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A.W. van Vuure, J. Vanderbeke, L. Osorio, E. Trujillo, C. Fuentes and I. Verpoest Katholieke Universiteit Leuven, Dept. MTM Kasteelpark Arenberg 44, Box 2450, B-3001 Leuven, Belgium aartwillem.vanvuure@mtm.kuleuven.be 6800$5< Silk fibres, due to their high intrinsic strain to failure, are converted into very tough composites, by combining them with matrices of high strain to failure and by targeting intermediate interfacial strength. Bamboo fibres, when extracted carefully, can maintain a high fibre strength and be turned into strong composites with good interfacial strength.

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Commensurate with the increased worldwide interest in sustainable and renewable materials, the Composite Materials Group in Leuven is engaged in a range of projects and activities concerning natural fibres and their composites. Research is focusing on 4 themes: 1) 2) 3) 4) Understanding the mechanical properties of natural fibres and their composites Understanding and improving the fibre-matrix interface Developing environmentally friendly matrices Developing environmentally friendly processes

In this context, research has been conducted on various natural fibres: Flax and hemp (recently in cooperation with the European flax and hemp organisation CELC), coconut (with Vietnam), jute (with Bangladesh), paper honeycombs and wood-PVC compounds. This paper highlights the work on silk and bamboo. Silk fibres show an exceptionally favourable combination of decent E-modulus (about 16 GPa) and strength (about 700 MPa) with a high strain to failure (around 20%). This means that silk fibre composites can combine good structural performance, with a high impact resistance as was reported previously [1,2,3]. This paper further highlights the good impact resistance as a function of matrix and interface properties and aims to summarise the mechanisms at work. Bamboo fibres have the potential to replace glass fibres, due to their high modulus (over 40 GPa) and good strength (up to 800 MPa), which means that their specific mechanical properties are comparable to glass fibre. This paper highlights the properties of Columbian bamboo fibres, which were obtained by a newly developed extraction process.

0$7(5,$/6 $1' 0(7+2'6 The silk fabric used in this work, was sourced from France. A balanced, degummed twill (2/2) weave fabric was used, with low yarn twist and an areal weight of 78 g/m2. A range of thermoplastic films was obtained from various suppliers in film thicknesses UDQJLQJ IURP  WR  P 'LIIHUHQW FKHPLFDO FRPSRVLWLRQV DQG D UDQJH RI VWUDLQ WR failures were selected. The epoxy used was a standard novolac resin from M.C. Technics, processed into resin infusion film. Balanced satin weave aramid fabrics of 170 g/m2 for reference testing were obtained from Teijin Twaron. Bamboo fibres of the species Guadua Angustifolia were obtained from well defined locations in Columbia. A newly developed and proprietary extraction process was used to obtain technical fibres from the culm. Long fibres with an average diameter of 150 P ZHUH VHOHFWHG 8' FRPSRVLWHV ZHUH SUHSDUHG E\ PDQXDOO\ DOLJQLQJ DQG FRPELQJ WKH fibres and fixing their ends by glue before composite preparation. As a reference, some bamboo fibres of the Dendrocalamus membranaceus species from Vietnam were tested, SURGXFHG E\ VWHDP H[SORVLRQ $YHUDJH ILEUH GLDPHWHU ZDV  P Some bamboo fibres were treated by NaOH at different concentrations (0%, 1%, 3% and 5%) for 20 minutes at room temperature, after which they were washed and neutralized thoroughly and then dried. Both silk and bamboo epoxy composites were prepared by resin film infusion and cured at 125C. Thermoplastic silk composites were prepared by compression moulding of stacks of silk fabrics and thermoplastic films. To obtain good impregnation the temperature used was about 25 degrees C higher than the melting temperature of the polymer and a pressure of 15 bars was used. In all cases, the natural fibres were dried overnight at 50C to prevent problems due to moisture. Fibre volume fraction was targeted at 50%. Tensile tests were performed according to ASTM D-3039 on an Instron testing machine, using an extensometer. Falling weight impact tests were performed on an impact rig according to ISO 6603-2. A hemispherical striker tip with radius 8 mm was used and samples of 100 x 100 mm were clamped by a support ring with a free surface of 80 mm diameter. The result reported is the impact energy needed for penetration, normalized to the thickness of the composite plate (about 1 mm thickness). Single fibre tensile tests were performed on a mini tensile testing machine with a loadcell of 200N. Single fibres were prepared with paper end-tabs to prevent slippage and damage to the fibres. No extensometer could be used, so the machine displacement was used. The test gage was 25 mm. Interface strength was estimated by transverse 3 point bending tests on UD samples and samples were tested according to ASTM D-790. Also, some longitudinal bending tests were performed according to the latter standard. 5(68/76 $1' ',6&866,21  6,/. ),%5( &20326,7(6 As mentioned, silk fibres show an exceptionally favourable combination of decent Emodulus and a high strain to failure. In this way silk fabrics show a high penetration impact resistance. This impact resistance can be enhanced further by creating silk fibre composites with tough thermoplastic matrices, as illustrated in figure 1, where balanced silk woven fabrics have been evaluated (see also [2,3]). Surrounded by a tough matrix,

