You are on page 1of 9

Composites: Part B 42 (2011) 1648–1656

Contents lists available at ScienceDirect

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

Effect of alkali treatment on interfacial and mechanical properties of coir fiber 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 fibers were developed. The effect of alkali treatment on the surface morphology and mechanical properties of coir fibers, interfacial shear strength (IFSS) and mechanical properties of coir fiber/PBS composites was studied. The effect of fiber mass content varying from 10% to 30% on the mechanical properties of coir fiber/PBS composites was also investigated. The coir fibers 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 fibers. The mechanical properties of alkali-treated coir fiber/PBS composites are significantly higher than those of untreated fibers. The best mechanical properties of alkali-treated coir fiber/PBS composite were achieved at fiber mass content of 25% in this study, which showed an increase of tensile strength by 54.5%, tensile modulus by 141.9%, flexural strength by 45.7% and flexural modulus by 97.4% compared to those of pure PBS resin. The fiber surface morphologies and fractured surface of the composites exhibited an improvement of interfacial fiber–matrix adhesion in the composites reinforced with alkali-treated coir fibers. Ó 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. Polymer–matrix composites (PMCs) B. Interface/interphase B. Mechanical properties E. Surface treatments

1. Introduction In the past decade, natural fiber 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 fiber composites are not fully environmentally friendly because matrix resins are non-biodegradable [3]. Therefore, biodegradable composites based on natural fibers and biodegradable polymeric matrix made from cellulose, starch, and other natural resources are called ‘‘green composites’’ and have been developed because of their environmentally beneficial properties [4–8]. In general, the research and development of natural fiber 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 fibers such as henequen, hemp, jute, kenaf, sisal, flax, bamboo, coir, banana, palm, silk, cotton and wood are renewable resources in many developing countries. These fibers offer specific benefits such as low cost, low density, low pollutant emissions, acceptable specific 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 Ó 2011 Elsevier Ltd. All rights reserved. doi:10.1016/j.compositesb.2011.04.001

characteristics, enhanced energy recovery, and complete biodegradability [9–12]. They are considered as strong candidates to replace the conventional glass fibers due to eco-friendliness, low cost, renewable resources and biodegradability. Among the natural fibers, plant fibers which contain strongly polarized hydroxyl groups are hydrophilic in nature [13]. These fibers are inherently incompatible with hydrophobic thermoplastics. Furthermore, due to the presence of pendant hydroxyl and polar groups in various constituents of fibers, moisture absorption of fibers 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 fibers by suitable surface chemical modification [14–17]. Among the plant fibers, coir fibers are nowadays extensively used in many industrial applications. Coir is a versatile lignocellulosic fiber extracted from the tissues surrounding the seed of coconut palm (Cocos nucifera). Coir consists of cellulosic fibers with hemicellulose and lignin as the bonding materials for the fibers. Table 1 summarizes several physical, chemical and mechanical properties of coir fiber compared with other typical natural fibers such as flax, hemp, jute, ramie and sisal [2,11,18]. Coir fiber has low cellulose and hemicellulose, high lignin content and high microfibrillar angle compared with other natural fibers (Table 1). As a result tensile strength and Young’s modulus of coir fiber are lower than those of other plant fibers. Coir fiber has low moduli due to high microfibrillar angle [19]. Besides, elongation at break

PBS has excellent biodegradability in nature. The high lignin content in coir fiber is responsible for other useful properties such as weather. sea.18]. The diameter (d) of coir fiber is calculated approximately as follows: d¼ pffiffiffiffiffiffi ab ð2Þ The coir fibers with the length exceeded 100 mm and the diameter varying from 100 to 450 lm were selected carefully to be used in this study. thus fiber cross sectional area (A) is determined approximately by a formula as follows: A¼ pab 4 ð1Þ where a and b are dimensions in Fig. Ltd. It can be completely combustible by fire without evolving toxic gases as described in [30]. Due to hardwearing quality. Finally. the Philippines and Indonesia. PBS can be a good candidate material for the matrix of biodegradable composites. Among the completely biodegradable polymers which have been frequently studied as biodegradable polymer matrices in the biocomposites. coir is used for marking a wide variety of floor-furnishing materials. such as coir-polypropylene and coir based polyester green composites [15–17. The melting temperature of the PBS is about 115 °C.6–7.33 100–300 74–75. 