IOP Conference Series: Materials Science and Engineering PAPER • OPEN ACCESS The Tensile Strength of Petung Bamboo Fiber Reinforced Epoxy Composites: The Effects of Alkali Treatment, Composites Manufacturing, and Water Absorption To cite this article: Gunawan Refiadi et al 2019 IOP Conf. Ser.: Mater. Sci. Eng. 547 012043 View the article online for updates and enhancements. This content was downloaded from IP address 114.5.219.184 on 07/09/2019 at 08:07 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 The Tensile Strength of Petung Bamboo Fiber Reinforced Epoxy Composites: The Effects of Alkali Treatment, Composites Manufacturing, and Water Absorption Gunawan Refiadi1* Yusi Syamsiar2 Hermawan Judawisastra3 1 Mechanical Engineering Vocational Education Study Program, College of Teacher Training and Education (STKIP) Sebelas April, Jl. Anggrek Situ 10 Sumedang 45323, Indonesia 2 Textile Chemistry Department, Polytechnic of Textile Technology, Jl. Jakarta 31 Bandung 40272, Indonesia 3 Material Engineering Department, Faculty of Mechanical and Aerospace Engineering, Bandung Institute of Technology (ITB), Jl.Ganesha 10 Bandung 40132, Indonesia *gunawan_refiadi@stkip11april.ac.id Abstract. Natural fiber application due to its competitiveness attracted many research in green composites. However, the tensile properties of natural fiber composites might be influenced by several factors such as treatment of the fibers, manufacturing processes, and water absorption levels. In this research, we use petung bamboo fibers as natural fibers candidate for a good reinforcement in green composites. The study focused on the tensile property of bamboo fiber reinforced epoxy composites due to alkali treatment, manufacturing process, and water absorption. The composites were made with three variations: the fibers were varied without and with alkaline treatment (5% NaOH); manual lay-up method and hot press were applied as manufacturing variation; moisture content in the composites was varied in dry condition and after water absorption treatment. Tensile testing and Scanning Electron Microscope (SEM), were performed to improve tensile strength of composite and fiber-matrix interface quality. The alkali treatment has less effect to the tensile strength than of the volume fraction gain and the void content. Composite manufacturing by hot press has a significant effect to the improvement of tensile strength up to 37% compare to the hand lay-up method. Water absorption up to 8.8% had decreased the tensile strength of composites up to 29%. The alkali treatment on the bamboo fibers had effectively reduced water absorption into the composite as well as the tensile strength reduction. Keywords: petung bamboo, alkali treatment, composites manufacturing, water absorption 1. Introduction Polymeric composites such as CFRP (Carbon Fiber-Reinforced Polymer) and GFRP (Glass Fiber-Reinforced Polymer) had abundantly produced due to their advantages as well as high mechanical specific performances. Unfortunately, the drawback of those materials is lack of sustainable environment due to pollutant expel both to the air and the land. However, this limitation in turn opens up other material research opportunities such as green composites. The composites use lignocellulosic structure natural resources as reinforcement such as ramie, coconut, hemp, jute, and bamboo. In tropical country such Indonesia, bamboo has a potential advantage as an abundance resource of natural fibers. In addition, bamboo have low-cost, fast Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI. Published under licence by IOP Publishing Ltd 1 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 growth, renewable, CO2 free, flexibility, as well high specific strength and stiffness compared to glass fiber [1][2]. Several considerable research dealing with bamboo were reviewed [3] and in Indonesia petung bamboo (Dendrocalamus asper) in the form of stems, slats, and fibers was studied also [4]–[6]. However, petung bamboo fibers as well as the other lignocellulose materials still have several weaknesses and problems. High variability in properties and high moisture absorption [7] affected the interfacial bonding quality between fibers and matrix. Meanwhile, composite materials in its application could be affected by hygroscopic conditions. To face the problem, several chemical methods such as alkalization, graph copolymerization, and coupling agents have been proposed to improve both interfacial quality and