Biocomposites Reinforced With Natural Fibers

Progress in Polymer Science 37 (2012) 15521596
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Progress in Polymer Science

journal homepage: www.elsevier.com/locate/ppolysci
Biocomposites reinforced with natural bers: 20002010

Omar Faruk a,d, , Andrzej K. Bledzki a,c , Hans-Peter Fink b , Mohini Sain d
a b c d
Institut fr Werkstofftechnik, Kunststoff- und Recyclingtechnik, University of Kassel, Moenchebergstrasse 3, D-34109 Kassel, Germany Fraunhofer Institute for Applied Polymer Research, Geiselbergstrasse 69, D-14476 Potsdam-Golm, Germany West Pomeranian University of Technology, Institute of Material Science and Engineering, 19 Piastow Ave, 70310 Szczecin, Poland Centre for Biocomposites and Biomaterials Processing, University of Toronto, 33 Willcocks Street, Toronto, ON M5S3B3, Canada
a r t i c l e
i n f o
a b s t r a c t
Due to environment and sustainability issues, this century has witnessed remarkable achievements in green technology in the eld of materials science through the development of biocomposites. The development of high-performance materials made from natural resources is increasing worldwide. The greatest challenge in working with natural ber reinforced plastic composites is their large variation in properties and characteristics. A biocomposites properties are inuenced by a number of variables, including the ber type, environmental conditions (where the plant bers are sourced), processing methods, and any modication of the ber. It is also known that recently there has been a surge of interest in the industrial applications of composites containing biobers reinforced with biopolymers. Biopolymers have seen a tremendous increase in use as a matrix for biober reinforced composites. A comprehensive review of literature (from 2000 to 2010) on the mostly readily utilized natural bers and biopolymers is presented in this paper. The overall characteristics of reinforcing bers used in biocomposites, including source, type, structure, composition, as well as mechanical properties, will be reviewed. Moreover, the modication methods; physical (corona and plasma treatment) and chemical (silane, alkaline, acetylation, maleated coupling, and enzyme treatment) will be discussed. The most popular matrices in biober reinforced composites based on petrochemical and renewable resources will also be addressed. The wide variety of biocomposite processing techniques as well as the factors (moisture content, ber type and content, coupling agents and their inuence on composites properties) affecting these processes will be discussed. Prior to the processing of biocomposites, semi-nished product manufacturing is also vital, which will be illustrated. Processing technologies for biober reinforced composites will be discussed based on thermoplastic matrices (compression molding, extrusion, injection molding, LFT-D-method, and thermoforming), and thermosets (resin transfer molding, sheet molding compound). Other implemented processes, i.e., thermoset compression molding and pultrusion and their inuence on mechanical performance (tensile, exural and impact properties) will also be evaluated. Finally, the review will conclude with recent developments and future trends of biocomposites as well as key issues that need to be addressed and resolved. Crown Copyright 2012 Published by Elsevier Ltd. All rights reserved.
Article history: Received 3 August 2011 Received in revised form 19 April 2012 Accepted 25 April 2012 Available online 2 May 2012 Keywords: Biocomposites Natural ber Biopolymer Nanober Acetylation Alkylation Silane Maleated coupling Enzyme treatment Thermoplastic Thermosets Injection molding Compression molding Extrusion Pultrusion Resin transfer molding Sheet molding compound LFT-D method Tensile Flexural Impact
Corresponding author at: Centre for Biocomposites and Biomaterials Processing, University of Toronto, 33 Willcocks Street, Toronto, ON M5S3B3, Canada. Tel.: +1 416 9781615; fax: +1 416 9783834. E-mail address: o.faruk@utoronto.ca (O. Faruk). 0079-6700/$ see front matter. Crown Copyright 2012 Published by Elsevier Ltd. All rights reserved. http://dx.doi.org/10.1016/j.progpolymsci.2012.04.003
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Contents 1. 2. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1554 Reinforcing bers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1554 2.1. Fiber source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1554 2.2. Fiber types . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1554 2.2.1. Flax . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1554 2.2.2. Hemp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1555 2.2.3. Jute . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1555 2.2.4. Kenaf . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1556 2.2.5. Sisal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1556 2.2.6. Abaca . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1557 2.2.7. Pineapple leaf ber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1558 2.2.8. Ramie . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1558 2.2.9. Coir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1558 2.2.10. Bamboo . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1558 2.2.11. Rice husk . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1559 2.2.12. Oil palm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1559 2.2.13. Bagasse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1559 2.3. Structure and chemical composition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1559 2.4. Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1560 2.5. Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1562 Modication of natural bers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1562 3.1. Physical method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1562 3.1.1. Corona treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1562 3.1.2. Plasma treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1562 3.2. Chemical method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1563 3.2.1. Silane treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1563 3.2.2. Alkaline treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1564 3.2.3. Acetylation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1565 3.2.4. Maleated coupling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1565 3.2.5. Enzyme treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1567 3.3. Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1567 Matrices for biocomposites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1567 4.1. Petrochemical based . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1567 4.1.1. Thermoplastic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1568 4.1.2. Thermosets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1571 4.2. Bio-based . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1571 4.2.1. PLA (polylactide acid) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1571 4.2.2. PHB (polyhydroxybutyrate) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1572 4.2.3. Starch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 4.2.4. Others . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 4.3. Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 Processing techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 5.1. Factors inuencing processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 5.1.1. Moisture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1574 5.1.2. Fiber type and content . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1575 5.1.3. Inuence on composites properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1575 5.2. Semi-nished product manufacturing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1576 5.3. Processing technologies for natural ber reinforced thermoplastics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1576 5.3.1. Compression molding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1576 5.3.2. Extrusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1576 5.3.3. Injection molding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1576 5.3.4. Long ber thermoplastic-direct (LFT-D) method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1577 5.4. Processing technologies for natural ber reinforced thermosets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1578 5.4.1. Resin transfer molding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1578 5.4.2. Sheet molding compound . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1578 5.5. Other processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1579 5.5.1. Thermosets compression molding . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1579 5.5.2. Pultrusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1579 5.5.3. Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1579 Performance of biocomposites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1580 6.1. Tensile properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1580 6.2. Flexural properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1581 6.3. Impact properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1581
3.
4.
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6.
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7. 8.
