as reinforcement is becoming stiffer and could with-
treated fibers had less weight loss than the untreated fibers. These stand higher stress at the same strain portion. The treatment
results indicate that alkali treatments removed portions of hemi- with alkali shows further increase in tensile modulus. Low stiff-
celluloses and lignin constituents from the fiber. Owing to this ness means that fibers are unable to absorb the tensile forces
fact, the decomposition process mainly occurred on the cellulose owing to the inefficiency of bonding between fiber and
which in turn increased the overall degradation temperature of matrix.13 Thus, the results show better interfacial bonding
the treated fibers. between UPR matrix and SMFs after alkali treatment of fibers.
This means that the fiber served well as reinforcement and
shared the major load for matrix.
Characterization of Composites
Tensile Properties. As shown in Figure 6, the tensile strength of
the composite is greater than the standard (neat resin), which
means that there is definitely an improvement in the tensile
strength with the inclusion of fiber material. Furthermore, with
increase in the treatment time of NaOH from 2 to 8 h, the ten-
sile strength value also increased. The tensile strength of
untreated SMF composite is 59.13 MPa and treated SMF com-
posite (for 8 h) is 80.69 MPa. Tensile strength of alkali-treated
SMF composites increased by about 36.46% as compared to
untreated SMF composites. Tensile strength of 6-h alkali-treated
fibers and 8-h-treated fibers is almost similar. This could be
because of no further improvement of fiber properties after 6-h
treatment; if treatment time is increased for more than 8 h,
then there are chances of deterioration in fiber strength and Figure 7. Effect on NaOH treatment on tensile modulus of SMF/UPR
other fiber properties. Hence, from the results it can be said composites.

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Figure 8. Effect of NaOH treatment on flexural strength of SMF/UPR Figure 10. Effect of NaOH treatment on izod impact strength of SMF/
composites. UPR composites.

Flexural Properties. The flexural strength of untreated SMF

improvement of about 29%. Impact strength of neat UPR is 151
composite was 65.34 N/mm2 and after alkali treatment of the
J/m2 which is very less than the fiber composites. Fibers play a
fibers for 8 h, flexural strength of composite was 114.93 N/mm2
vital role in impact strength of the composites as they act as
as shown in Figure 8 which is 76% improvement in flexural
stress-transferring medium and resist crack formation.15 SEM
strength. The observations made earlier for the tensile strength
images of SMFs before alkali treatment show that the surface of
on the effect of fiber–matrix adhesion are also seen clearly here.
fiber is covered with a layer of substance, which may include pec-
The fiber surface treatments also have effect on the flexural
tin, lignin, and other impurities. After alkali treatment, impor-
strength. The increment of interfacial area of contact was bene-
tant modification done is the disruption of hydrogen bonding in
ficial for the flexural strength. This indicates that the increase in
network structure, thereby increasing surface roughness. The
area of contact between the fiber and the matrix improves the
removal of lignin made more cellulosic sites available for contact
level of adhesion.14
with the resin which led to better mechanical interlocking.16
Figure 9 shows the flexural modulus of SMFs/UPR composites for Higher impact strength of alkali-treated SMF specimen was
untreated and the alkali-treated fibers. It is seen that the improve- owing to good interface bonding between fiber and matrix.
ment of the flexural modulus emerges when the time of treatment
increases. The modulus of untreated SMF composite is 4106 MPa Thermogravimetric Analysis. As shown in Figure 11, the UPR
and alkali-treated SMF composites is 6452 MPa, and hence matrix is thermally stable up to 394 C. The composites started
improvement in modulus is about 57%. The flexural modulus is degrading at lower temperatures than UPR. This is the result of
the stiffness parameter. After the alkali treatment, SMFs provide the presence of SMFs which degrades at lower temperatures. The
improved crystallinity of cellulose and remove part of the hemicel- degradation of the polymer backbone in the 8-h alkali-treated
lulose and lignin content beyond the removal of impurities. This composites sample occurs at a higher temperature than the other
suggests that fiber becomes relatively ductile after the removal of alkali-treated samples. The alkali treatment brings about an
some hemicellulose and lignin. This can result in higher fiber stiff- increased surface roughness in the fiber which results in better
ness owing to the increased crystallinity of hard cellulose. mechanical interlocking between the filler and the matrix. As a
result, the fiber may retard the movement of free radicals formed
Izod Impact Strength. Figure 10 shows that impact strength of during the initiation of degradation, or it may interact with
untreated SMF composite was found to be 236.1 J/m2, whereas
for 8-h alkali-treated SMF composites, it is 305.4 J/m2, showing