the silk fabrics can shear extensively and the fibres can stretch substantially before penetration occurs.

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Figure 1 Penetration impact resistance for silk twill (2/2) weave fabric composites as a function of matrix strain to failure, with the effect of interfacial adhesion illustrated; also dry silk fabric was evaluated. (IIHFW RI LQWHUIDFH VWUHQJWK The other important parameter determining the impact resistance is the fibre-matrix interfacial adhesion strength, as also illustrated in figure 1. The interfacial adhesion was measured by transverse 3 point bending tests on UD composites in only a limited number of cases. For the rest it was determined qualitatively by observing fracture surfaces (pull-out length of 0 fibres and polymer patches on 90 fibres in the woven composite), by observing the 45 tensile yield stress and the bending yield stress (with higher yield stress in case of better adhesion). Too high adhesion typically reduces impact resistance, as localisation of damage occurs. For brittle matrices this is totally detrimental as illustrated by the case of epoxy resin. Hydrophobic PLA though has very limited adhesion to silk and the performance of an un-impregnated silk fabric is recovered. For tougher matrices the reduction in impact resistance is much more modest. Reference tests were conducted on aramid fabric composites. Results are shown in figure 2, for a range of polymers with relatively high strains to failure. Dry aramid fabric has a very high impact resistance, which decreases rapidly when incorporated into a composite, depending on the level of interfacial wetting and adhesion. When incorporated into well adhering polyamide matrices, very little impact resistance is maintained.

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Some tests were conducted on aramid fabric composites, by keeping the polymer chemistry the same, but by varying the polymer strain to failure. A very limited effect was observed, showing that for aramid fibres, with a strain to failure of a few percent, the extra benefit of an increase in matrix strain to failure, is soon not apparent anymore.

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Figure 2 Penetration impact resistance for aramid satin weave fabric composites with various matrices, leading to different levels of interfacial adhesion. Current further research is focusing on quantifying interfacial strength by micromechanical testing and on understanding (and controlling) adhesion by measuring (and manipulating) fibre and matrix surface tensions, where it is understood highest physical adhesion will be obtained by high polarity matching of the ingredients. The Owens Wendt approach is adopted, where both the disperse and polar components of the surface tensions of the ingredients are matched. A more simplified approach is to measure the ingredients contact angle with water, to obtain a measure of hydrophilicity and then to match the hydrophilicity of the ingredients. 2WKHU SDUDPHWHUV DIIHFWLQJ LPSDFW UHVLVWDQFH As reported before [3] the other parameters strongly affecting impact resistance, are the degree of balance of the fabric used and yarn twist. In unbalanced fabrics, damage will progress quickly in the weakest fabric direction, whereas in a balanced fabric, cracks have to grow in both fabric directions. In quasi-isotropic lay-ups the impact resistance is reduced, probably because of the mismatch in deformation between 0/90 orientated fabrics and 45 orientated layers. Yarn twist is detrimental for strength and thus for impact resistance.

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%$0%22 ),%5( &20326,7(6 A new (proprietary) mechanical process has been developed for the extraction of technical bamboo fibre from the stem, causing very limited fibre damage. This has resulted in high strength fibres as illustrated in figure 3.

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Figure 3 Average technical bamboo fibre strength obtained in various extraction processes. After extraction, the fraction of long fibres (with the length of the internode distance) was selected for analysis and composite manufacture. Single fibre tensile tests were performed on a span of 25 mm, giving an average E-modulus of 38 GPa and an average fibre strength of 740 MPa, which is quite high compared to literature values. With a density of bamboo fibre of 1.4, specific mechanical properties are very close to these of glass fibre. Uni-directional bamboo-epoxy composites were prepared by resin film infusion and flexural tests were performed. Both longitudinal composite flexural modulus and flexural strength followed simple composite mechanics (rule of mixtures). The flexural modulus was actually higher than anticipated and when the E-modulus of the fibres was back calculated from these results a fibre modulus of 42 GPa was obtained. The lower value for the directly measured modulus can be attributed to the fact that no extensometer was used in the single fibre testing. Recently, a procedure has been adapted where single fibre properties are measured on a range of test spans [4]. When E-modulus is plotted against 1/span and the E-modulus is extrapolated to 1/span = 0, or in other words to infinite fibre length, effects of fibre slippage in the clamps and system compliance can be ignored. This procedure is currently applied to the Guadua Angustifolia fibres. In [4], measurements were done on bamboo fibres of the Dendrocalamus membranaceus species from Vietnam, produced by steam explosion. This resulted in an average strength of 640 MPa at a test span of 25 mm and an extrapolated E-modulus of 34 GPa.