6.4. Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1582 Development and future trends of biocomposites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1582 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1584 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1584
2. Reinforcing bers 1. Introduction There is a growing trend to use biobers as llers and/or reinforcers in plastics composites. Their exibility during processing, highly specic stiffness, and low cost (on a volumetric basis) make them attractive to manufacturers. This century has witnessed ever-increasing demands for the utilization of plastics as important raw materials, more than 80% of which are thermoplastics. Biober reinforced plastic composites are gaining more and more acceptance in structural applications. Technological development connected with consumer demands and expectations continues to increase demands on global resources, leading to major issues of material availability and environmental sustainability. Over the last few decades biober composites have been undergoing a remarkable transformation. These materials have become more and more sufcient as new compositions and processes have been intensively researched, developed and consequently applied. The petroleum crisis made biocomposites signicantly important and biocomposites have become engineering materials with a very wide range of properties. However, like all materials, they are constantly under competitive pressure from the global market, which in turn, necessitates continuous research. The times of simply mixing plastics with natural waste llers and characterizing their main properties are gone. The concept of using bio-based plastics as reinforced matrices for biocomposites is gaining more and more approval day by day. The developments in emerging biobased plastics are spectacular from a technological point of view and mirror their rapid growth in the market place. The average annual growth rate globally was 38% from 2003 to 2007. In the same period, the annual growth rate was as high as 48% in Europe. The worldwide capacity of bio-based plastics is expected to increase from 0.36 million metric ton (2007) to 2.33 million metric ton by 2013 and to 3.45 million metric ton in 2020. The main product in terms of production volumes will be starch-based plastics, PLA and PHA [1]. The increasing number of publications during the recent years including reviews [29] and books [1014] reect the growing importance of these new biocomposites. Bledzki and Gassan have reviewed the reinforcement of the most readily used natural bers in polymer composites up until 1999 in their review paper [15]. This paper aims to review more current reinforcement of natural bers in polymer composites from 2000 to 2010. This paper will not address natural bers from animals (e.g., silk or wool) or cotton or man-made cellulosic bers. This review also excludes wood ber or our. Given the broadscope of this article, it will inevitably be incomplete, but will hopefully provide a sensible overview of the most popular natural bers in polymeric composite materials in the last 11 years. An increased awareness that non-renewable resources are becoming scarce and our inevitable dependence on renewable resources has arisen. This century could be called the cellulosic century, because more and more renewable plant resources for products are being discovered. It has been generally stated that natural bers are renewable and sustainable, but they are in fact, neither. The living plants are renewable and sustainable from which the natural bers are taken, but not the bers themselves. 2.1. Fiber source The plants, which produce natural bers, are classied as primary and secondary depending on their utilization. Primary plants are those grown for their ber content while secondary plants are plants in which the bers are produced as a by-product. Jute, hemp, kenaf, and sisal are examples of primary plants. Pineapple, oil palm and coir are examples of secondary plants. Table 1 shows the main bers used commercially in composites, which are now produced throughout the world [16]. 2.2. Fiber types There are six basic types of natural bers. They are classied as follows: bast bers (jute, ax, hemp, ramie and kenaf), leaf bers (abaca, sisal and pineapple), seed bers (coir, cotton and kapok), core bers (kenaf, hemp and jute), grass and reed bers (wheat, corn and rice) and all other types (wood and roots). 2.2.1. Flax Flax, Linum usitatissimum, belongs to the bast bers. It is grown in temperate regions and is one of the oldest ber crops in the world. The bast ber ax is most frequently used in the higher value-added textile markets. Nowadays, it is widely used in the composites area. The static and dynamic mechanical properties of nonwoven based ax ber reinforced PP composites were
Table 1 Commercially major ber sources. Fiber source Bamboo Jute Kenaf Flax Sisal Hemp Coir Ramie Abaca Sugar cane bagasse Grass World production (103 ton) 30,000 2300 970 830 378 214 100 100 70 75,000 700
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studied considering the effect of zein coupling agent [17]. Zein is a protein, extracted from corn and used as solution. Composites containing zein coupling agent were found to possess improved mechanical properties. The storage modulus of composites was found to increase with zein coupling agent coating due to enhanced interfacial adhesion. The tensile mechanical properties of ax bers are estimated according to their diameter and their location in the stems [18]. The large scattering of these properties is ascribed to the variation of the ber size along its longitudinal axis. The higher values of the mechanical properties of the bers issued from the middle of the stems are associated with the chemical composition of their cell walls. The mechanical properties of unidirectional ax ber/epoxy matrix composites are studied as a function of their ber content. The properties of the composites are lower than those expected from single ber characteristics. Various investigations of ax ber/polypropylene composites have been completed. These studies focus on many different variables, including: comparison between NMT (natural ber thermoplastic mat) and GMT (glass ber thermoplastic mat) [19], the inuence of ber/matrix modication and glass ber hybridization [20], the effect of ber treatment on thermal and crystallization properties [21], the inuence of surface treatment on interface by glycerol triacetate, thermoplastic starch, -methacryl oxypropyl trimethoxy-silane and boiled ax yarn [22], comparison of matrices (PP and PLA) on the composite properties [23], the effects of material and processing parameters [24], and the inuence of processing methods [25]. Buttler [26] presented the feasibility of using ax ber composites in the coachwork and bus industry. The effect of bio-technical ber modication [27], fracture behavior and toughness [28], the inuence of alkaline ber treatment on unidirectional composites [29], the effect of processing parameters [30] on the consecutive decortication stages of ax bers (retting, scutching, and hackling) on the ax ber reinforced epoxy composites have also been evaluated. Flax ber composites reinforced with polyester resin have been evaluated for thermal degradation and re resistance [31], chemical treatments on surface properties and adhesion [32], and the effect of chemical treatments on water absorption and mechanical properties [33]. Three resins from soybean oil (methacrylated soybean oil, methacrylic anhydride modied soybean oil, and acetic anhydride modied soybean oil) were used also as matrices for ax ber reinforced biocomposites [34]. 2.2.2. Hemp Another notable bast ber crop is hemp, which belongs to the Cannabis family. It is an annual plant that grows in temperate climates. Hemp is currently the subject of a European Union subsidy for non-food agriculture, and a considerable initiative in currently underway for their further development in Europe. Composites of PP with hemp bers, which were functionalized by means of melt grafting reactions with glycidyl methacrylate (GMA) and prepared by batch mixing, were examined [35]. The modication of bers and the PP matrix,
as well as the addition of various compatibilizers were carried out to improve the bermatrix interactions. Compared to the unmodied system, a modied composite showed improved ber dispersion in the PP matrix and higher interfacial adhesion as a consequence of chemical bonding between the ber and the polymer (PP/Hemp). The thermal stability and phase behavior of the composites was largely affected by the ber and matrix modication. Changes in the spherulithic morphology and crystallization behavior of PP were observed in the composites due to the nucleating effect of the hemp bers. Moreover, a marked increase in the PP isothermal crystallization rate (in the range 120138 C) was recorded with increasing content of modied hemp. All composites displayed a higher tensile modulus (about 2.9 GPa) and lower elongation at break as compared to plain PP; compatibilization with modied PP (10 phr) resulted in an increased stiffness of the composites as a result of improved bermatrix interfacial adhesion. Pickering and co-workers [3638] investigated the effects of chelator, white rot fungi, and enzyme treatments on the separation of hemp bers from bundles, and the improvement of the interfacial bonding of the hemp bers with the PP matrix. The obtained results showed that the interfacial shear strength of the treated ber composites was higher than that for untreated ber composites. This veries that the hemp ber interfacial bonding with PP was improved by the white rot fungi treatment. Composites consisting of hemp bers treated with chelator concentrate had the highest tensile strength of 42 MPa, which equals an increase of 19% compared to composites with untreated hemp ber. Hemp ber reinforced PP composites exhibited interesting recyclability [39]. The obtained results prove that the mechanical properties of hemp ber/PP composites remain well preserved, despite the number of reprocessing cycles. The Newtonian viscosity decreases with cycles, indicating a decrease in molecular weight and chain scissions induced by reprocessing. The decrease of ber length with reprocessing could be another reason for decrease of viscosity. Epoxy resins, which were used as a matrix for hemp ber reinforced composites, were studied regarding the effect of ber architecture on the falling weight impact properties [40], properties and performances of composites for curved pipes [41], impact load performance of resin transfer molded composites [42], micro-mechanics of the composites [43], the inuence of hybrid blends made of soybean oil and nanoclay [44], and the usefulness of unretted hemp as a source of ber for biocomposites [45]. Kunanopparat et al. [46,47] studied the feasibility of wheat gluten as a matrix for hemp ber reinforced composites regarding their thermal treatment and plasticization effect on the mechanical properties. 2.2.3. Jute Jute is produced from plants of the genus Corchorus, which includes about 100 species. It is one of the cheapest natural bers and is currently the bast ber with the highest production volume. Bangladesh, India and China provide the best condition for the growth of jute. Ray and co-workers [4850] extensively investigated alkali treated jute ber reinforced with vinyl ester resin.
