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Composites: Part B 42 (2011) 16481656

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Composites: Part B
journal homepage: www.elsevier.com/locate/compositesb

Effect of alkali treatment on interfacial and mechanical properties of coir ber


reinforced poly(butylene succinate) biodegradable composites
Tran Huu Nam a,, Shinji Ogihara a, Nguyen Huy Tung b, Satoshi Kobayashi c
a

Department of Mechanical Engineering, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba 278-8510, Japan
Polymer Center, Hanoi University of Technology, No. 1, Dai Co Viet, Hanoi, Viet Nam
c
Department of Mechanical Engineering, Tokyo Metropolitan University, 1-1 Minami-Osawa, Hachioji, Tokyo 192-0397, Japan
b

a r t i c l e

i n f o

Article history:
Received 6 January 2011
Received in revised form 3 March 2011
Accepted 7 April 2011
Available online 12 April 2011
Keywords:
A. Polymermatrix composites (PMCs)
B. Interface/interphase
B. Mechanical properties
E. Surface treatments

a b s t r a c t
The poly(butylene succinate) (PBS) biodegradable composites reinforced with coir bers were developed.
The effect of alkali treatment on the surface morphology and mechanical properties of coir bers, interfacial shear strength (IFSS) and mechanical properties of coir ber/PBS composites was studied. The effect
of ber mass content varying from 10% to 30% on the mechanical properties of coir ber/PBS composites
was also investigated. The coir bers which are soaked in 5% sodium hydroxide solution at room temperature (RT) for 72 h showed the highest IFSS with 55.6% higher than untreated coir bers. The mechanical
properties of alkali-treated coir ber/PBS composites are signicantly higher than those of untreated
bers. The best mechanical properties of alkali-treated coir ber/PBS composite were achieved at ber
mass content of 25% in this study, which showed an increase of tensile strength by 54.5%, tensile modulus
by 141.9%, exural strength by 45.7% and exural modulus by 97.4% compared to those of pure PBS resin.
The ber surface morphologies and fractured surface of the composites exhibited an improvement of
interfacial bermatrix adhesion in the composites reinforced with alkali-treated coir bers.
2011 Elsevier Ltd. All rights reserved.

1. Introduction
In the past decade, natural ber composites based on petroleumbased thermoplastics or thermosets matrices have been used in
various industrial sectors, especially in automobile industry such
as door panels, seat backs, headliners, package trays, dashboards,
and interior parts [1,2]. However, these natural ber composites
are not fully environmentally friendly because matrix resins are
non-biodegradable [3]. Therefore, biodegradable composites based
on natural bers and biodegradable polymeric matrix made from
cellulose, starch, and other natural resources are called green composites and have been developed because of their environmentally
benecial properties [48]. In general, the research and development of natural ber biodegradable composites from renewable resources for a wide range of applications is increasing due to their
advantages, such as eco-friendliness, lightweight, carbon dioxide
reduction and biodegradable characteristics.
The commercial natural bers such as henequen, hemp, jute,
kenaf, sisal, ax, bamboo, coir, banana, palm, silk, cotton and wood
are renewable resources in many developing countries. These
bers offer specic benets such as low cost, low density, low
pollutant emissions, acceptable specic properties, renewable

Corresponding author. Tel.: +81 (0)4 7124 1501x3917; fax: +81 (0)4 7123 9814.
E-mail addresses: trannam@rs.noa.tus.ac.jp, thnam.hut@gmail.com (T.H. Nam).
1359-8368/$ - see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesb.2011.04.001