hydrophobing of the fibers [8], [9]. Studies of water absorption effects on bamboo fiberreinforced polyester through fibers surface modifications through alkali treatment [6] have been reported. In terms of composite manufacture methods, hand layup and hot press were commonly used to fabricate natural fiber composites considering time and cost [11]. However, the effects of combination between manufacturing methods, alkali treatment and water absorption to tensile properties of petung bamboo fiber reinforced composite has not been investigated yet. This study is aimed to investigate tensile strength of petung bamboo fiber-reinforced epoxy composites resulting from alkali treatment, composites manufacturing, and water absorption. 2. Materials and Methods 2.1 Materials Supplied from Hutan Penelitian Bambu in Arcamanik, Bandung (West Java, Indonesia), petung bamboo stems then extracted into 100~300 mm fiber bundles by chemo-mechanical methods. The resulting fibers then variably prepared both by non-alkali (NA) and alkali method using 5% v/v NaOH solution (A). Resulted before [12], both treated fibers (NA and A) has density of 1.05 and 1.11 g/mm3, respectively. The 5% alkali was found as the optimum solution resulted maximum bamboo fiber strength [12] and least water uptake in bamboo composites [10]. The matrix used in this study was Lycal GLR 1011 Part A epoxy resin with curing agent GLR 1011 Part B with density of 1.13 g/mm3. 2.2 Composites Manufacturing and Testing Prior to composites manufacturing by hand lay-up (LU) and hot press (HP) methods, bamboo fibers were oven dried 24 hours – 110oC to achieve dry condition. After petung bamboo fiber aligned unidirectionally on the molding surface, we poured epoxy mixing. For HP method, pressure, temperature, and holding time were set on 10 MPa 60 oC, and 1 hour, respectively. With the LU process, impregnation were apllied manually using specific roll at 25oC. Demolding then performed after the composite 24 h cured. Composites characterization were evaluated physically by volume fraction and density measurements. Fiber volume fraction (Vf) and void volume fraction (Vv) calculated using eq. (1) and eq. (2) as per ASTM D-3171 based on bamboo petung fibers and epoxy densities. We measured composite density by pycnometry method. (π€π ⁄ππ ) ππ (%) = [ ] π₯ 100% (π€π ⁄ππ ) + (π€π ⁄ππ ) .......... (1) ππ£ (%) = 1 − ππ [(π€π ⁄ππ ) + (π€π ⁄ππ )]π₯ 100% .......... (2) 2 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 where Wb, Wm, are weight fractions of bamboo fibers, epoxy matrix and ο²b, ο²m and ο²c are densities of bamboo fibers, epoxy matrix, composites, respectively. Water absorption tests were performed to the tensile specimen as per ASTM D570-98 but modified as per previous research [6]. in this study, we use water absorption by two intervals of immersion. Firstly, weighing the samples in boiling water 60 minutes for every 10 minute. Secondly, with 30 minute intervals from the minutes of 60 up to 240. The water uptake in the composites was weighted by electronic balance with accuracy 10-4. Moisture content in the composite samples then calculating by weight difference using Eq.3. ππ‘ (%) = π1 − π0 π₯ 100% π0 .......... (3) where Wt total water-absorbed in composites, W0 and W1 are composites weighs on H0 and H1 respectively. Tensile testing of composites were conducted on both H0 and H1 samples per ASTM D3039. We use Tensilon machine equipped by a 5 kN load cell to get the tensile property. Besides, SEM (Scanning Electron Microscope) analysis using JEOL GSM-636OLA type were also conducted after tensile test to evaluate fracture surface of the composites. 3. Results and discussion 3.1 Physical Properties of Petung Bamboo-Reinforced Epoxy Table 1 and Figure 1(a) and (b) show the fiber volume fraction and the void volume fraction of petung bamboo-reinforced epoxy under varying processing conditions. The fiber volume fraction was 22% up to 28% and the void volume fraction ranges from 0% to 6%. The higher pressure with uniform distribution in hot press processing method resulted in higher fiber content as shown in Figure 1(a). Alternatively, the composite fabricated by manual lay-up had a higher void content as shown in Figure 1(b). Table 1. Fiber and void volume fractions of petung bamboo fiber-reinforced epoxy Manufacture Processes LU HP Vf (%) NA A 24 22 28 28 Vv (%) NA A 1 6 1 0 Vf – fiber volume fraction, Vv – void volume fraction; NA – Non-Alkalized; A – 5% Alkalized (a) (b) 3 