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In their studies, they regarded the dynamic, mechanical, thermal, and impact fatigue behavior compared to that of untreated jute bervinyl ester composites. Longer alkali treatment removed the hemicelluloses and improved the crystallinity, enabling better ber dispersion. The dynamic, mechanical, thermal and impact properties were superior owing to the alkali treatment, comprising treatment time, concentration and conditions. Mohanty et al. [51] investigated effects and inuence of surface modication on the mechanical and biodegradability of jute/Biopol and jute/PA (Poly Amide) composites. Enhancements in tensile strength of more than 50%, 30% in bending strength and 90% in impact strength were observed in the composites and are comparative to values achieved for pure Biopol sheets. Degradation studies showed that after 150 days of compost burial more than 50% weight loss of the jute/Biopol composites occurs. The effects of hybridization [52] on the tensile properties of jutecotton woven fabric reinforced polyester composites were investigated as functions of the ber content, orientation and roving texture. It was observed that tensile properties along the direction of jute roving alignment (transverse to cotton roving alignment) increase steadily with ber content up to 50% and then show a tendency to decrease. The tensile strength of composites with 50% ber content parallel to the jute roving is about 220% higher than pure polyester resin. Jute ber reinforced PP composites were evaluated regarding the effect of matrix modication [53], the inuence of gamma radiation [54], the effect of interfacial adhesion on creep and dynamic mechanical behavior [55], the inuence of silane coupling agent [56,57], and the effect of natural rubber [58]. The properties of jute/plastic composites were studied, including the thermal stability, crystallinity, modication, trans-esterication, weathering, durability, ber orientation on frictional and wear behavior, eco-design of automotive components, and alkylation [5966]. Polyester resin was used as matrix for jute ber reinforced composites and the relationship between water absorption and dielectric behavior [67], the elastic properties, notched strength and fracture criteria [68], impact damage characterization [69], weathering and thermal behavior [70], and effect of silane treatment [71] were examined. 2.2.4. Kenaf Kenafbelongs to the genus Hibiscus and there are about 300 species. Kenaf is a new crop in the United States and shows good potential as a raw material for usage in composite products. Latest advances in decortications equipment which separates the core from the bast ber combined with ber shortages, have renewed the interest in kenaf as a ber source. Thermoforming has proven to enable the successful fabrication of kenaf ber reinforced PP sheets into sheet form [72]. The optimal fabrication method found for these materials was at the compression molding process, which utilizes a layered sifting of a micro-ne PP powder and chopped kenaf bers. The ber content (30 and 40 wt%) provided adequate reinforcement to increase the strength
of the PP matrix. The kenafPP composites compression molded in this study proved to have superior tensile and exural strength when compared to other compression molded natural ber composites such as other kenaf, sisal, and coir reinforced thermoplastics. With the aid of the elastic modulus data, it was also possible to compare the economic benets of using kenaf composites instead of other natural bers and E-glass. The manufactured kenafmaleated PP composites have a higher modulus/cost and a higher specic modulus than sisal, coir, and even E-glass. Thus, they provide an option for replacing existing materials with a higher strength, lower cost alternative that is environmentally friendly. Hybrid composites of wood our/kenaf ber and PP were prepared to investigate the hybrid effect on the composite properties [73]. The results indicated that while non-hybrid composites of kenaf ber and wood our exhibited the highest and lowest modulus values respectively, the moduli of hybrid composites were closely related to the ber to particle ratio of the reinforcements. With the help of the hybrid mixtures equation it was possible to predict the elastic modulus of the composites better than when using the HalpinTsai equation. Variations of the mechanical and thermal properties induced by the exposure of kenaf ber reinforced composites with PP to electron beam radiation [74], the comparison of kenaf/PP composites with feather ber/PP, recycled kraft pulp ber/PP, and recycled news pulp ber/PP composites [75] and, surface modied kenaf bers with modied polyester resin as matrix [76], and inuence of toughening by natural rubber on kenaf bers with polyester resin as matrix [77] were also evaluated.
2.2.5. Sisal Sisal is an agave (Agave sisalana) and commercially produced in Brazil and East Africa. Between 19982000 and 2010, the global demand for sisal ber and its products is expected to decline by an annual rate of 2.3% as agricultural twine. The traditional market for bers continues to be eroded by synthetic substitutes and by the adoption of harvesting technologies that utilizes less or no twine. Magnesium hydroxide and zinc borate were incorporated into sisal/PP composites as ame retardants [78]. Adding ame retardants into sisal/PP composites reduced the burning rate and increased the thermal stability of the composites. No synergistic effect was observed when both magnesium hydroxide and zinc borate were incorporated into the sisal/PP composites. In addition, the sisal/PP composites exhibited insignicant differences in shear viscosity at high shear rates indicating that the types of ame retardants used in this study had no impact on the processability of the composites. The sisal/PP composites which ame retardants were added to, exhibited tensile and exural properties comparable to those of the sisal/PP composites, which ame retardants had not been added to. Sisal /PP composites were investigated regarding the environmental effects on the degradation behavior [79], the inuence of coupling agents on the abrasive wear
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properties [80], and the effect of ageing on the mechanical properties [81]. Zhang et al. [82] developed all plant ber composites by converting wood our into thermoplastics using an appropriate benzylation treatment and compounding both discontinuous and continuous sisal bers to produce composites from renewable resources. The degradation tests demonstrated that the prepared sisal/plasticized wood our composites were fully biodegradable. To accelerate the decomposition process, both cellulose and lignin in the composites should be considered. The hydrophobicity and ame resistance of composites is important when regarding practical applications. Molecular modication and/or incorporation of inorganic additives are proper measures provided that the composites biodegradability remains unchanged. Many other studies were carried out on sisal ber reinforced polyester composites regarding their moistureabsorption properties [83], and ber treatment with admicellar [84]. Sisal ber reinforced phenolic resin composites were investigated with regard to the chemical modication of such with lignins [85], the modication using hydroxy terminated polybutadiene rubber [86], the effect of cure cycles [87], using glyoxal from natural resources [88], and the effect of alkali treatment [89]. Furthermore epoxy resin was used as a matrix for sisal ber reinforced composites and examined regarding the inuence of ber orientation on the electrical properties [90], and the degree of reinforcement [91]. Investigations were also carried out using cement as a matrix for sisal ber reinforced composites focusing on their cracking micro-mechanisms [92], and the effects of accelerated carbonation on cementitious roong [93]. Towo et al. [94,95] prepared the treated sisal ber composites with an epoxy and polyester resin matrix. Fatigue evaluation and dynamic thermal analysis tests were performed. Composites containing alkali treated ber bundles proved to have better mechanical properties than those with untreated ber bundles. Alkali treatment had the greatest effect on the polyester resin matrices. An improvement in the fatigue lives of composites was observed for the alkali treatment of sisal ber bundles. Constant-life diagrams of epoxy matrix composites with untreated or alkali treated ber bundles show the superiority of the alkali treated ber composites regarding low cycle fatigue. Epoxy matrix composites have a longer fatigue life than polyester matrix composites. The effect of chemical treatment on the fatigue life is signicantly positive for polyester matrix composites but has much less inuence on the fatigue life of epoxy matrix composites. Sisal bers were also investigated with other matrices, such as rubber [96,97], phenol formaldehyde [98], cellulose acetate [99], bio polyurethane [100], and polyethylene [101] regarding their mechanical, morphological, chemical, and Cure characteristics. 2.2.6. Abaca The abaca/banana ber, which comes from the banana plant, is durable and resistant to seawater. Abaca, the strongest of the commercially available cellulose bers, is indigenous to the Philippines and is currently produced
6 5
5mm 5mm+MAH-PP
Notched charpy impact strength [mJ/mm]
4 3 2 1 0 Abaca-PP Flax-PP Jute-PP
Fig. 1. Comparison of notch Charpy strength of abaca/jute/ax berPP composites with and without MAHPP. Adopted from [103]. Copyright 2007. By permission from Budapest University of Technology.
there and in Ecuador. It was once the preferred cordage ber for marine applications. Bledzki et al. [102,103] examined the mechanical properties of abaca ber reinforced PP composites regarding different ber lengths (5, 25 and 40 mm) and different compounding processes (mixer-injection molding, mixercompression molding and direct compression molding process). It was observed that, with increasing ber length (540 mm), the tensile and exural properties showed an increasing tendency though not a signicant one. Among the three different compounding processes compared, the mixer-injection molding process displayed a better mechanical performance (tensile strength is around 90% higher) than the other processes. When abaca ber PP composites were compared with jute and ax ber PP composites, abaca ber composites had the best notched Charpy (Fig. 1) and falling weight impact properties. Abaca ber composites also showed higher odor concentration (Fig. 2) compared to jute and ax ber composites. A dynamic mechanical analysis of, polarity parameters of banana ber reinforced polyester composites were carried out by Thomas and co-workers [104,105] with special reference to the effects of ber loading, frequency and temperature. The storage modulus was found to be highest for composites with 40% ber loading, indicating
Fig. 2. Comparison of odor emission concentration abaca/jute/ax berPP composites. Adopted from [103]. Copyright 2007. By permission from Budapest University of Technology.