2). Ltd.2(B) 60–67(I) 10–13. mainly in India and Sri Lanka followed by Thailand.28]. Coir fiber surface morphology and fractured surfaces of untreated and alkali-treated coir fiber/PBS composites were investigated by scanning electron microscope (SEM) providing the information for the evaluation of interfacial fiber–matrix adhesion.. Therefore. According to official website of International Year for Natural Fibres 2009.21–25]. and compost [29]. Hence. tensile properties of untreated and alkali-treated coir fibers were reported.5–12 500–870 44 1. 1 depicts the chemical structure of PBS used in this study.2 41–45 30–45 105–175(I) 95–118(B) 4–6(I) 17–47(I) 23. so the fiber becomes stiffer and tougher.5 40–50 68–76 13–14 0. the coir fibers were air-dried for more than 2 days.2 550–900 70 1. polypropylene and polystyrene.6 8 Jute 1. The effect of alkali treatment and fiber content on mechanical properties of coir fiber/PBS biodegradable composites was studied.4 7 Hemp 1. 1. The effect of alkali treatment on the interfacial shear strength (IFSS) of coir fiber/PBS system was evaluated by single fiber pull-out test.2. Furthermore.1. 3 1649 Coir 1.9 8–12(I) 7.48 25 67–75 16–18 2.3 6. Vietnam.7 7. Bentre. Fig. Experimental 2. #1001. about 500. Showa High Polymers. 72 h and 96 h) at room temperature (RT).000 tonnes of coir are produced annually.11. Tokyo. yarn.5 100–450 36–43 0. The combination of coir fibers and PBS resin can produce the environment-friendly biodegradable composite.4(B) 10 Flax 1. Tokyo. Alkali treatment of coir fibers First of all coir fibers were treated with 5% NaOH solution in a glass beaker for different soaking time (24 h. the density is 1.8–12. fungal.25–1.8 12 Ramie 1. Properties/fibers Density (g/m ) Diameter (lm) Cellulose content (%) Hemicellulose content (%) Lignin content (%) Microfibrillar angle (°) Tensile strength (MPa) Young’s modulus (GPa) Elongation at break (%) Moisture absorption (%) (B) – Brazilian. and bacterial resistance [20]. The PBS biodegradable composites reinforced with untreated and alkali-treated coir fibers were fabricated by compression molding method.98(B) 10–20 600–700 38 3.. This property of coir fiber is certainly useful in cushion applications. durability and other advantages. 2 measured by an optical microscope MX-7575CS (Hirox Co.2 12–17 Sisal 1. Chemical structure of PBS used in the present study.64–5. rope. The mean IFSS of 5% alkali-treated coir fibers for 72 h which will be shown in next section is higher than that of untreated and other alkali-treated coir fibers.12(I) 2–2. It was found that the cross section of coir fiber is not completely circular (Fig. Materials Poly(butylene succinate) pellets (PBS.4 100 62–72 16–18 2–2. 48 h. Next the fibers were taken out of the solution. polylactic acid (PLA) and poly(butylene succinate) (PBS) are increasing commercial interest [26]. Japan).26–1.6–0.16–1.5(B) 11 of natural fibers increases with increasing microfibrillar angle. / Composites: Part B 42 (2011) 1648–1656 Table 1 Physical. (I) – Indian. Nam et al.9–51. lake. etc.T.. In the present work.26 g/cm3. then washed several times with fresh water and subsequently with distilled water. .8–3. aliphatic polyester and also biodegradable polymer.. An example of the application to seat cushion for automobiles is reported in [21]. another series of experiments with the same procedure were followed ex- Fig. The lignin content in coir fiber is quite high. the research and development efforts have been underway to find new utilization of coir as a reinforcement in polymer composites. thus the elongation at break of coir is the highest among typical natural fibers [20]. PBS is commercially available at lower cost than PLA.9 7–9 400–800 10–30 1. JSC.5 10 800–1500 60–80 1.45 60 59–71 12–13 11.H. 2. these traditional coir products consume only a small percentage of the potential total world production of coconut husk. Therefore. PBS can be naturally degraded into the environment by bacteria and fungi [27. Its total value is estimated at $100 million. chemical and mechanical properties of coir fiber compared with other natural fibers [2. The golden brown coir fibers in the present work were supplied from Betrimex.2–2. Vietnam. It has comparable mechanical properties with several thermoplastics such as polyethylene. However. A fully biodegradable composite reinforced by natural fibers is usually made from completely biodegradable polymeric matrix. However. 2. Japan) is thermoplastic. such as in soil.