Figure 9. Effect of NaOH treatment on flexural modulus of SMF/UPR

composites. Figure 11. TGA of SMF/UPR composites.

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Figure 12. SEM image of SMF composites. (a) Untreated SMF composite. (b) Two-hour alkali-treated SMF composite. (c) Four-hour treated SMF com-
posite. (d) Six-hour alkali-treated SMF composite. (e) Eight-hour alkali-treated SMF composite.

volatile degradation products and in the process slow down their fiber and matrix. Improved interfacial bonding between the
diffusion out of the sample. Thus, the alkali treatment increases fiber and the matrix can be attributed to the removal of lig-
the thermal resistance of the fiber composite. nin, hemicelluloses, and other structural effects, which causes
rough surface morphology of fibers. This finding corresponds
Scanning Electron Microscopy. The results of scanning elec- with the results in improvement in mechanical properties.
tron microscopy of impact fractured surface of SMF compo- Thus, alkali treatment results in significant change in mor-
sites illustrates the improvement of the interaction between phology of the fiber surface and is effective for increasing the
the fiber and the matrix. SEM images/micrographs of the available contact between the fibers and the UPR matrix. The
treated fiber composites show that the fibers are closely enhancement of impact strength of the treated fiber composite
adhered to the matrix. Comparing Figure 12(a–e), it is as compared to untreated fiber composite can also be attrib-
observed that the number of pores in untreated fiber compos- uted to the flexibility of the interface molecular chains,
ite is higher than that in composite made using alkali-treated resulting in comparatively greater energy absorption.
fibers. Also, the pore size is higher. Thus, the presence of
CONCLUSIONS
pores is indicative of weak interaction between untreated fiber
and UPR resin. Although SEM images of treated fibers indi- Use of natural fibers as reinforcement in composite is a very
cate that the distance between fiber and matrix has reduced to important and significant approach in composite industry and
large extent, resulting in improved interfacial bonding between SMF has potential to be one such fiber. Tensile properties, flexural,

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and impact strength of the fibers show comparable values with the 6. Liu, W.; Mohanty, A. K.; Askeland, P.; Drzal, L. T.; Misra,
reinforcing fibers used today. There are various ways of chemical M. Polymer 2004, 45, 7589.
modification of fibers to improve the performance of fibers in 7. Maheswari, C. U.; Guduri, B. R.; Rajulu, A. V. J. Appl.
composite and the modification of SMFs by alkali treatment has Polym. Sci. 2008, 110, 1986.
shown improved fiber performance in composites. Commerciali-
zation of the fibers and their use in composite can give comple- 8. Yuhazri, M. Y.; Phongsakorn, P. T.; Haeryip Sihombing, I.
P.; Jeefferie, A. R.; Puvanasvaran A. P.; Kamarul, A. M.;
mentary income in agriculture at minimal investment costs.
Rassiah, K. Int. J. Eng. Technol. 2011, 11, 106.
ACKNOWLEDGMENTS 9. Randriamanantena, T.; Razafindramisa, F. L.; Ramanantsizehena, G.;
The authors thank the UCG–SAP for providing funding for the Bernes, A.; High-energy Physics International Conference, Antana-
project. The work of colleagues and students Kundan Dekate, San- narivo, Madagascar, 2009, p 1.
tosh Biranje, and Abhinav Nathany is much appreciated. 10. Thakur, V. K.; Singha, A. S. Iran. Polym. J. 2010, 19, 3.
11. Saha, A. K.; Das, S.; Bhatta, D.; Mitra, B. C. J. Appl. Polym.
Sci. 1999, 71, 1505.
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