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that the incorporation of abaca ber in the polyester matrix induces reinforcing effects at higher temperatures. Increased dynamic modulus values and low damping values veried improved interactions between the ber and the matrix. Abaca bers have been investigated with cement [106], polyurethane [107], aliphatic polyester resin [108], PP [109], urea formaldehyde [110], PE [111], polyester [112], and polyvinyl alcohol [113] as matrices, in order to evaluate the composites properties. 2.2.7. Pineapple leaf ber Pineapple (Ananas comosus) is a tropical plant native to Brazil. Pineapple leaf ber is rich in cellulose, relatively inexpensive and abundantly available. Furthermore, it has the potential for polymer reinforcement. At present pineapple leaf bers are a waste product of pineapple cultivation and therefore these relatively inexpensive pineapple ber can be obtained for industrial purposes. Pineapple leaf ber was reinforced with polycarbonate to produce functional composites [114]. The silane treated modied pineapple leaf bers composite exhibited the highest tensile and impact strengths. The thermogravimetric analysis showed that the thermal stability of the composites is lower than that of neat polycarbonate resin. In addition, the thermal stability decreased with increasing pineapple leaf ber content. The thermal conductivity and thermal diffusivity of pineapple leaf ber reinforced phenol formaldehyde composites were studied using the Transient Plane Source (TPS) technique [115]. It is found that the effective thermal conductivity and effective thermal diffusivity of the composites decrease, as compared with pure phenol formaldehyde as the fraction of ber loading increases. The quality enhancement of pineapple leaf ber has been attempted using different surface modications like dewaxing, alkali treatment, cyanoethylation and grafting acrylonitrile onto dewaxed bers [116]. The mechanical properties reach an optimum at ber load of 30 wt% and among all modications, 10% acrylonitrile grafted ber reinforced polyester composite exhibited the maximum tensile strength (48.36 MPa). However, cyano-ethylated ber composites exhibited better exural and impact strengths, i.e., 41% and 27% more than the detergent washed composite respectively. The inuence of surface treatment and ber content of pineapple leaf ber was also investigated with PP [117] and natural rubber as matrix [118]. 2.2.8. Ramie Ramie belongs to the family Urticaceae (Boehmeria), which includes about 100 species. Ramies popularity as a textile ber has been limited largely by regions of production and a chemical composition that has required more extensive pre-treatment than is required of the other commercially important bast bers. Ramie ber reinforced PP composites were fabricated using a hybrid method of melt-blending and injection molding processes [119]. Different ramie ber/PP composites were fabricated by varying the ber length, ber content and method of ber pre-treatment. The results
exhibited increases in ber length and ber content also show increased tensile strength, exural strength and compression strength noticeably in turn. Yet, they also result in negative inuences on the impact strength and elongation behavior of the composites. Thermoplastic biodegradable composites consisting of ramie bers and a PLA/PCL matrix were manufactured using the in situ polymerization method [120]. The effects of ber length and content on the tensile and impact strengths of this natural-ber-reinforced biodegradable composite were discussed, including the inuence of a silane coupling agent for improved interfacial adhesion. The results showed that the tensile strength and impact strength were highest when a silane coupling agent was employed, the ramie ber length was 56 mm and when the ber content was 45 wt%. Bulletproof panels were made from ramie ber reinforced composites by hand lay-up process with epoxy as a matrix [121]. These prototype bulletproof panels were believed to be lighter in weight and more economical than conventional bulletproof panels. Conventional bulletproof panels are made from ceramic plates, kevlar/aramid composites, and steel-based material, which are popular in military standard antiballistic equipment today. The bullet testing results showed that the panels could resist the penetration of a high-impact projectile (level II) obtaining only minimal fractures. Level IV ballistic testing showed that all prototype panels could not resist the high-impact velocity of the projectile. Therefore, tests proved that ramie bers have sufcient breaking strength and toughness for level II bullet testing. Ramie bers were also reinforced using polyester [122,123], epoxybioresin [124], soy protein [125,126], epoxy [127] and PP [128] for the matrix. 2.2.9. Coir Coir husk bers are located between the husk and the outer shell of the coconut. As a by-product of the production of other coconut products, coir production is largely determined by demand. Abundant quantities of coconut husk imply that, given the availability of labor and other inputs, coir producers can adjust relatively rapidly to market conditions and prices. It is estimated that approximately 10% of all husks are utilized for ber extraction, satisfying a growing demand for ber and coir products. Characterization and utilization of coir ber in coir /natural rubber composites [129], dynamic mechanical behavior of coir/natural rubber composites [130], durability of coir/cement composites [131], the effect acetylation on the coir/epoxy composites [132], the inuence of treated coir ber on the physico-mechanical properties of coir/PP composites [133,134], and the effect of ber physical, chemical and surface properties on the thermal and mechanical properties of coir/PP composites were investigated and evaluated [135]. 2.2.10. Bamboo Bamboo (Bambusa Shreb.) is a perennial plant, which grows up to 40 m in height in monsoon climates. Generally, it is used in construction, carpentry, weaving and plaiting etc. Curtains made of bamboo ber can absorb ultraviolet
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radiation in various wavelengths, making it less harmful to human body. The development of composites for ecological purposes (eco-composites) using bamboo bers and their basic mechanical properties were evaluated [136]. The steam explosion technique was applied to extract bamboo bers from raw bamboo trees. The experimental results showed that the bamboo bers (bundles) had a sufcient specic strength, equivalent to that of conventional glass bers. The tensile strength and modulus of PP based composites increased about 15 and 30% when using steam-exploded bers. This increase was due to good impregnation and a reduction of the number of voids, in comparison to composites using bers that were mechanically extracted. The mechanical and thermal properties of bamboo ber reinforced epoxy composites [137], the effects of ber loading, coupling and bonding agents on the mechanical properties of bamboo ber/natural rubber composites [138,139], the isothermal crystallization kinetics of modied bamboo cellulose/PCL composites [140], the inuence of environmental aging on the mechanical properties of bamboo/glass ber reinforced PP hybrid composites [141], and the effect of ceramic llers on mechanical properties of bamboo ber/epoxy composites [142] were evaluated. 2.2.11. Rice husk Rice is only one of the large group of cereal grains that can be used to produce hull bers. Nowadays wheat, corn, rye, oats and other cereal crops are used to produce bers and investigating to reinforce in composites area. Ismail et al. [143147] studied the mechanical properties of rice husk lled polymer composites and their relation to ber loading, coupling agent, processability, hygrothermal aging, and hybridization effect. Other studies have focused on: ame retardant properties of rice husk/PE composites [148], the using of rice husk as ller for rice husk/PP composites [149], the thermogravimetric analysis of rice husk lled HDPE and PP composites [150], the enhancement of the processability of rice husk/HDPE composites [151], the effect of the percentage of rice husk content, hydroxyl groups and size on the exural, tensile, and impact properties of rice husk/polyurethane composites [152], nonlinear viscoelastic creep characterization of HDPE-rice husk composites [153], the effect of the rice husk size and composition on the injection molding processability of rice husk/PE composites [154], photocatalytic performance of a carbon/TiO2 composite with rice husk [155], the effect of different concentrations and sizes of particles of rice husk ash-in the mechanical properties of rice husk/PP composites [156], the effect of different coupling agent on rice husk/copolymer PP composites [157], dimensional properties of rice husk/unsaturated polyester composites [158], and carbon/silica composites fabricated from rice husk by means of binder-less hot-pressing [159]. 2.2.12. Oil palm Oil palms (Elaeis) comprise two species of the Arecaceae or palm family. Nowadays, oil palm empty fruit bunch bers possess potential as a reinforcement ber for plastic. Thomas et al. [160,161] investigated the stress relaxation