3. mounted and glued on a paper tab before testing. The series are designated by 3NX. The average tensile properties of untreated and alkali-treated coir fibers were measured at least from thirty successful specimens. Next the dried coir fibers were slightly stretched out straight within the elastic region. 15%. The mean IFSSs between coir fibers and PBS matrix were obtained from twenty successful pull-out test specimens. glued by adhesive tape and placed in the mold between the PBS sheets. 5N24. The composite plates made from PBS and different untreated and alkali-treated coir fiber mass content (10%. The schematic representation of single fiber pull-out test is shown in Fig. then clamped securely between two steel mold plates and last quickly quenched by ice water. 5NX and 7NX in which 3N. Typical cross section of coir fiber.. 5% and 7% NaOH solution. 5N72. Composite fabrication To begin with coir fibers were dried at 80 °C in the vacuum oven for 24 h. . Individual untreated and alkali-treated coir fibers were carefully chosen. on the mold using glue as described in [25]. There seems to be no water uptake and no moisture absorption during Fig. Kyoto. The reaction of sodium hydroxide with coir fiber is described as follows: alkali-treated coir fibers having length over 120 mm were used for preparing pull-out test specimens by pressing the fibers between two PBS sheets using a hot press equipment (Imoto Corp. Single fiber 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. After that coir fibers were weighed and aligned in a parallel array. The fiber embedded length in the PBS matrix was obtained by cutting the fiber by punching a hole through the specimen. 5N and 7N corresponding to the soaking in 3%. Specimens with a thickness of 1 mm were removed from the mold after quickly cooling in ice water. 20%. IFSS value of untreated and alkali-treated coir fiber/PBS system was estimated from the maximum debonding force (Fd) using following equation: Coir—OH þ NaOH ! Coir—O Na þ H2 O 2. 2. 3.4. Schematic representation of single fiber pull-out test.. Canton. Interfacial characterization A single fiber pull-out test was used to measure the IFSS of untreated and alkali-treated coir fiber/PBS system. Schematic representation of the hot press used to fabricate composite plates. cept that the coir fibers 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. 2. Nam et al. / Composites: Part B 42 (2011) 1648–1656 Fig. Next the mold was removed from the press. Mean diameter of coir fiber was calculated using the formula (2) in which the dimensions of a and b were measured at the intersection between coir fiber and PBS matrix. respectively and X corresponding to the soaking time in hours. The untreated and The single fiber pull-out test was carried out for untreated. A force is applied to the free end of fiber to pull it out of the matrix while the force is continuously monitored and recorded. Gauge length of single fiber tensile specimens is 10 mm. The fibers were kept straight and oriented by fixing its both ends.H. Coir fiber characterization À þ ð 3Þ s¼ Fd pÂdÂL ð4Þ The single fiber tensile tests were carried out by a universal testing machine Instron 4442 (Instron Corp. 3N72 and 7N72 treated coir fibers to investigate the effect of soaking time and concentration of sodium hydroxide on the IFSS of coir fiber/PBS system in order to make a right choice of alkali treatment. MA) with a crosshead speed of 5 mm/min at RT. extending outside the PBS sheets. 4. Japan). in which d is mean diameter of coir fiber and L is embedded length. 5N96. 2. 25% and 30%) were fabricated using above hot press equipment. Then they were cut into the segments with the length of 100 mm. Fig.5.3.1650 T. 5N48. 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.

21 + 37. The dimension of flexural specimens was 50 Â 25 Â 1 mm3.52 ± 38. 3. Smooth surface of 5N96 treated coir fiber can be explained due to the removal of all globular particles and cuticles deposited on the fiber surface.54 5. The flexural test was carried out at RT with a crosshead speed of 2 mm/ min.42 218.60 32. 2.85 29.76 4.81 5.38 227. respectively.73 5. the micrograph in Fig.27 ± 0. The globular particles which cover the pits on the cell walls are embedded in the fiber surface [15]. 6a). With alkali concentration of 7%.1. Coir fiber Untreated 5N24 treated 5N48 treated 5N72 treated 5N96 treated 3N72 treated 7N72 treated Strength (MPa) 139. Both PBS sheets and composite plates were prepared with the same thermal history.84 5.10 33. 5) were glued by two glass fiber reinforced plastic (GFRP) tabs. / Composites: Part B 42 (2011) 1648–1656 1651 quenching of the sample. Tensile test The tensile specimens of 100 Â 10 Â 1 mm3 were cut out from pure PBS and composite plate by cutting machine AC-300CF (MARUTO Testing Machine Co.96 ± 5.70 ± 5.09 209. Nam et al.40 ± 3. but over 5% they decreased. b and h are the width and thickness of the specimen.5 mm/min. nearly all globular particles on the fiber surface were intact. Tensile specimens were chosen carefully before testing.95 ± 0.44 .07 ± 35. Lignin.H. 6 showed the effect of different alkali treatment on the coir fiber surface.52 ± 6. The both clamped ends of the specimens (Fig.13 30.43 ± 40. Effect of alkali treatment on coir fiber surface rf ¼ Ef ¼ 3FLs 2bh 2 ð 5Þ L3 sm 4bh 3 ð 6Þ Alkali treatment improves the fiber–matrix adhesion due to the removal of natural and artificial impurities from the fiber surface as well as changing in the arrangement of units in the cellulose macromolecule [31]. Ls is the length of support span. The mean flexural properties of each composite were obtained from five successful test specimens. Japan). Fig. SEM micrograph of untreated coir fiber shows globular particles and cuticles on the fiber surface (Fig. However the strain at failure of coir fiber is quite high compared with other natural and synthetic fibers such as glass and carbon.6. The increase in tensile strength and modulus of coir fiber after alkali treatment was explained in detail [15]. flax. The mean tensile properties of pure PBS and coir fiber/PBS composites were obtained from five successful specimens for each fiber content. 