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

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.

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

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

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 Density (g/m ) Diameter (lm) Cellulose content (%) Hemicellulose content (%) Lignin content (%) Microbrillar angle () Tensile strength (MPa) Youngs modulus (GPa) Elongation at break (%) Moisture absorption (%) (B) Brazilian; (I) Indian.
3

1649

Coir 1.251.5 100450 3643 0.2 4145 3045 105175(I) 95118(B) 46(I) 1747(I) 23.951.4(B) 10

Flax 1.4 100 6272 1618 22.5 10 8001500 6080 1.22.4 7

Hemp 1.48 25 6775 1618 2.83.3 6.2 550900 70 1.6 8

Jute 1.45 60 5971 1213 11.812.9 79 400800 1030 1.161.8 12

Ramie 1.5 4050 6876 1314 0.60.7 7.512 500870 44 1.2 1217

Sisal 1.261.33 100300 7475.2(B) 6067(I) 1013.9 812(I) 7.67.98(B) 1020 600700 38 3.645.12(I) 22.5(B) 11

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
4

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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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:

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:

CoirOH NaOH ! CoirO Na H2 O

2.3. Coir ber characterization

Fd

pdL

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

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

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

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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:

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

rf
Ef

3FLs 2bh
2

L3 sm 4bh
3

6
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%,

Fig. 5. Shape and dimensions of tensile specimen.

Table 2 The mean tensile properties of untreated and alkali-treated coir ber. Coir ber Untreated 5N24 treated 5N48 treated 5N72 treated 5N96 treated 3N72 treated 7N72 treated Strength (MPa) 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 Modulus (GPa) 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 Failure strain (%) 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

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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 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 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).

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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.

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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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.

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).

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.

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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(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 30%. In this study, the incorporation of 25% ber mass content showed best mechanical properties of coir ber/PBS biodegradable 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.
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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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