behavior of phenol formaldehyde resins reinforced with oil palm empty fruit bunch bers and hybrid composites composed of oil palm bers and glass bers. The effects of ber loading, ber treatment, physical ageing and strain level on the stress relaxation behavior were examined and the rate of relaxation at different time intervals was calculated in order to explain gradual changes in relaxation mechanisms. Abu Baker et al. [162,163] investigated the effect of oil palm empty fruit bunch and acrylic impact modier on mechanical properties and inuence of oil extraction of oil palm empty fruit bunch on the processability of PVC composites. The effects of oil extraction, compounding techniques and ber loading [164], and the effect of matrix modication [165] on the mechanical properties of oil palm empty fruit bunch lled PP composites were examined. In addition, a comparative study of oil palm empty fruit bunch ber/PP composites and oil palm derived cellulose/PP composites [166] were studied. The inuence of chemical modication on oil palm/phenol formaldehyde composites [167], a comparison of epoxy and polyester matrixes reinforced with oil palm bers [168], dielectric relaxation properties of oil palm/polyester resin composites [169], the effect of palm tree ber orientation on dynamic electrical properties of palm tree ber-reinforced polyester composites [170] have also been investigated. 2.2.13. Bagasse Bagasse is the brous residue which remains after sugarcane stalks are crushed to extract their juice. It is currently used as a renewable natural ber for the manufacture of composites materials. The compression and injection molding processes were performed in order to evaluate which is the better mixing method for bers (sugarcane bagasse, bagasse cellulose and benzylated bagasse) and PP matrixes [171]. The injection molding process performed under vacuum proved to work best. Composites were obtained with a homogeneous distribution of bers and without blisters. Although, the composites did not have good adhesion between the ber and the matrix according to their mechanical properties. The effect of botanical components of bagasse on the setting of bagasse/cement composites [172], design and optimization of PHB/bagasse ber composites [173], tribological properties of bagasse/polyester composites [174], creep properties of bagasse ber reinforced PVC and HDPE composites [175], bagasse/HDPE composites for radiation shielding [176], molecular mobility information of bagasse ber and their distribution in bagasse/EVA composites [177], silane treated bagasse ber reinforcement for cementitious composites [178], using polyurethane from castor oil [179], durability of bagasse/PP composites exposed to rainbow fungus [180], and ecodesign and life cycle assessment as strategy for automotive components from bagasse/PP composites [181] were examined. 2.3. Structure and chemical composition Climatic conditions, age and the degradation process inuence not only the structure of bers, but also the chemical composition. The major chemical component of a living
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Table 2 Chemical composition of some common natural bers. Fiber Bagasse Bamboo Flax Kenaf Jute Hemp Ramie Abaca Sisal Coir Oil palm Pineapple Curaua Wheat straw Rice husk Rice straw Cellulose (wt%) 55.2 2643 71 72 6171 68 68.676.2 5663 65 3243 65 81 73.6 3845 3545 4157 Hemicellulose (wt%) 16.8 30 18.620.6 20.3 1420 15 1316 2025 12 0.150.25 9.9 1531 1925 33 Lignin (wt%) 25.3 2131 2.2 9 1213 10 0.60.7 79 9.9 4045 29 12.7 7.5 1220 20 819 Waxes (wt%) 1.5 0.5 0.8 0.3 3 2 1417 838
tree is water. However, on dry basis, all plant cell walls consist mainly of sugar based polymers (cellulose, hemicellulose) that are combined with lignin with lesser amount of extractives, protein, starch and inorganics. The chemical components are distributed throughout the cell wall, which is composed of primary and secondary wall layers. The chemical composition varies from plant to plant, and within different parts of the same plant. Table 2 [182184] shows the range of the average chemical constituents for a wide variety of plant types. 2.4. Properties The properties of natural bers differ among cited works, because different bers were used, different moisture conditions were present, and different testing methods were employed. The natural ber reinforced polymer composites performance depends on several factors, including bers chemical composition, cell dimensions, microbrillar angle, defects, structure, physical properties, and mechanical properties, and also the interaction of a ber with the polymer. In order to expand the use of natural bers for composites and improved their performance, it is essential to know the ber characteristics. The range of the characteristic values, as one of the drawbacks for all natural products, is remarkably higher than those of glass-bers, which can be explained by
Table 3 Physico-mechanical properties of natural bers. Fiber Abaca Bagasse Bamboo Flax Hemp Jute Kenaf Sisal Ramie Oil palm Pineapple Coir Curaua Tensile strength (MPa) 400 290 140230 3451035 690 393773 930 511635 560 248 400627 175 5001150
differences in the ber structure due to the overall environment conditions during growth. Natural bers can be processed in different ways to yield reinforcing elements with different mechanical properties. Mechanical properties of natural bers can be inuenced by many factors. Such as either ber bundles or ultimate ber is being tested. Table 3 [182,183] presents the important physicomechanical properties of commonly used natural bers. The hydrophilic nature of bers is a major problem for all cellulose-bers if used as reinforcement in plastics. The moisture content of the bers is dependent on the content of non-crystalline parts and the void content of the bers. Overall, the hydrophilic nature of natural bers inuences the mechanical properties. Table 4 [185] shows the equilibrium moisture content of some natural bers. The moisture content at a given relative humidity can have a great effect on the biological performance of a composite made from natural bers. For example, a composite made from abaca bers would have much greater moisture content than would a composite made from ax bers. The physical properties of each natural ber are critical, and include the ber dimensions, defects, strength and structure. There are several physical properties that are important to know about for each natural ber before that ber can be used to reach its highest potential. Fiber dimensions, defects, strength, variability, crystallinity, and structure must be taken into consideration.
Youngs modulus (GPa) 12 17 1117 27.6 70 26.5 53 9.422 24.5 3.2 1.44 46 11.8
Elongation at break (%) 310 2.73.2 1.6 1.51.8 1.6 2.02.5 2.5 25 14.5 30 3.74.3
Density [g/cm3 ] 1.5 1.25 0.61.1 1.5 1.48 1.3 1.5 1.5 0.71.55 0.81.6 1.2 1.4
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Fig. 3. Illustration of a single ber cell. Adopted from [186] Copyright 2001. By permission from Springer Publishing.