6e).67 ± 39.15 Modulus (GPa) 2. The flexural strength (rf) and modulus (Ef) were calculated using the following equations: where F is the maximal applied force. The mean tensile strength of coir fiber is quite low compared to other natural fiber such as jute. but the surface impurities were removed. Japan). The tensile strength and modulus of coir fibers increased by about 71% and 113% when the fibers were soaked in 5% sodium hydroxide solution for 72 h. Osaka. being a phenolic natural polymer.. but they decreased beyond 72 h. All the tensile tests were carried out at RT with a crosshead speed of 0. Kyoto.64 ± 0.74 30.82 Failure strain (%) 29. thus the roughness of fiber surface increased. m is the slope of the force–deflection curve. Results and discussion 3. respectively.69 228. alkali treatment of coir fibers improved significantly their tensile properties.68 ± 0.54 ± 37. Morphological characterization The coir surface morphologies and fractured surface of the composites after tensile tests were examined using SEM (VE-7800. hemp. The removal of cuticle layer will expose lignin on the fiber surface. Fig. ramie or sisal fiber. Alkali treatment increases the surface roughness and the amount of cellulose exposed on the fiber surface resulting in better mechanical interlocking [16]. In addition with the soaking time of 72 h tensile properties of coir fiber increased with increasing concentration of alkali solution up to 5%. 6c). 3. Therefore.89 31. For alkali concentration of 3% (Fig. Some of globular particles were intact but at a few isolated places they were removed creating the pits on 5N48 treated coir fiber surface (Fig.59 ± 4. 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. 6b). As shown in Table 2.86 238. 6d shows that 5N96 treated coir fiber surface is smoother than that of 5N72 fiber surface. 5.79 ± 0. Keyence Inc. Table 2 The mean tensile properties of untreated and alkali-treated coir fiber. the development of a rough surface tomography and enhancement in aspect ratio offer better fiber–matrix interfacial bond resulting in increasing mechanical properties.2. Tensile properties were measured according to JIS K7113 using a universal testing machine Senstar SC-5H (JT Tohsi Inc. 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 fibers increased.T. Strain gauges were glued at the center of the specimens to measure the elongation at break. Effect of alkali treatment on mechanical properties of coir fiber Tensile properties of untreated and alkali-treated coir fiber were presented in Table 2. 2. The ratio between span distance and thickness of pure PBS and composite specimens was 16. Tokyo. Tokyo.. 4.53 ± 3. Shape and dimensions of tensile specimen.8.79 5.92 ± 0.7. Flexural test The flexural properties of pure PBS and coir fiber/PBS biodegradable composites were measured by a three-point bending method according to JIS K7171 standard using universal testing machine Autograph AGS-1000A (Shimadzu.47 ± 0. However. Japan) and kept in desiccator at 25 °C and 35% relative humidity before testing. Japan). The schematic representation of the hot press for composite fabrication is shown in Fig.00 ± 4.26 ± 39..91 210. 2. should be chemically compatible with PBS resin. Flexural specimens were chosen carefully before testing.

7. The mean IFSSs of untreated and alkali-treated coir fiber/PBS composites were shown in Fig. 7. 8 also showed the effect of soaking time on the IFSS between 5% alkalitreated coir fiber and PBS matrix. 8. the micrograph in Fig. However. This behavior shows a small change in the case of 5N24 and 5N48 treated coir fibers due to the removal of cuticles on the fiber surface. In the case of untreated coir. (e) 3N72 treated fiber. . 6f depicted the removal of cuticles and globular particles creating the pits on the fiber surface. and (f) 7N72 treated fiber.1652 T. it can be seen that first the force increases gradually till it reaches a maximum value. IFSS of untreated and 5% alkali-treated coir fiber/PBS composites with different soaking time (mean value and standard deviation). Fig.H. once the force reaches its maximum value there are clearly significant differences in the way these curves drop. This is due to the higher roughness of alkali-treated fiber surface leading to better interfacial fiber–matrix bond. because of the incompatibility between hydrophilic fiber and hydrophobic matrix and existence of the impurities on the coir fiber surface.3. This response agrees well with that of a poor interface because of the incompatibility between hydrophilic fiber and hydrophobic matrix [31. However. (c) 5N72 treated fiber. Interfacial shear strength measurement The typical force–displacement curves obtained from single fiber pull-out test for the untreated and alkali-treated coir fiber reinforced PBS composites were shown in Fig. (b) 5N48 treated fiber. / Composites: Part B 42 (2011) 1648–1656 Fig. In the case of 5N72 treated coir fiber. (d) 5N96 treated fiber. thus the fiber–matrix interaction is improved. the fiber is sliding along the hole-surface until the total embedded length of the fiber is pulled-out of PBS matrix. Nam et al. the force shows no immediate drop after it reaches the maximum value. it is observed that the fiber surface roughness of 7N72 treated coir fiber is lower than that of 5N72 due to the higher alkali concentration which results in the higher removal of fiber surface impurities. 5N72 Fig. Typical force–displacement curves of single fiber pull-out tests for untreated and different alkali-treated coir fiber/PBS composite. 3. The IFSS of 5N24. 6. Mean IFSS of untreated coir fiber/PBS system calculated from maximal debonding force of single fiber pull-out tests is low (2. SEM micrographs of coir fibers: (a) untreated fiber. then the force suddenly drops to a lower value.054 MPa).32]. The force–displacement curve of 5N96 treated coir fiber has a similar shape compared with 5N72 treated coir fiber. 5N48. Fig. 8. Subsequently. It can be noted that all the curves exhibit nonlinear behavior due to the characteristics of the ductile matrix.