characteristics, enhanced energy recovery, and complete biodegradability [912]. They are considered as strong candidates to replace the conventional glass bers due to eco-friendliness, low
cost, renewable resources and biodegradability. Among the natural
bers, plant bers which contain strongly polarized hydroxyl
groups are hydrophilic in nature [13]. These bers are inherently
incompatible with hydrophobic thermoplastics. Furthermore, due
to the presence of pendant hydroxyl and polar groups in various
constituents of bers, moisture absorption of bers is very high
and leads to poor interfacial bonding with the hydrophobic matrix
polymers. Therefore, it is necessary to decrease the moisture
absorption and hydrophilic character of bers by suitable surface
chemical modication [1417].
Among the plant bers, coir bers are nowadays extensively
used in many industrial applications. Coir is a versatile lignocellulosic ber extracted from the tissues surrounding the seed of coconut palm (Cocos nucifera). Coir consists of cellulosic bers with
hemicellulose and lignin as the bonding materials for the bers.
Table 1 summarizes several physical, chemical and mechanical
properties of coir ber compared with other typical natural bers
such as ax, hemp, jute, ramie and sisal [2,11,18]. Coir ber has
low cellulose and hemicellulose, high lignin content and high
microbrillar angle compared with other natural bers (Table 1).
As a result tensile strength and Youngs modulus of coir ber are
lower than those of other plant bers. Coir ber has low moduli
due to high microbrillar angle [19]. Besides, elongation at break

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T.H. Nam et al. / Composites: Part B 42 (2011) 16481656


Table 1
Physical, chemical and mechanical properties of coir ber compared with other natural bers [2,11,18].
Properties/bers

Coir

Flax

Hemp

Jute

Ramie

Sisal

Density (g/m )
Diameter (lm)
Cellulose content (%)

1.251.5
100450
3643

1.4
100
6272

1.48
25
6775

1.45
60
5971

1.5
4050
6876

Hemicellulose content (%)


Lignin content (%)

0.2
4145

1618
22.5

1618
2.83.3

1213
11.812.9

1314
0.60.7

Microbrillar angle ()
Tensile strength (MPa)

3045
105175(I)
95118(B)
46(I)
1747(I)
23.951.4(B)
10

10
8001500

6.2
550900

79
400800

7.512
500870

1.261.33
100300
7475.2(B)
6067(I)
1013.9
812(I)
7.67.98(B)
1020
600700

6080
1.22.4

70
1.6

1030
1.161.8

44
1.2

12

1217

Youngs modulus (GPa)


Elongation at break (%)
Moisture absorption (%)

38
3.645.12(I)
22.5(B)
11

(B) Brazilian; (I) Indian.

of natural bers increases with increasing microbrillar angle, thus


the elongation at break of coir is the highest among typical natural
bers [20]. This property of coir ber is certainly useful in cushion
applications. An example of the application to seat cushion for
automobiles is reported in [21]. The high lignin content in coir ber
is responsible for other useful properties such as weather, fungal,
and bacterial resistance [20]. The lignin content in coir ber is
quite high, so the ber becomes stiffer and tougher.
Due to hardwearing quality, durability and other advantages,
coir is used for marking a wide variety of oor-furnishing materials, yarn, rope, etc. However, these traditional coir products consume only a small percentage of the potential total world
production of coconut husk. According to ofcial website of International Year for Natural Fibres 2009, about 500,000 tonnes of coir
are produced annually, mainly in India and Sri Lanka followed by
Thailand, Vietnam, the Philippines and Indonesia. Its total value
is estimated at $100 million. Hence, the research and development
efforts have been underway to nd new utilization of coir as a reinforcement in polymer composites, such as coir-polypropylene and
coir based polyester green composites [1517,2125].
A fully biodegradable composite reinforced by natural bers is
usually made from completely biodegradable polymeric matrix.
Among the completely biodegradable polymers which have been
frequently studied as biodegradable polymer matrices in the biocomposites, polylactic acid (PLA) and poly(butylene succinate)
(PBS) are increasing commercial interest [26]. However, PBS is
commercially available at lower cost than PLA. PBS can be naturally
degraded into the environment by bacteria and fungi [27,28]. Furthermore, PBS has excellent biodegradability in nature, such as in
soil, lake, sea, and compost [29]. It can be completely combustible
by re without evolving toxic gases as described in [30]. It has
comparable mechanical properties with several thermoplastics
such as polyethylene, polypropylene and polystyrene. Therefore,
PBS can be a good candidate material for the matrix of biodegradable composites.
The combination of coir bers and PBS resin can produce the
environment-friendly biodegradable composite. In the present
work, tensile properties of untreated and alkali-treated coir bers
were reported. The effect of alkali treatment on the interfacial
shear strength (IFSS) of coir ber/PBS system was evaluated by single ber pull-out test. The PBS biodegradable composites reinforced with untreated and alkali-treated coir bers were
fabricated by compression molding method. The effect of alkali
treatment and ber content on mechanical properties of coir ber/PBS biodegradable composites was studied. Coir ber surface
morphology and fractured surfaces of untreated and alkali-treated
coir ber/PBS composites were investigated by scanning electron