Knowledge about ber length and width is important for comparing different kinds of natural bers. A high aspect ratio (length/width) is very important in cellulose based ber composites as it give an indication of possible strength properties. The ber strength can be an important factor in selecting a specic natural ber for a specic application. Changes in the physical properties can be due to differences in ber morphology. Major differences in structure such as density, cell wall thickness, length and diameter result in differences in physical properties. It is also interesting to note that the morphology of the land plant bers is very from different to that of water plant bers. In between ber qualities, the cellulose content and spiral angle is differed from ber to ber and also in a single ber design. Natural ber is a composite of the three polymers (cellulose, hemicelluloses and lignin), in which the unidirectional cellulose microbrils constitute the reinforcing elements in the matrix blend of hemicellulose and lignin. The structure of such a ber was built as multiply construction with layers P, S1, S2 and S3 of cellulose microbrils at different angles to the ber axis (Fig. 3) [186]. Depending on the single ber cell layer, the different spiral angle of those layers will have a pronounced inuence on the properties of the ber. The elastic modulus dependency on the spiral angle of the ber is determined
Table 4 The equilibrium moisture content of different natural bers at 65% relative humidity (RH) and 21 C. Fiber Sisal Hemp Jute Flax Abaca Ramie Pineapple Coir Bagasse Bamboo Equilibrium moisture content (%) 11 9.0 12 7 15 9 13 10 8.8 8.9
(Fig. 4) assuming that the bers (holocellulose bers) were lignin-free with a cellulose content of 65 wt% (which is typical cellulose content for natural bers [186]). The relative thickness of the different layers were chosen to be P = 8%, S1 = 8%, S2 = 76%, and S3 = 8%. It is seen that the elastic modulus decreases with increasing spiral angle. Crystallinity values of natural bers vary in different parts of the plant. The crystallinity tends to decrease as the plant matures, but the difference between bast and core bers is inconclusive. The permeability of kenaf core is highest and is closely followed by cotton. The effect of transcrystallinity on the interface in ax ber (green ax, dew-retted ax, Duralin-treated ax and stearic acid-treated ax ber)/isotactic PP composites has been investigated [187,188]. A signicant strengthening of the interface was observed when transcrystallinity was present. Surface modication (stearation) of ax ber also induced transcrystallinity. The interfacial shear strength increased from 12.75 MPa for the samples without transcrystallinity to 23.05 MPa for the transcrystallized samples according to the single ber fragmentation test.
Fig. 4. Correlation between spiral angle and elastic modulus of a natural ber. Adopted from [186]. Copyright 2001. By permission from Springer Publishing.
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The chemical composition varies from plant to plant, and within different parts of the same plant. It also varies within plants from different geographical regions, ages, climate and soil conditions. The chemical properties are inuenced by the ber growth time (days after planting), the botanical classication of the ber and the stalk height. The chemical composition can also vary within the same part of a plant. Both the root and stalk core have a higher lignin content than that of the bers. 2.5. Summary There are thousands of different bers in the world and in fact only few of these bers have been studied. Most research has been carried out to study the potential use of natural bers for technical applications and this review paper has only covered the most widely studied and used natural bers in reinforced composites materials. Among the most popular natural bers; ax, jute, hemp, sisal, ramie, and kenaf bers were extensively researched and employed in different applications. But nowadays, abaca, pineapple leaf, coir, oil palm, bagasse, and rice husk bers are gaining interest and importance in both research and applications due to their specic properties and availability. It should be mentioned that there are also shortcomings; a lack of consistency of ber qualities, high levels of variability in ber properties related to the location and time of harvest, processing conditions, as well as their sensitivity to temperature, moisture and UV radiation. A multi-step manufacturing process is required in order to produce high quality natural bers, which contributes to the cost of high-performance natural bers as well as the improved mechanical properties of the composites. 3. Modication of natural bers The main disadvantages of natural bers in reinforcement to composites are the poor compatibility between ber and matrix and their relative high moisture absorption. Therefore, natural ber modications are considered in modifying the ber surface properties to improve their adhesion with different matrices. An exemplary strength and stiffness could be achieved with a strong interface that is very brittle in nature with easy crack propagation through the matrix and ber. The efciency of stress transfer from the matrix to the ber could be reduced with a weaker interface. 3.1. Physical method Physical methods include stretching, calendaring, thermotreatment, and the production of hybrid yarns for the modication of natural bers. Physical treatments change structural and surface properties of the ber and thereby inuence the mechanical bonding of polymers. Physical treatments do not extensively change the chemical composition of the bers. Therefore the interface is generally enhanced via an increased mechanical bonding between the ber and the matrix.
3.1.1. Corona treatment Corona treatment is one of the most interesting techniques for surface oxidation activation. This process changes the surface energy of the cellulose bers. Corona discharge treatment on cellulose ber and hydrophobic matrix was found to be effective for the improvement of the compatibilization between hydrophilic bers and a hydrophobic matrix. Tossa jute bers [189] were corona discharge treated to improve the mechanical properties of natural ber/epoxy composites. Corona-treated bers exhibited signicantly higher polar components of free surface energy with increasing treatment energy output. Owing to difculties in effective treatment of three-dimensional objects with corona discharge, the increased polarity of treated yarns is relatively small. Furthermore a decrease in the yarn tenacity was observed with an increasing corona energy level. The mechanical properties of corona treated hemp ber/PP composites were characterized by tensile and compressive stressstrain measurements [190]. The treatment of compounds (bers or matrix) leads to a signicant increase in tensile strength. The modication of cellulosic reinforcements rather than PP matrix allows greater improvement of the composites properties with an enhancement of 30% of Young modulus. The observation of the fracture surfaces enables discussion about adhesion improvement. Flax and Hemp ber mats were corona treated and the optimum length of corona treatment to improve the composites (with a natural resin matrix) tensile modulus and strength was determined [191]. The composite tensile breaking strength reaches a maximum earlier, namely after only 5 min of corona treatment and declines rapidly afterwards. The ber appearance conrmed that relatively short periods of corona treatment are more than sufcient to improve adhesion in the bers. In addition, it was also proven that there is no further improvement achieved when longer corona treatments are applied, because the surface opening of the ber does not improve further after 15 min of treatment. However, the degradation of the bers proceeds further.
3.1.2. Plasma treatment Plasma treatment is another physical treatment method and is, similar to corona treatment. The property of plasma is exploited by the method to induce changes on the surface of a material. A variety of surface modications can be achieved depending on the type and nature of the gases used. Reactive free radicals and groups can be produced, the surface energy can be increased or decreased and surface cross-linking can be introduced. Polyester composites reinforced with ax bers, which were submitted to helium cold plasma treatment, were investigated by means of water permeation measurements and mechanical tests [192]. The analysis of the permeation and mechanical results showed that plasma treatment improves the ber/matrix adhesion and enhances the mechanical property stiffness. Martin et al. [193] prepared sisalHDPE composites and showed that some improvements of the mechanical
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properties of the composites are achieved due to the plasma treatments. Jute bers were subjected to oxygen plasma treatment as a function of the plasma power in order to enhance interfacial adhesion [194]. The interlaminar shear strength of plasma treated jute ber/HDPE composites, which were exposed to plasma powers of 30 W and 60 W, increased by approximately 32 and 47%, respectively compared to untreated composites. In turn, the exural strength of untreated composites increases by only 45%. It can be concluded that exposure to plasma powers of 60 W for 15 min in the studied range is the most suitable parameter for oxygen plasma treatment of jute bers and enables the achievement of the best interfacial adhesion with HDPE. The inuence of plasma treatment on the morphology, wettability, and ne structure of jute bers and its impact on the interfacial adhesion of jute bers/unsaturated polyester were investigated [195]. A scanning electron microscopic micrograph showed the rough surface morphology and degradation of ber due to an etching mechanism caused by the plasma. Plasma treatment resulted in the development of hydrophobicity in bers. However, among all treated ber composites, the exural strength of composites prepared with bers treated for 10 min with plasma only showed an improved mechanical strength of approximately 14% in comparison to raw ber composites. Jute bers were treated indifferent plasma reactors (radio frequency RF and low frequency LF plasma reactors) using O2 for different plasmapowers to increase the interface adhesion between the jute ber and polyester matrix. The interlaminar shear strength increased from 11.5 MPa for the untreated jute ber/polyester composite to 19.8 and 26.3 MPa for LF and RF oxygen plasma treated jute ber/polyester composites, respectively. The tensile and exural strengths improved of jute ber/polyester composites for both plasma systems. It is clear that oxygen plasma treatment of jute bers by using RF plasma system showed greater improvement on the mechanical properties of jute/polyester composites compared to using LF plasma system [196].