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,QWHUIDFLDO VWUHQJWK The extracted Guadua Angustifolia bamboo fibres appear to have a good adhesion to epoxy resin, as determined by transverse 3-point bending. This means that no additional fibre surface treatment or matrix modification is necessary in this case. High composite longitudinal bending strength is measured, close to the predictions from composite mechanics. It was evaluated if the adhesion could be further improved by applying an alkali treatment. Results for the transverse 3 point bending strength are shown in figure 4.

Figure 4 Effect of bamboo treatment in alkali on the transverse 3 point bending strength of bamboo-epoxy composites. It is shown that some further improvement in adhesion strength is possible, but this did actually lead to reduction in composite longitudinal strength, so was not deemed very useful. The transverse flexural strength of 33 MPa for untreated bamboo in epoxy is high. This is illustrated in figure 5, where this result is compared to some previous results on flax-epoxy composites [5]. Further research is aiming at quantifying the surface properties of untreated and treated bamboo fibres. Surface tension analysis is conducted, as in the case of silk fibres. Bamboo fibres will have to be compatibilised with a range of matrix polymers of interest. First results on the extracted bamboo fibres show that these have a contact angle of approximately 70 with water, which means that the surface is not particularly hydrophilic, respectively polar. This could mean that there is scope for further improvement in the adhesion with relatively polar epoxy resin. It is hypothesised that part of the good adhesion between the extracted bamboo and epoxy resin is due to mechanical interlocking due to surface roughness.

Figure 5 Benchmarking of the interfacial adhesion strength for untreated bamboo-epoxy composites against untreated and treated flax fibre epoxy composites [5] &21&/86,216 Tough silk fibres can be turned into tough silk composites, by incorporating the silk fibres in thermoplastic matrices, with a high strain to failure and with a rather modest adhesion strength to the silk fibres. The adhesion effect needs to be further quantified by physical chemical and micromechanical characterisation. Furthermore, the use of balanced fibre architectures and low fibre twist was previously seen to be beneficial for impact resistance. Results on aramid fabric composites show that in this case, with a much lower fibre strain to failure, the main effect is from the fibre-matrix adhesion, with best impact results for poor wetting and adhesion (due to the very high impact resistance of dry aramid fabrics). Technical bamboo fibre is difficult to extract undamaged from the culm, but once a good extraction process is used, as developed at KU Leuven, fibres are obtained with specific mechanical properties comparable to glass fibre. Untreated bamboo appeared to have a high adhesion strength to epoxy resin, taking away the necessity to do any treatment. Further work aims at quantifying adhesion aspects. $&.12:/('*(0(176 The research on bamboo fibres is sponsored by the Belgian Science Policy Office, in a cooperative project with Vietnam.

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5HIHUHQFHV 1. A.W. van Vuure, K. Wolnik, S. Dupont, J. Vanderbeke, N. El-Asmar, I. Verpoest, Silk Fibre Composites, Proc. European SAMPE Symposium, March 2006, Paris, 6p. Aart W. van Vuure, Jan Vanderbeke, Nedda El-Asmar, Ignaas Verpoest, Silk Fibre Composites, Proc. 16th ICCM, Kyoto, July 2007, 5p. Jan Vanderbeke, Aart Willem van Vuure and Ignaas Verpoest, Designing natural silk fibre reinforced thermoplastic composites as tough composite materials against low velocity impact, Proc. European SAMPE Symposium, March 2008, Paris, 6p. Nele Defoirdt, Subhankar Biswas, Linde De Vrieze, Le Quan Ngoc Tran, Qumrul Ahsan, Aart van Vuure and Ignaas Verpoest, Assessment of the tensile properties of coir, bamboo and jute fibre, submitted to Composites, Part A. Isabel Van de Weyenberg, Flax Fibres as a reinforcement for epoxy composites, PhD thesis KU Leuven, December 2005.

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