microscope (SEM) providing the information for the evaluation of


interfacial bermatrix adhesion.
2. Experimental
2.1. Materials
Poly(butylene succinate) pellets (PBS, #1001, Showa High Polymers, Ltd., Tokyo, Japan) is thermoplastic, aliphatic polyester and
also biodegradable polymer. The melting temperature of the PBS
is about 115 C, the density is 1.26 g/cm3. Fig. 1 depicts the chemical structure of PBS used in this study. The golden brown coir bers in the present work were supplied from Betrimex, JSC.,
Bentre, Vietnam. It was found that the cross section of coir ber
is not completely circular (Fig. 2), thus ber cross sectional area
(A) is determined approximately by a formula as follows:

pab

where a and b are dimensions in Fig. 2 measured by an optical


microscope MX-7575CS (Hirox Co., Ltd., Tokyo, Japan).
The diameter (d) of coir ber is calculated approximately as
follows:

p
ab

The coir bers with the length exceeded 100 mm and the diameter varying from 100 to 450 lm were selected carefully to be used
in this study.
2.2. Alkali treatment of coir bers
First of all coir bers were treated with 5% NaOH solution in a
glass beaker for different soaking time (24 h, 48 h, 72 h and 96 h)
at room temperature (RT). Next the bers were taken out of the
solution, then washed several times with fresh water and subsequently with distilled water. Finally, the coir bers were air-dried
for more than 2 days. The mean IFSS of 5% alkali-treated coir bers
for 72 h which will be shown in next section is higher than that of
untreated and other alkali-treated coir bers. Therefore, another
series of experiments with the same procedure were followed ex-

Fig. 1. Chemical structure of PBS used in the present study.

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T.H. Nam et al. / Composites: Part B 42 (2011) 16481656

Fig. 2. Typical cross section of coir ber.

cept that the coir bers were soaked in various concentrations of


NaOH solution (3% and 7%) for 72 h in order to select the best alkali
concentration for the treatment. The series are designated by 3NX,
5NX and 7NX in which 3N, 5N and 7N corresponding to the soaking
in 3%, 5% and 7% NaOH solution, respectively and X corresponding
to the soaking time in hours. The reaction of sodium hydroxide
with coir ber is described as follows:


CoirOH NaOH ! CoirO Na H2 O

2.3. Coir ber characterization


The single ber tensile tests were carried out by a universal
testing machine Instron 4442 (Instron Corp., Canton, MA) with a
crosshead speed of 5 mm/min at RT. Individual untreated and alkali-treated coir bers were carefully chosen, mounted and glued on
a paper tab before testing. Gauge length of single ber tensile specimens is 10 mm. The average tensile properties of untreated and
alkali-treated coir bers were measured at least from thirty successful specimens.
2.4. Interfacial characterization
A single ber pull-out test was used to measure the IFSS of untreated and alkali-treated coir ber/PBS system. The untreated and

Fig. 3. Schematic representation of single ber pull-out test.

alkali-treated coir bers having length over 120 mm were used for
preparing pull-out test specimens by pressing the bers between
two PBS sheets using a hot press equipment (Imoto Corp., Kyoto,
Japan). The bers were kept straight and oriented by xing its both
ends, extending outside the PBS sheets, on the mold using glue as
described in [25]. Specimens with a thickness of 1 mm were removed from the mold after quickly cooling in ice water. The ber
embedded length in the PBS matrix was obtained by cutting the ber by punching a hole through the specimen. The schematic representation of single ber pull-out test is shown in Fig. 3, in which
d is mean diameter of coir ber and L is embedded length. Mean
diameter of coir ber was calculated using the formula (2) in which
the dimensions of a and b were measured at the intersection between coir ber and PBS matrix. Single ber pull-out test was performed by above universal testing machine Instron 4442 with a
load cell of 50N and a crosshead speed of 1 mm/min. A force is applied to the free end of ber to pull it out of the matrix while the
force is continuously monitored and recorded. IFSS value of untreated and alkali-treated coir ber/PBS system was estimated
from the maximum debonding force (Fd) using following equation:

Fd

pdL

The single ber pull-out test was carried out for untreated,
5N24, 5N48, 5N72, 5N96, 3N72 and 7N72 treated coir bers to
investigate the effect of soaking time and concentration of sodium
hydroxide on the IFSS of coir ber/PBS system in order to make a
right choice of alkali treatment. The mean IFSSs between coir bers
and PBS matrix were obtained from twenty successful pull-out test
specimens.
2.5. Composite fabrication
To begin with coir bers were dried at 80 C in the vacuum oven
for 24 h. Next the dried coir bers were slightly stretched out
straight within the elastic region. Then they were cut into the segments with the length of 100 mm. After that coir bers were
weighed and aligned in a parallel array, glued by adhesive tape
and placed in the mold between the PBS sheets. The composite
plates made from PBS and different untreated and alkali-treated
coir ber mass content (10%, 15%, 20%, 25% and 30%) were fabricated using above hot press equipment. The pure PBS and composite plates were pressed in a stainless steel mold with a thickness of
1 mm under 10 MPa pressure for 10 min at 150 C. Next the mold
was removed from the press, then clamped securely between two
steel mold plates and last quickly quenched by ice water. There
seems to be no water uptake and no moisture absorption during

Fig. 4. Schematic representation of the hot press used to fabricate composite plates.

T.H. Nam et al. / Composites: Part B 42 (2011) 16481656

quenching of the sample. The schematic representation of the hot


press for composite fabrication is shown in Fig. 4. Both PBS sheets
and composite plates were prepared with the same thermal
history.
2.6. Tensile test
The tensile specimens of 100  10  1 mm3 were cut out from
pure PBS and composite plate by cutting machine AC-300CF (MARUTO Testing Machine Co., Tokyo, Japan) and kept in desiccator at
25 C and 35% relative humidity before testing. The both clamped
ends of the specimens (Fig. 5) were glued by two glass ber reinforced plastic (GFRP) tabs. Strain gauges were glued at the center
of the specimens to measure the elongation at break. Tensile properties were measured according to JIS K7113 using a universal testing machine Senstar SC-5H (JT Tohsi Inc., Tokyo, Japan). All the
tensile tests were carried out at RT with a crosshead speed of
0.5 mm/min. Tensile specimens were chosen carefully before testing. The mean tensile properties of pure PBS and coir ber/PBS
composites were obtained from ve successful specimens for each
ber content.
2.7. Flexural test
The exural properties of pure PBS and coir ber/PBS biodegradable composites were measured by a three-point bending
method according to JIS K7171 standard using universal testing
machine Autograph AGS-1000A (Shimadzu, Kyoto, Japan). The exural test was carried out at RT with a crosshead speed of 2 mm/
min. The dimension of exural specimens was 50  25  1 mm3.
The ratio between span distance and thickness of pure PBS and
composite specimens was 16. The exural strength (rf) and modulus (Ef) were calculated using the following equations:

rf
Ef

3FLs

2bh

1651

where F is the maximal applied force, Ls is the length of support


span, m is the slope of the forcedeection curve, b and h are the
width and thickness of the specimen, respectively. Flexural specimens were chosen carefully before testing. The mean exural properties of each composite were obtained from ve successful test
specimens.
2.8. Morphological characterization
The coir surface morphologies and fractured surface of the composites after tensile tests were examined using SEM (VE-7800, Keyence Inc., Osaka, Japan).
3. Results and discussion
3.1. Effect of alkali treatment on mechanical properties of coir ber
Tensile properties of untreated and alkali-treated coir ber
were presented in Table 2. The mean tensile strength of coir ber
is quite low compared to other natural ber such as jute, ax,
hemp, ramie or sisal ber. However the strain at failure of coir ber
is quite high compared with other natural and synthetic bers such
as glass and carbon. As shown in Table 2, alkali treatment of coir
bers improved signicantly their tensile properties. It is seen that
at 5% alkali solution when soaking time increases from 24 h to 72 h
the tensile properties of alkali-treated coir bers increased, but
they decreased beyond 72 h. In addition with the soaking time of
72 h tensile properties of coir ber increased with increasing concentration of alkali solution up to 5%, but over 5% they decreased.
The tensile strength and modulus of coir bers increased by about
71% and 113% when the bers were soaked in 5% sodium hydroxide solution for 72 h, respectively. The increase in tensile strength
and modulus of coir ber after alkali treatment was explained in
detail [15].
3.2. Effect of alkali treatment on coir ber surface

L3s m

4bh

Fig. 5. Shape and dimensions of tensile specimen.