Chemical modications of natural bers aimed at improving the adhesion within the polymer matrix using different chemicals were investigated.
3.2. Chemical method Cellulose bers, which are strongly polarized, are inherently incompatible with hydrophobic polymers due to their hydrophilic nature. In many cases, it is possible to induce compatibility in two incompatible materials by introducing a third material that has properties intermediate between those of the other two. There are several coupling mechanisms in materials (e.g., weak boundary layers, deformable layers, restrained layers, wettability, chemical bonding, and acidbase effect). The development of a denite theory for the mechanism of bonding using coupling agents in composites is a complex problem. The main chemical bonding theory alone is not sufcient. So the consideration of other concepts appears to be necessary. These include the morphology of the interphase, the acidbase reactions in the interface, surface energy and the wetting phenomena.
3.2.1. Silane treatment The surface energy of bers is closely related to the hydrophilic nature of the ber. Some investigations are concerned with methods to decrease hydrophilicity. Silane coupling agents may contribute hydrophilic properties to the interface, especially when amino-functional silanes, such as epoxies and urethanes silanes, are used as primers for reactive polymers. The primer may supply much more amine functionality than can possibly react with the resin in the interphase. Those amines, which could not react, are hydrophilic and therefore responsible for the poor water resistance of bonds. An effective way to use hydrophilic silanes is to blend them with hydrophobic silanes such as pheniltrimethoxysilane. Mixed siloxane primers also have an improved thermal stability, which is typical for aromatic silicones. The surface of the kenaf ber was modied using a silane coupling agent to promote adhesion with the PS matrix [197]. The bermatrix adhesion increased through a condensation reaction between alkoxysilane and hydroxyl groups of kenaf cellulose. Due to the ber modication, kenaf/PS composites exhibited higher storage modulus and lower tan than those with untreated ber indicating a greater interfacial interaction between the matrix resin and the ber. Silane treatment improved the storage modulus of abaca ber reinforced polyester composites [198]. Chemical modications with silane A174 (-methacryl oxypropyl trimethoxy-silane) and also with NaOH resulted in maximum increase of the modulus. The hydrogen-bond donating acidity is found to be the lowest for bers treated with silane A174, after pre-treatment with 0.5% NaOH. On the contrary, the highest value was noted for bers treated with silane A151 (vinyl triethoxysilane). The overall polarity was found to be at a maximum for bers treated with silane A151 (vinyl triethoxysilane). The effects of different chemical treatments on the bermatrix compatibility in terms of the surface energy and the mechanical properties of composites were reported [199]. The composites were compounded with two kinds of ax bers (natural ax and ax pulp) and a PP matrix. The applied treatments were vinyl trimethoxy silane (VTMO), maleic anhydride (MA) and maleic anhydride-polypropylene copolymer (MAPP). The three treatments reduced the polar component of the surface energy of the ber. Composites containing MAPPtreated bers possessed the highest mechanical properties, while the MA and VTMO-treated bers obtained similar values to those of the untreated ones. Ismail et al. [200,201] treated oil palm empty fruit bunch and coir bers with silane coupling agents and found that with the addition of silane, the scorch time and cure time increased. Furthermore, the tensile strength, tensile modulus, tear strength, fatigue life and hardness of oil palm empty fruit bunch and coir ber reinforced polyester and natural rubber composites were enhanced.
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Table 5 Variation of the structure and properties of hemp Yarn (hemp 10/1, Rohemp) due to mercerization (22% NaOH). Mercerization temperature time ( C) Untreated 4 10 20 10 10 60 60 60 40 60 Mercerization (min) Stress at the mercerization Isometric Isometric Isometric Free shrinkage Constant load (100 g) Degree of conversion cell I in cell II (%) 50 50 50 70 40 Tensile strength (cN/tex) 29.8 28.5 24.9 28.2 17.6 29.2 Elongation at break (%) 3.15 2.34 2.45 2.27 6.86 2.60 Tension modulus (cN/tex) 1148 1617 1214 1701 357 1499
Note: Distance of clamped support = 500 mm, test speed = 250 mm/min.
3.2.2. Alkaline treatment Alkaline treatment or mercerization is one of the most used chemical method (removes a certain amount of lignin, wax and oils covering the external surface of the ber cell wall) for natural bers when used to reinforce thermoplastics and thermosets. The important modication achieved with alkaline treatment is the disruption of the hydrogen bonding in the network structure, thereby increasing the surface roughness. The effect of alkali treatment on the wetting ability and coherence of sisalepoxy composites has been examined [202]. Treatment of sisal ber in a 0.5 N solution of sodium hydroxide resulted in more rigid composites with lower porosity and higher density. The treatment improved the adhesion characteristics, due to improved work of adhesion because it increases the surface tension and surface roughness. The resulting composites showed improvements in the compressive strength and water resistance. It was also discovered that the removal of intracrystalline and intercrystalline lignin and other waxy surface substances by the alkali substantially increases the possibility for mechanical interlocking and chemical bonding. The effects of alkali treatment of pineapple leaf ber on the performance of the pineapple leaf ber/PLA composites have been shown [203]. It was found that alkali-treated ber reinforced composite offered superior mechanical properties compared to untreated ber reinforced composites. This study also suggested that the appropriate modication of ber surfaces signicantly contributes to improving the interfacial properties of the biocomposites. Since improvement of the interfacial adhesion increases the impact performance, surface properties of bers can be greatly modied in terms of different treatments as characterized by an increased surface energy, which improves wettability of the ber when compounding with a PLA matrix. DMA showed that treated ber composites have a higher storage modulus, which indicates greater interfacial bond strength and adhesion between the matrix resin and the ber. The alkalized ber composites have high storage modulus values, which correspond with their high exural modulus. The effect of alkylation on the tensile properties of ramie ber was explored [204]. The load application technique was employed during alkali treatment, in order to improve the mechanical properties of the ber. The ramie ber was alkali-treated with a solution containing 15% NaOH and was subjected to applied loads of 0.049 and 0.098 N. The results showed that the tensile strength of the treated ramie ber was by improved 418% more than for
untreated ramie bers. The treated bers Youngs modulus decreased. It should be noted that fracture strains of the treated ramie ber drastically increased to 0.0450.072. That equals twice to three times higher than those of the untreated ramie ber. It was considered that such property improvements upon alkylation were correlated with a change of the morphological and chemical structures in microbrils of the ber. Jute bers were subjected to alkali treatment with a solution containing 5% NaOH for 0, 2, 4, 6 and 8 h at 30 C [205]. The modulus of the jute bers improved by 12%, 68% and 79% after 4, 6 and 8 h of treatment, respectively. The tenacity of the bers improved by 46% after 6 and 8 h treatment and the percentage of breaking strain was reduced by 23% after 8 h treatment. For 35% of the composites with ber treated for 4 h, the exural strength improved by 20% from 199.1 to 238.9 MPa. The exural modulus improved by 23% from 11.89 to 14.69 GPa and the laminar shear strength increased by 19% from 0.238 to 0.283 MPa. Ramie ber [206], green coconut ber [207], sisal [208], jute [209] and coir [210] bers were alkalized and their properties evaluated. The variation of mechanical and structural properties of hemp yarn upon alkylation in dissimilar conditions was investigated [211]. Alkylation with a rather high alkali concentration (22%) never led to a complete lattice conversion of cellulose I in cellulose II (Table 5). As expected, the highest degree of conversion (70%) was reached by a freely shrinking yarn. Further, the alkylation of hemp yarn under isometric conditions or with constant ber load (100 p) at a NaOH concentration of 22% results in a crystalline lattice conversion of only 4050%. However, this occurs only when combined with the highest strengths and moduli of the ber bundles. It was also observed that only the tensile modulus of elasticity exceeds the value of the original unmodied material.