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 Figure 1. Fiber volume fraction, (a) and void volume fraction, (b) of composites as per manufacturing methods and alkali treatments. [LU: Hand Layup, HP: Hot Press] The high void content in composite primarily due to several factors such as air bubbles entrapped during matrix mixing and composite fabrication. The air from the process of manual lay-up, and the volatile component from the heat process due to chemical reactions [13]–[15]. The void content resulted in both of hot press and lay up methods are the same which is only 1.0%. After the alkali treatment the void content become 6% and 0% in both of the hand lay-up and hot press methods, respectively. Tightly controlled parameters in the hot press method through closed-loop system resulting in the lower void content whereas the open-loop controlled system in the hand lay-up method showed an anomaly result by increasing void content. 3.2. The Effects of Alkali Treatment on Tensile Strength and Water Uptake Table 2 shows the influence of alkali treatments (0% and 5% NaOH) on tensile strength and water absorption of petung bamboo fiber reinforced epoxy composites were varied from 79 MPa up to 126 MPa while the water absorption gain was ranged from 3 up to 8.8%. Table 2. The tensile properties and water absorption of petung bamboo fiber reinforced epoxy composites before and after alkali treatment. Manufacture Process LU HP Tensile Strength (MPa) NA A 83 79 126 126 Water absorption (%) NA A 5,15 3,79 8,82 6,57 NA – Non-Alkalized; A – 5% Alkalized Figure 2 shows that the alkali treatment effect in the hot press (HP) method did not increase the composite’s strength as stated in the literature [16]. Moreover, using lay up (LU) method, the effect of alkali treatment showed slight reduction of tensile strength due to high void content, 6% (see Table 1). The void causes stress concentrations and tend to weaken the fiber-matrix bonding [17]. The tensile strength of hot-pressed composites seem to be more dominated by high fiber volume fraction, 28%Vf, and lower void content than that of the alkali effect. 4 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 Figure 2. Tensile properties of petung bamboo fiber reinforced epoxy before and after alkali treatment as per hand layup (LU) and hot press (HP) methods. [NA: Non-Alkalized, A: 5% Alkalized] Figure 3 shows water absorption reduction after fiber alkali treatment on lay-up (LU) and hot press (HP) composites. The higher fiber volume fraction in the hot press composites lead to higher water uptake than that of the lay-up composites. This uptake was due to the inherent hygroscopic properties of bamboo fibers as lignocellulosic materials[16] which contain polar hydroxyl groups produced by both cellulose and hemicellulose content. Figure 3. Water absorption characteristics of composites based on alkali treatment. [NA: Non-Alkalized, A: 5% Alkalized] Both composites have 26% reduction of water uptake after the alkali treatment. This was due to the removal of hemicellulose and lignin content during the treatment [16]. In the previous report [10] hemicellulose was responsible for water absorption of the fibers. Alkali treatment makes the fibers less hydrophilic as the number of hydrophilic hydroxyl groups reduces by react which 5% NaOH [17], [18]. Therefore, reduction of water absorption enhanced the water resistance of composites. Besides, alkali treatment increases fiber fibrillation and therefore decreases fiber diameter, which in turn improve the effect of surface area for contact with the matrix [16]. This might be contributing to decrease water absorption due to bamboo fibers more encapsulated by the epoxy matrix. 3.3. Effect of Manufacture Process on Tensile Strength Figure 4 shows the comparison of tensile strength of composites resulting from manual lay-up (LU) and hot press (HP) processing. The highest tensile strength of composites was obtained by using hot press method. It can be seen that hot press processing has improved the tensile strength of composites up to 37%. The combination of higher fiber volume fraction and lower void content improved tensile strength, see Table 1. The higher fiber volume fraction in the hot press (HP) was achieved by homogenous temperature and steadier pressure distributions. In this method temperature and pressure are tightly controlled in closed-loop system. Conversely, processing parameters in hand lay-up (LU) controlled manually through the operator skills level which is the