Table 2
The mean tensile properties of untreated and alkali-treated coir ber.
Coir ber

Strength (MPa)

Modulus (GPa)

Failure strain (%)

Untreated
5N24 treated
5N48 treated
5N72 treated
5N96 treated
3N72 treated
7N72 treated

139.67 39.42
218.52 38.38
227.43 40.86
238.26 39.91
210.07 35.09
209.21 + 37.69
228.54 37.15

2.79 0.54
5.64 0.73
5.68 0.81
5.95 0.79
5.27 0.76
4.92 0.84
5.47 0.82

29.52 6.89
31.40 3.60
32.70 5.10
33.96 5.74
30.00 4.85
29.59 4.13
30.53 3.44

Alkali treatment improves the bermatrix adhesion due to the


removal of natural and articial impurities from the ber surface
as well as changing in the arrangement of units in the cellulose
macromolecule [31]. Alkali treatment increases the surface roughness and the amount of cellulose exposed on the ber surface
resulting in better mechanical interlocking [16]. Therefore, the
development of a rough surface tomography and enhancement in
aspect ratio offer better bermatrix interfacial bond resulting in
increasing mechanical properties.
Fig. 6 showed the effect of different alkali treatment on the coir
ber surface. SEM micrograph of untreated coir ber shows globular particles and cuticles on the ber surface (Fig. 6a). The globular
particles which cover the pits on the cell walls are embedded in the
ber surface [15]. Some of globular particles were intact but at a
few isolated places they were removed creating the pits on 5N48
treated coir ber surface (Fig. 6b). When the soaking time increased to 72 h the cell was exposed and a much greater proportion of globular particles appeared to be removed (Fig. 6c), thus
the roughness of ber surface increased. The removal of cuticle
layer will expose lignin on the ber surface. Lignin, being a phenolic natural polymer, should be chemically compatible with PBS resin. However, the micrograph in Fig. 6d shows that 5N96 treated
coir ber surface is smoother than that of 5N72 ber surface.
Smooth surface of 5N96 treated coir ber can be explained due
to the removal of all globular particles and cuticles deposited on
the ber surface. For alkali concentration of 3% (Fig. 6e), nearly
all globular particles on the ber surface were intact, but the surface impurities were removed. With alkali concentration of 7%,

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T.H. Nam et al. / Composites: Part B 42 (2011) 16481656

Fig. 6. SEM micrographs of coir bers: (a) untreated ber, (b) 5N48 treated ber, (c) 5N72 treated ber, (d) 5N96 treated ber, (e) 3N72 treated ber, and (f) 7N72 treated
ber.

The typical forcedisplacement curves obtained from single ber pull-out test for the untreated and alkali-treated coir ber reinforced PBS composites were shown in Fig. 7. It can be noted that all
the curves exhibit nonlinear behavior due to the characteristics of
the ductile matrix. However, once the force reaches its maximum
value there are clearly signicant differences in the way these
curves drop. In the case of untreated coir, it can be seen that rst
the force increases gradually till it reaches a maximum value, then
the force suddenly drops to a lower value. Subsequently, the ber
is sliding along the hole-surface until the total embedded length of

the ber is pulled-out of PBS matrix. This response agrees well


with that of a poor interface because of the incompatibility between hydrophilic ber and hydrophobic matrix [31,32]. This
behavior shows a small change in the case of 5N24 and 5N48 treated coir bers due to the removal of cuticles on the ber surface,
thus the bermatrix interaction is improved. In the case of
5N72 treated coir ber, the force shows no immediate drop after
it reaches the maximum value. This is due to the higher roughness
of alkali-treated ber surface leading to better interfacial bermatrix bond. The forcedisplacement curve of 5N96 treated coir ber
has a similar shape compared with 5N72 treated coir ber.
The mean IFSSs of untreated and alkali-treated coir ber/PBS
composites were shown in Fig. 8. Mean IFSS of untreated coir ber/PBS system calculated from maximal debonding force of single
ber pull-out tests is low (2.054 MPa), because of the incompatibility between hydrophilic ber and hydrophobic matrix and existence of the impurities on the coir ber surface. Fig. 8 also
showed the effect of soaking time on the IFSS between 5% alkalitreated coir ber and PBS matrix. The IFSS of 5N24, 5N48, 5N72

Fig. 7. Typical forcedisplacement curves of single ber pull-out tests for untreated
and different alkali-treated coir ber/PBS composite.