Fig. Regarding the untreated coir fiber.942 MPa.8%. 20%. 6) resulting in the increase of interfacial fiber–matrix adhesion. 6f) was treated by high alkali concentration resulting in decreasing mechanical interlocking between the fiber and PBS resin. and 14. Elongation at break of untreated and 5N72 treated coir fiber/PBS biodegradable composites (mean value and standard deviation). 10. 3. Fig. however there was a decrease in the tensile strength and modulus of the composite with 30% fiber mass content (as seen in Figs. It can be realized that tensile strength and modulus gradually increased with increasing fiber mass content from 0% to 25%. However. because the strength and modulus of coir fiber are higher than those of PBS matrix. Effect of different NaOH concentration on the IFSS between 5% alkali-treated coir fibers for 72 h and PBS matrix (mean value and standard deviation).196 MPa and 3. 6c). Nam et al. 11. This can be explained by the fact that the cuticles and globular particles still exist on the surface of 3N72 treated coir fiber (Fig.913 MPa. 6d) is smoother than that of 5N72 leading to the less mechanical interlocking between the fiber and PBS resin. the IFSS of 5N96 treated coir fiber/PBS is lower than that of 5N72 treated fiber. It is known according to composite theory that the tensile modulus of a fiber-reinforced composite depends on the modulus of the fiber and the matrix. The mean IFSS of 3N72 and 7N72 treated coir fiber/PBS is 2. Tensile modulus of untreated and 5N72 treated coir fiber/PBS biodegradable composites (mean value and standard deviation).9%. Fig. 3.4.8%. 6e) leading to less interfacial fiber–matrix adhesion. Tensile properties of the composites Tensile properties of both untreated and alkali-treated coir/PBS biodegradable composites with different fiber mass content from 0% to 30% were represented in Figs.5% and 40. 28.732 MPa and 2. The surface of 7N72 treated fiber (Fig. It is observed that the IFSS of alkali-treated coir fibers reinforced PBS matrix increases with increasing soaking time from 24 h to 72 h.7% and 69. Besides. Furthermore. 15. The increase in tensile strength and modulus of the composites is due to the reinforcement of coir fibers in PBS matrix in the direction of external load. It can be explained that the surface of 5N96 treated coir fiber (Fig. respectively. The presence of coir fibers in PBS matrix contributes effectively to enhance the tensile modulus of PBS resin. This can be explained due to the removal of cuticle layer on the fiber surface (as seen in Fig. . The results show that the higher the surface roughness leads to higher IFSS. the fiber content and orientation. 9. [22]. the removal of globular particles on the fiber surface during alkali treatment had led to a very rough fiber surface with the pits (Fig. 10–12. 10 and 11). / Composites: Part B 42 (2011) 1648–1656 1653 and 5N96 treated coir fiber/PBS was 2. 12.T. respectively and lower than that of 5N72 treated fiber. The pits could conveniently increase the mechanical interlocking between the fiber and PBS resin. 9. Similar results were also reported earlier for coir fiber reinforced polyester composites Fig.H.1% and 57.016 MPa. 2. the tensile strength and modulus of coir/PBS biodegradable composites at 15%. 25% and 30% fiber mass content were 6.4% higher than those of pure PBS. respectively. Tensile strength of untreated and 5N72 treated coir fiber/PBS biodegradable composites (mean value and standard deviation). the effect of NaOH concentration on the IFSS between alkali-treated coir fibers for 72 h and PBS matrix was shown in Fig.698 MPa.2% and 71.