open-loop system. Dealing with the lower void content in the 5 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 hot pressed composite, this could be achieved due to uniformly high pressure – forced out the entrapped void – supported by the molding mechanism. Tensile Strength, MPa Layup Hot Press 140 120 100 80 60 40 20 0 Non Alkalized 5% Alkalized Alkali Treatment Figure 4. The comparison of the tensile strength by using manual lay-up (LU) and hot press (HP) processing Figure 5 shows the composites fracture surfaces resulting from both the layup and hot press processes. Lower extent of fiber pullout in HP composites (Fig. 5b) compared to LU composites confirms the improvement of fiber-matrix interface, resulting in higher tensile strength. This improvement might be resulted from the combined temperature and pressure energy supply in HP method. (b) (a) Figure 5. Comparison of the fracture surface of composites manufactured by (a) Hand Lay Up and (b) Hot Press 3.4. Effect of Water Absorption on Tensile Strength Table 3 and Figure 6 depicted the effect of water absorption on tensile strength of petung bamboo fiber-reinforced epoxy composites based on alkali treatment and manufacturing processes. The absorption of water from 3.79% up to 8.8% leads to the degradation of fibermatrix interface [18]. The result was a reduction of composites tensile strength from 17% up to 29% (see Table 3). Besides, water composites immersion swelled the hydrophilic bamboo fibers resulting in micro cracking of the brittle matrix[19]. As water, penetrating into the interface through the micro cracks fiber-matrix debonding occurs and leads to composite 6 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 failure [20]. High strength reduction on both non-alkalized composites (LU-NA and HP-NA) as high as 25% and 24% were due to high water absorption 5.15% and 8.8%, respectively. This water absorption made hydrogen bonds to the fibers and decreased fiber-matrix interconnections. Large strength reduction on the alkalized lay-up (LU-A) composites was dominated by high void content (see Fig. 1) than the water uptake in the composites. From Fig. 6 the best composite with the lowest strength reduction was resulting from alkalized hot press composites (HP-A). The composite shows only 17% tensile strength reduction, showing the effectiveness of alkalization to reduce water absorption and minimize the strength reduction. Table 3. Tensile properties decrement of Petung bamboo fiber reinforced epoxy composites due to water absorption Composite - Fiber Tensile decrements Water uptake treatments (%) (%) LU-NA 25 5.15 LU-A 29 3.79 HP-NA 24 8.8 HP-A 17 6.57 NA – Non-Alkalized; A – 5% Alkalized Figure 6. The effect of water absorption on tensile strength petung bamboo fiber reinforced epoxy composites. Supporting tensile test results, SEM qualitative evaluation were added in Fig. 7. Fracture surfaces were based on fiber treatments, manufacturing processes, and water absorption conditions. Fracture surfaces of composites after water immersion (Fig. 7b, d, f, h) show larger extent of fibers pullout that related to poor fiber-matrix interface. These results corroborate with the tensile strength reduction of composites due to water absorption. 7 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 Composites (Manufacture – Treatment) Before immersed in water (H0) After immersed in water (H1) (a) (b) (c) (d) (e) (f) (g) (h) Layup-Non Alkali [LU-NA] Layup-Alkali [LU-A] Hot Press-Non Alkali [HP-NA] Hot Press-Alkali [HP-A] 8 IC-DAEM 2018 IOP Publishing IOP Conf. Series: Materials Science and Engineering 547 (2019) 012043 doi:10.1088/1757-899X/547/1/012043 Figure 7. Comparison of composites fracture surfaces due to alkali treatment, manufacturing technique, and water absorption 4. Conclusion The effects of alkali treatment, composite manufacturing, and water absorption on the tensile strength of petung bamboo fiber-reinforced epoxy composites have been studied. In this research, the alkali treatment has less effect to the tensile strength than of the volume fraction gain and the void content. Hot press composites manufacturing method has significant effect to the improvement of tensile strength up to 37% than that of lay-up method. Water absorption up to 8.8% decreased the tensile strength of composites up to 29%. The alkali treatment had effectively reduced water absorption and consequently minimized the tensile strength decrement. 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