Fig. 8. IFSS of untreated and 5% alkali-treated coir ber/PBS composites with


different soaking time (mean value and standard deviation).

the micrograph in Fig. 6f depicted the removal of cuticles and globular particles creating the pits on the ber surface. However, it is
observed that the ber surface roughness of 7N72 treated coir ber
is lower than that of 5N72 due to the higher alkali concentration
which results in the higher removal of ber surface impurities.

3.3. Interfacial shear strength measurement

T.H. Nam et al. / Composites: Part B 42 (2011) 16481656

and 5N96 treated coir ber/PBS was 2.698 MPa, 2.942 MPa,
3.196 MPa and 3.016 MPa, respectively. It is observed that the IFSS
of alkali-treated coir bers reinforced PBS matrix increases with
increasing soaking time from 24 h to 72 h. This can be explained
due to the removal of cuticle layer on the ber surface (as seen
in Fig. 6) resulting in the increase of interfacial bermatrix adhesion. Furthermore, the removal of globular particles on the ber
surface during alkali treatment had led to a very rough ber surface with the pits (Fig. 6c). The pits could conveniently increase
the mechanical interlocking between the ber and PBS resin. However, the IFSS of 5N96 treated coir ber/PBS is lower than that of
5N72 treated ber. It can be explained that the surface of 5N96
treated coir ber (Fig. 6d) is smoother than that of 5N72 leading
to the less mechanical interlocking between the ber and PBS
resin.
Besides, the effect of NaOH concentration on the IFSS between
alkali-treated coir bers for 72 h and PBS matrix was shown in
Fig. 9. The mean IFSS of 3N72 and 7N72 treated coir ber/PBS is
2.732 MPa and 2.913 MPa, respectively and lower than that of
5N72 treated ber. This can be explained by the fact that the cuticles and globular particles still exist on the surface of 3N72 treated
coir ber (Fig. 6e) leading to less interfacial bermatrix adhesion.
The surface of 7N72 treated ber (Fig. 6f) was treated by high alkali
concentration resulting in decreasing mechanical interlocking between the ber and PBS resin. The results show that the higher
the surface roughness leads to higher IFSS.

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Fig. 10. Tensile strength of untreated and 5N72 treated coir ber/PBS biodegradable composites (mean value and standard deviation).

3.4. Tensile properties of the composites


Tensile properties of both untreated and alkali-treated coir/PBS
biodegradable composites with different ber mass content from
0% to 30% were represented in Figs. 1012. It can be realized that
tensile strength and modulus gradually increased with increasing
ber mass content from 0% to 25%, however there was a decrease
in the tensile strength and modulus of the composite with 30% ber mass content (as seen in Figs. 10 and 11). Regarding the untreated coir ber, the tensile strength and modulus of coir/PBS
biodegradable composites at 15%, 20%, 25% and 30% ber mass
content were 6.5% and 40.8%, 15.1% and 57.9%, 28.2% and 71.8%,
and 14.7% and 69.4% higher than those of pure PBS, respectively.
The increase in tensile strength and modulus of the composites is
due to the reinforcement of coir bers in PBS matrix in the direction of external load, because the strength and modulus of coir ber are higher than those of PBS matrix. Similar results were also
reported earlier for coir ber reinforced polyester composites

Fig. 11. Tensile modulus of untreated and 5N72 treated coir ber/PBS biodegradable composites (mean value and standard deviation).

Fig. 12. Elongation at break of untreated and 5N72 treated coir ber/PBS biodegradable composites (mean value and standard deviation).

Fig. 9. Effect of different NaOH concentration on the IFSS between 5% alkali-treated


coir bers for 72 h and PBS matrix (mean value and standard deviation).