25% and 30% fiber mass content were 21% and 22. 76. because applied force is perpendicular to reinforced fibers of the composite specimens in flexural test. Alkali-treated coir fiber/PBS composite reinforced with 25% fiber content showed an increase in mean flexural strength by 6% and mean flexural modulus by 16.4% and 95. 34%. with 10% untreated fiber mass content the mean tensile strength of coir/PBS biodegradable composite slightly decreased. This can be explained that the fracture of PBS matrix occurred before coir fiber failure. respectively. a weak interface might form cracks. Fig. 15%. As demonstrated in Figs.2% and 25. It is found that the flexural properties are gradually increased with increasing fiber mass content from 0% to 25%. processing technique. 6 by comparing the SEM micrographs of alkali-treated fiber with the untreated fiber. by . Therefore. 45. 10–12. Compared to pure PBS resin. Flexural properties of the composites Effect of alkali treatment on flexural properties of coir/PBS biodegradable composites with different fiber mass content from 0% to 30% was represented in Figs. which leads to greater wetting.1%. This reflects the contribution of sodium hydroxide in terms of changes of fiber properties and enhancement of fiber–matrix adhesion. Flexural modulus of untreated and 5N72 treated coir fiber/PBS biodegradable composites (mean value and standard deviation). In this study. leading to failure similarly as shown in [22]. This decrease may be explained by the poor wettability leading to a weak interface. 15%. fiber aspect ratio. The optimum fiber content varies with the nature of both fiber and matrix. The experimental results in this study show that best tensile properties can be obtained at the fiber mass content of 25%.5% and 40. 24. at lower tensile stress. The mechanical strength and modulus of coir fiber/PBS biodegradable composite can show an optimum fiber content. The decrease in mean flexural strength beyond 25% coir fiber content can be explained due to a shortage of PBS resin to fully wet out between the coir fibers. [4]. alkali treatment of coir fibers improved the tensile properties of coir fiber reinforced PBS biodegradable composites.H. fiber agglomeration. The results show that surface modification by alkali treatment has less influence on flexural properties compared to tensile properties. 20%. The formations of the pits result in greater mechanical interlocking of the matrix on the fiber surfaces and make the interfacial adhesion stronger. 13. the tensile properties of alkali-treated biocomposites are significantly greater than those of the untreated biocomposites. The high tensile strength at the fiber mass content of 25% might be also due to adequate fiber content in composites.4% and 24. Therefore. Similar investigations have also been reported by Rout et al. [22] for coir/polyester composites in which the optimum fiber content is about 17–25%. fiber–matrix interfacial adhesion. the results of tensile properties point out the importance by using the right amount of natural fiber as reinforcement in the composites. This also indicates that the ductile nature of PBS resin slightly decreases with the addition of coir fibers. Interestingly.5. 14. / Composites: Part B 42 (2011) 1648–1656 Besides. because physical bonding also increases after alkali treatment due to the dipolar interactions between fiber–matrix [22]. After such initial drop. leading to quicker fracture than pure PBS [4].4%.6% in flexural modulus. end. the flexural properties have the same trend as the tensile properties with the increase of fiber content. Actually. since elongation at break of coir fibers are higher than that of PBS resin. alkali-treated coir fiber/PBS composites at 10%. 20. 97. because the PBS resin content is not sufficient to wet all the fiber surfaces leading to poor interfacial adhesion. the decrease in elongations at break which was shown in Fig.1%.1%. etc. the best flexural properties can be obtained at fiber mass content of 25% corresponding with the tensile properties.1%. 23.9%. 20%. and increasing fiber content imply poor interfacial fiber–matrix adhesion. The elongation at break of untreated coir fiber/PBS composite with 10% fiber mass content significantly reduced by approximately 35% compared to the one of PBS resin. 25% and 30% fiber mass content exhibited 20. but with 30% fiber content they are slightly decreased or nearly remain constant. As shown above.1% and 29. the percent elongation at break decreases inconsiderably or nearly remains constant with increasing fiber content.6%. 51.6%. respectively.1654 T. 12 is mainly due to the structural integrity of PBS being destroyed by the loading of coir fiber. alkali treatment cleans surface impurities and makes the roughness with many pits on the fiber surface.7% compared to those of untreated fiber. Flexural strength of untreated and 5N72 treated coir fiber/PBS biodegradable composites (mean value and standard deviation). This was well depicted in Fig.8%. 3. The increase in tensile properties in case of 5% alkali-treated fiber composite may be due to greater fiber– matrix interfacial and physical bonding. 13 and 14. and 14.2% higher than those of untreated coir fiber/PBS composites. The alkali-treated coir fiber/PBS composites yielded higher mean flexural properties compared to pure PBS resin and the untreated ones. Therefore. In addition the decrease in tensile strength at 30% fiber mass content probably resulted from the poor fiber wetting. However. the increase in the tensile strength up to 25% fiber content is due to increased wetting of the fiber with the matrix. The tensile strength and modulus of 5N72 treated coir fiber/PBS composites at 10%.9% enhancement in flexural strength and 45. This can be explained that the flexural failure mode usually shows little or no fiber pull-out [4]. Fig. 22. alkali treatment is mainly a process of surface activation leading to the formation of rough fiber surface. Furthermore. Nam et al.7% and 42.