[22]. The presence of coir bers in PBS matrix contributes effectively to enhance the tensile modulus of PBS resin. It is known
according to composite theory that the tensile modulus of a ber-reinforced composite depends on the modulus of the ber
and the matrix, the ber content and orientation.

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T.H. Nam et al. / Composites: Part B 42 (2011) 16481656

Besides, the increase in the tensile strength up to 25% ber content is due to increased wetting of the ber with the matrix. The
high tensile strength at the ber mass content of 25% might be also
due to adequate ber content in composites, which leads to greater
wetting. However, with 10% untreated ber mass content the
mean tensile strength of coir/PBS biodegradable composite slightly
decreased. This decrease may be explained by the poor wettability
leading to a weak interface. Therefore, at lower tensile stress, a
weak interface might form cracks, leading to failure similarly as
shown in [22]. In addition the decrease in tensile strength at 30%
ber mass content probably resulted from the poor ber wetting,
because the PBS resin content is not sufcient to wet all the ber
surfaces leading to poor interfacial adhesion.
Furthermore, the decrease in elongations at break which was
shown in Fig. 12 is mainly due to the structural integrity of PBS
being destroyed by the loading of coir ber, and increasing ber
content imply poor interfacial bermatrix adhesion, leading to
quicker fracture than pure PBS [4]. The elongation at break of untreated coir ber/PBS composite with 10% ber mass content signicantly reduced by approximately 35% compared to the one of
PBS resin. After such initial drop, the percent elongation at break
decreases inconsiderably or nearly remains constant with increasing ber content. This can be explained that the fracture of PBS matrix occurred before coir ber failure, since elongation at break of
coir bers are higher than that of PBS resin. This also indicates that
the ductile nature of PBS resin slightly decreases with the addition
of coir bers.
As demonstrated in Figs. 1012, alkali treatment of coir bers
improved the tensile properties of coir ber reinforced PBS biodegradable composites. Actually, alkali treatment is mainly a process
of surface activation leading to the formation of rough ber surface. As shown above, alkali treatment cleans surface impurities
and makes the roughness with many pits on the ber surface. This
was well depicted in Fig. 6 by comparing the SEM micrographs of
alkali-treated ber with the untreated ber. The formations of
the pits result in greater mechanical interlocking of the matrix
on the ber surfaces and make the interfacial adhesion stronger.
Therefore, the tensile properties of alkali-treated biocomposites
are signicantly greater than those of the untreated biocomposites.
The tensile strength and modulus of 5N72 treated coir ber/PBS
composites at 10%, 15%, 20%, 25% and 30% ber mass content were
21% and 22.1%, 22.4% and 24.1%, 24.1% and 29.4%, 20.5% and 40.8%,
and 14.2% and 25.2% higher than those of untreated coir ber/PBS
composites, respectively. The increase in tensile properties in case
of 5% alkali-treated ber composite may be due to greater ber
matrix interfacial and physical bonding, because physical bonding
also increases after alkali treatment due to the dipolar interactions
between bermatrix [22]. The experimental results in this study
show that best tensile properties can be obtained at the ber mass
content of 25%. Therefore, the results of tensile properties point out
the importance by using the right amount of natural ber as reinforcement in the composites.

3.5. Flexural properties of the composites


Effect of alkali treatment on exural properties of coir/PBS biodegradable composites with different ber mass content from 0%
to 30% was represented in Figs. 13 and 14. It is found that the exural properties are gradually increased with increasing ber mass
content from 0% to 25%, but with 30% ber content they are slightly
decreased or nearly remain constant. The decrease in mean exural
strength beyond 25% coir ber content can be explained due to a
shortage of PBS resin to fully wet out between the coir bers. Interestingly, the exural properties have the same trend as the tensile
properties with the increase of ber content.

Fig. 13. Flexural strength of untreated and 5N72 treated coir ber/PBS biodegradable composites (mean value and standard deviation).

Fig. 14. Flexural modulus of untreated and 5N72 treated coir ber/PBS biodegradable composites (mean value and standard deviation).

The alkali-treated coir ber/PBS composites yielded higher


mean exural properties compared to pure PBS resin and the untreated ones. This reects the contribution of sodium hydroxide
in terms of changes of ber properties and enhancement of bermatrix adhesion. Compared to pure PBS resin, alkali-treated
coir ber/PBS composites at 10%, 15%, 20%, 25% and 30% ber mass
content exhibited 20.9%, 23.1%, 34%, 45.7% and 42.9% enhancement
in exural strength and 45.6%, 51.1%, 76.6%, 97.4% and 95.6% in
exural modulus, respectively. In this study, the best exural properties can be obtained at ber mass content of 25% corresponding
with the tensile properties. Alkali-treated coir ber/PBS composite
reinforced with 25% ber content showed an increase in mean exural strength by 6% and mean exural modulus by 16.7% compared
to those of untreated ber. The results show that surface modication by alkali treatment has less inuence on exural properties
compared to tensile properties. This can be explained that the exural failure mode usually shows little or no ber pull-out [4], because applied force is perpendicular to reinforced bers of the
composite specimens in exural test.
The mechanical strength and modulus of coir ber/PBS biodegradable composite can show an optimum ber content. The optimum ber content varies with the nature of both ber and matrix,
ber aspect ratio, bermatrix interfacial adhesion, ber agglomeration, processing technique, end, etc. [4]. Similar investigations
have also been reported by Rout et al. [22] for coir/polyester composites in which the optimum ber content is about 1725%, by

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1655

(1) The mechanical properties of investigated coir bers have


been measured and evaluated. Alkali treatment of coir bers
improved signicantly their tensile properties.
(2) Alkali treatment of coir ber increased ber surface roughness leading to the increase of mechanical interlocking
between the ber and PBS matrix in the composites. Treatment of coir ber with 5% sodium hydroxide for 72 h
resulted in the highest ber surface roughness.
(3) Alkali treatment of coir ber enhanced the IFSS of coir ber/
PBS system. The highest IFSS between alkali-treated coir
ber and PBS matrix obtained when coir bers were soaked
in 5% sodium hydroxide for 72 h.
(4) Alkali treatment of coir bers increased the interfacial bonding strength and the wettability of the bers by PBS resin
leading to the enhancement in mechanical properties of
the composites.
(5) Mean mechanical strength and modulus of the composites
increased with increasing ber mass content up to 25%,
but over 25% ber content the tensile strength and modulus
of coir ber/PBS biodegradable composite decreased. The
authors propose that the 25% coir ber content reinforced
PBS biodegradable composites have the best tensile properties in this study.
(6) The experimental results in the present work suggest that a
useful composite with good strength could be successfully
developed using coir ber as a reinforcing agent for the
PBS matrix.
Fig. 15. SEM micrograph of tensile fractured surface of PBS biodegradable
composite reinforced with 20% mass content of: (a) untreated coir bers, (b)
5N72 treated coir bers.

References
Brahmakumar et al. [25] for coir/LDPE composites is about 25%,
and by Prasad et al. [15] for coir/polyester composites is about
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composites.
3.6. Fractured surface morphologies of the composites
Tensile fractured surface morphologies of untreated and alkalitreated coir ber/PBS composites were shown in Fig. 15. Fig. 15a
depicts several holes that were left after the bers are pulled-out
from the matrix. Visible gaps can be found between ber and
PBS matrix in Fig. 15a, suggesting poor interfacial adhesion. However, the gaps are almost disappeared in the case of 5N72 treated
coir ber (Fig. 15b), proving good compatibility being formed in
PBS composites leading to increase in the interfacial and mechanical properties of the composites. It is obvious that untreated coir
ber can be easily pulled-out from the interfacial region with poor
compatibility, resulting in rapid partial-collapse of PBS composite.
However, alkali-treated coir ber having a good adhesion with PBS
matrix can effectively disperse and transfer stress, leading to the
improvement in mechanical properties of coir/PBS biodegradable
composites. Consequently, the results suggest that alkali treatment
of coir ber is necessary to enhance the interfacial bermatrix
adhesion prior to composite processing.

4. Conclusions
Coir ber/PBS biodegradable composites with different ber
content have been developed. Effect of alkali treatment on the
interfacial and mechanical properties of coir ber/PBS biodegradable composites has been studied. The following conclusions can
be drawn from this study:

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