100:4972–80. Composites Part B 2009. However. Surface treatment of coir (Cocos nucifera) fibers and its influence on the fibers’ physico-mechanical properties. Ferreira AS. Yu W.13(4):460–76. Physico-mechanical properties of chemically treated coir reinforced polypropylene composites. Composites Part A 2010. Okada A. the results suggest that alkali treatment of coir fiber is necessary to enhance the interfacial fiber–matrix adhesion prior to composite processing. Lee SG. Lau KT.T. Khan MA. References Brahmakumar et al. Mechanical properties in a bamboo fiber/PBS biodegradable composite. [16] Rahman MM. 15b).58(11):80–6. [17] Islam MN. (6) The experimental results in the present work suggest that a useful composite with good strength could be successfully developed using coir fiber as a reinforcing agent for the PBS matrix. 15a. Lee SM. The authors propose that the 25% coir fiber content reinforced PBS biodegradable composites have the best tensile properties in this study. In this study. Kobayashi S. Pavithran C. Fig. Development of high strength biodegradable composites using Manila hemp fiber and starch-based biodegradable resin. [5] Han SO. / Composites: Part B 42 (2011) 1648–1656 1655 (1) The mechanical properties of investigated coir fibers have been measured and evaluated. Lu X. Cho D. Nam et al. Polym Compos 2008. [12] Zhang MQ. tougher. Haque MM. Polym Sci Technol 2002.40:655–63. Park WH. Liu T.6. and environmentally friendly. J Mater Sci 1983. Cardona F. Park WH. the gaps are almost disappeared in the case of 5N72 treated coir fiber (Fig. leading to the improvement in mechanical properties of coir/PBS biodegradable composites. (3) Alkali treatment of coir fiber enhanced the IFSS of coir fiber/ PBS system. [3] Cho D.36:523–34. [1] Holbery J.H.2(3):291–9. Anandjiwala RD. Nascimento DCO. 15. [15] for coir/polyester composites is about 30%. Composites Part A 2006. [6] Cheng S. J Solid Mech Mater Eng 2008.65:2514–25. biodegradable polymers and biocomposites: an overview. Effect of alkali treatment on the interfacial and mechanical properties of coir fiber/PBS biodegradable composites has been studied. Biofibres. [14] John MJ. Yu J. Treatment of coir fiber with 5% sodium hydroxide for 72 h resulted in the highest fiber surface roughness. 3.34(9):982–1021. resulting in rapid partial-collapse of PBS composite. Mechanical properties of poly(butylene succinate) (PBS) biocomposite reinforced with surface modified jute fibre. J Appl Polym Sci 2006. [25] for coir/LDPE composites is about 25%. 15a depicts several holes that were left after the fibers are pulled-out from the matrix. The highest IFSS between alkali-treated coir fiber and PBS matrix obtained when coir fibers were soaked in 5% sodium hydroxide for 72 h. Berg JC. the incorporation of 25% fiber mass content showed best mechanical properties of coir fiber/PBS biodegradable composites. Visible gaps can be found between fiber and PBS matrix in Fig. Natural fiber reinforced polymer composites in automotive applications. Lau KT. Cheng L. However.37:1879–83. JOM 2009. Natural fibre-reinforced composites for bioengineering and environmental engineering applications. [2] Cheung HY. Composites Part A 2009. (4) Alkali treatment of coir fibers increased the interfacial bonding strength and the wettability of the fibers by PBS resin leading to the enhancement in mechanical properties of the composites. Houston D. Fig. Alkali treatment of coir fibers improved significantly their tensile properties. SEM micrograph of tensile fractured surface of PBS biodegradable composite reinforced with 20% mass content of: (a) untreated coir fibers.67:2369–76. Huque MM. Composites Part B 2009. Lopes FPD.276/277:1–24. [15] Prasad SV. Wypych F. (2) Alkali treatment of coir fiber increased fiber surface roughness leading to the increase of mechanical interlocking between the fiber and PBS matrix in the composites. [9] Mohanty K. Compos Sci Technol 2005. Mechanical and thermal properties of waste silk fiber-reinforced poly(butylene succinate) biocomposites. Fully biodegradable natural fiber composites from renewable resources: all plant fiber composites. [4] Liu L. Prog Polym Sci 2009. Arizaga GGC. Natural-fiber polymer– matrix composites: cheaper. Mechanical and thermal properties of chicken feather fiber/PLA green composites. Yin Y. Han SO. Hinrichsen G. J Appl Polym Sci 1988. Surface energy of untreated and surface-modified cellulose fibres. [7] Ochi S. Rong MZ. Lam PM. Ho MP. Conclusions Coir fiber/PBS biodegradable composites with different fiber content have been developed. and by Prasad et al. Macromol Mater Eng 2000.29(2):187–207. [13] Westerlind BS. [10] Monteiro SN. Misra M.61(1):17–22.40:650–4. alkali-treated coir fiber having a good adhesion with PBS matrix can effectively disperse and transfer stress. 15. Rohatgi PK. 4. Consequently. Alkali treatment of coir fibers for coir– polyester composites. Hui D. [8] Ogihara S. Rahman MR.18:1443–54. [11] Satyanarayana KG. Compos Sci Technol 2007. but over 25% fiber content the tensile strength and modulus of coir fiber/PBS biodegradable composite decreased. Eco-friendly biocomposites materials using biofibres. (5) Mean mechanical strength and modulus of the composites increased with increasing fiber mass content up to 25%.41:192–8. Fractured surface morphologies of the composites Tensile fractured surface morphologies of untreated and alkalitreated coir fiber/PBS composites were shown in Fig. proving good compatibility being formed in PBS composites leading to increase in the interfacial and mechanical properties of the composites. (b) 5N72 treated coir fibers. Zhao Y. Recent development in chemical modification and characterization of natural fiber-reinforced composites.40:669–74. The following conclusions can be drawn from this study: . suggesting poor interfacial adhesion. It is obvious that untreated coir fiber can be easily pulled-out from the interfacial region with poor compatibility. Biodegradable composites based on lignocellulosic fibers – an overview. JOM 2006.

[23] Asasutjarit C. / Composites: Part B 42 (2011) 1648–1656 interfacial bonding and strength of composites. Luo S.34:3709–19.40:633–7. J Appl Polym Sci 2001. J Mater Sci 1999. Herrera-Franco PJ. J Appl Polym Sci 2000. Properties and biodegradation of poly(ethylene adipate) and poly(butylene succinate) containing styrene glycol units. Eur Polym 2000. Cervantes-Uc JM. Composites Part B 1999. Terrones LAH. Lee SM.1656 T.76:1197–206. Lopes FPD. [18] Satyanarayana KG. Kim MN. editors. Compos Sci Technol 2005.H. J Appl Polym Sci 2000. Khedari J. [21] Monteiro SN. Kim DY. Wang A. Park WH. Mohanty AK. Characterization of natural fibers. Masuda T.36(12):2693–8.65:653–69. Mechanical strength of polyester matrix composites reinforced with coconut fiber wastes. Interfacial and mechanical properties of environmentfriendly ‘‘green’’ composites made from pineapple fibres and poly(hydroxybutyrate-co-valerate) resin. Valadez-Gonzalez A. Netravali AN.40:222–37. Drzal LT. [24] Leblanc JL. Rhee YH. Pavithran C. In: Fakirov S. [20] Satyanarayana KG. Investigating polypropylene–green coconut fiber composites in the molten and solid states through various techniques. Charoenvai S. Choa D.65:647–57. Biodegradable polymers/bamboo fiber biocomposite with bio-based coupling agent. Munich: Hanser Publishers. Plasma surface treatments and biodegradation of poly (butylene succinate) sheets.10(4):571–6.102:1922–36. d’Almeida JRM. Pillai RM. [25] Brahmakumar R. Furtado CRG. Rev Mater 2005. Materials and mechanical properties of pretreated coir-based green composites. Misra M. p. Yoon JS. blends and composites. Nakayama K. Engineering biopolymers homopolymers. Nayak SK. De Souza DA. Bhattacharyya D. Visconte LLY.30:309–20. Composites Part B 2009. Lee SH. Han SO. Composites Part A 2006. Jin HJ. [19] Silva GG. Kulkarni AG. Lee BY. Biodegradation of microbial and synthetic polyesters by fungi. [22] Rout J. Wypych F.61(4):300–8. Appl Microbiol Biotechnol 2003. Leite MCAM. Novel silk/poly(butylene succinate) biocomposites: the effect of short fibre content on their mechanical and thermal properties. J Appl Polym Sci 2006. Lee SG. Effect of fiber surface treatment on the fiber–matrix bond strength of natural fiber reinforced composites. Ishizaki MH. 3–48. Machado JC. Mechanical and thermal characterization of native Brazilian coir fiber. J Sci Ind Res 1981. Rohatgi PK. Tsujisaka T. Tripathy SS.37:80–91. Coconut fibre reinforced polyethylene composites: effect of natural waxy surface layer of the fibre on fibre/matrix [26] [27] [28] [29] [30] [31] [32] . 2007.78:1121–9. Hourston DJ. Potential of natural fibres as a resource for industrial material in Kerala. Nam et al. Compos Sci Technol 2005. Hirotsu T.22:468–76. Hirunlabh J. The influence of fiber surface modification on the mechanical properties of coir–polyester composites. Olayo R.