Table 6 Inuence of different ber treatments on exural strength of unidirectional axPP composites. Fiber treatment Untreated Mercerizeda MAHPPb Mercerized + MAHPP Note: Lengthwise, ber content: 36 vol%. a 29% NaOH at 20 C, 20 min, isometric. b 1% Licomont AR 504 in toluene, 10 min. Flexural strength (N/mm2 ) 77 115 127 149
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Fig. 5. Inuence of acetylation of ax ber on the degree of polymerization and degree of crystallinity of cellulose. Adopted from [212]. Copyright 2008. By permission from Budapest University of Technology.
Fig. 6. Inuence of acetylation of ax bers on the moisture absorption property at 95% relative humidity. Adopted from [212]. Copyright 2008. By permission from Budapest University of Technology.
Table 6 [211] explicitly shows that, besides the significant effects of single alkylation and MAHPP treatments, a combination of the isometric alkylation procedure (e.g., increasing ber strength) and coupling agents results in the highest increase of the composite properties (90%) in comparison to a composite with untreated ax bers for reinforcement. 3.2.3. Acetylation Acetylation is another method of modifying the surface of natural bers and making them more hydrophobic. It describes the introduction of an acetyl functional group into an organic compound. The main idea of acetylation is to coat the OH groups of bers which are responsible for their hydrophilic character with molecules that have a more hydrophobic nature. The inuence of acetylation on the structure and properties of ax bers were investigated. Modied ax ber reinforced PP composites were also prepared [212]. The effect of acetylation on the degree of polymerization and crystallinity of ax ber is illustrated in Fig. 5. It was observed that the degree of polymerization slowly decreased while the degree of acetylation increased until 18%. Once reaching an acetyl content of 18% acetyl content, the degree of polymerization decreased rapidly due to vigorous degradation of cellulose. It was also notable that the degree of crystallinity increased a little bit regarding the degree of acetylation, because of the removal of lignin and extractibles. After that, the degree of crystallinity of the cellulose decreased with respect to the degree of acetylation owing to the decomposition of acetylated amorphous components on the cellulose surface. The inuences of the degree of acetylation of ax bers on the moisture absorption properties are illustrated in Fig. 6 [212]. At 95% RH, the 3.6%, 12%, 18% and 34% degree of acetylated ax bers showed about 14%, 18%, 27% and 42% lower moisture absorption properties than untreated ax ber respectively. The moisture absorption properties decreased proportionally with the increase of acetyl content of bers due to the reduction of hydrophilicity of the bers. Seena et al. investigated the effect of acetylation on abaca ber reinforced phenol formaldehyde composites and reported that the tensile strength, tensile modulus and
impact strength were found to improve compared to nontreated abaca ber composites [213]. Tserki and co-workers [214] investigated the acetylation of ax, hemp and wood bers. A removal of the non-crystalline constituents of the bers, an alteration of the characteristics of the surface topography, a change of the ber surface free energy and an improvement of the stress transfer efciency in the interface took place. The effects of acetylation on the biological degradation and shear strength of coir and oil palm ber reinforced polyester composites were evaluated [215,216]. It was reported that acetylated natural ber reinforced polyester composites exhibit higher bio-resistance and less tensile strength loss compared to composites with silane treated ber in biological tests. Zafeiropoulos and co-workers extensively investigated the inuence of acetylation on the engineering and characterization of the interface in ax ber/PP composites [217,218]. Furthermore, they also investigated the application of Weibull statistics [219] and Gaussian statistics [220] to the tensile strength of ax bers. 3.2.4. Maleated coupling Nowadays, maleated coupling is widely used to strengthen natural ber reinforced composites. The fundamental difference with other chemical treatments is that maleic anhydride is not only used to modify ber surface but also the polymeric matrix to achieve better interfacial bonding in between ber and matrix and improved mechanical properties in composites. There are numerous published studies in which the effect of maleic anhydride grafting on the mechanical properties of natural bers has been investigated and it is impossible to list all of them here. Hence, only a few representative studies are discussed here. Mohanty et al. [221] used MAPP as a coupling agent for the surface modication of jute bers. It was found that a ber loading of 30% with a MAPP concentration of 0.5% in toluene and 5 min of impregnation time with 6 mm average ber lengths resulted in the best possible outcomes. An increase in exural strength of 72.3% was observed for the treated composites. In addition to the PP matrix, Mishra et al. [222] reported that maleic anhydride treatment reduced the water absorption to a great extent in abaca, hemp and sisal ber-reinforced novolac composites. Mechanical properties like Youngs modulus,
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Fig. 7. Micrograph of abaca ber surface morphology (a) unmodied (b) NDS modied (c) fungamix modied. Adopted from [233]. Copyright 2010. By permission from Elsevier Ltd.
exural modulus, hardness and impact strength of plant ber-reinforced composites increased after maleic anhydride treatment. The effects of MAHPP coupling agents on rice-husk our reinforced PP composites were evaluated [223]. The tensile strengths of the composites decreased as the ller loading increased, but the tensile properties were signicantly improved with the addition of the coupling agent. Both the notched and unnotched Izod impact strengths remained almost the same with the addition of coupling agents. A morphological study revealed the positive effect of a compatibilizing agent on interfacial bonding. Abaca ber reinforced composites based on HDPE/Nylon-6 blends were prepared [224]. Maleic anhydride grafted styrene/ethylenebutylene/styrene triblock polymers (SEBS-g-MA) and maleic anhydride grafted polyethylene (PE-g-MA) were used to enhance the impact performance and interfacial bonding between the abaca bers and the resins. By employing SEBS-g-MA, better strengths and moduli were obtained for HDPE/Nylon-6 based composites than for corresponding HDPE based composites. It was found that the addition of SEBS-g-MA had a positive inuence on the reinforcing effect of the Nylon-6 component in the composites. Thermal analysis results showed that fractionated crystallization of the
Nylon-6 component in the composites was induced by the addition of both SEBS-g-MA and PE-g-MA. The thermal stability of both composite systems differed slightly, except for an additional decomposition peak, which is related to the minor Nylon-6 for the composites from the HDPE/Nylon-6 blends. In combination with SEBS-g-MA, the addition of Nylon-6 and the increased ber loading level led to an increase in the water absorption value of the composites. The inuence of MAHPP on the bermatrix adhesion in jute ber-reinforced PP composites and on the material behavior under fatigue and impact loadings was investigated [225]. The bermatrix adhesion was improved by treating the bers surface with the coupling agent MAHPP. It was shown that a strong interface is connected with a higher dynamic modulus and reduction in stiffness degradation with increasing load cycles and applied maximum stresses. The specic damping capacity resulted in higher values for the composites with poor bonded bers. Furthermore, the stronger bermatrix adhesion reduced the loss-energy for non-penetration impact tested composites about roughly 30%. Tests, which were performed at different temperatures, showed higher loss energies for cold and warm test conditions compared to those carried out at room temperature. The post-impact dynamic
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to improve by 40%. Enzymatic treatment was also investigated with hemp ber [234,235], and ax bers [236]. 3.3. Summary Though natural ber reinforced composites have developed signicantly over the past few years because of their low cost, low relative density, and high specic strength, the interfacial adhesion between ber and matrix is still an issue. Extensive research was carried out and reported in literature and reviewed in this paper, showing the importance of the interface and the inuence of various types of surface modications on the physical and mechanical properties of biocomposites. The observed trend lied with the chemical modication compared to physical modication. It has also been shown that maleated and silane treatment is becoming a choice method due to benecial results. Additive suppliers improved the additives with higher amounts of anhydride functional groups than previous grades (used in 1980s and 1990s), which create more sites for chemical links, resulting in signicant performance improvement at low additive contents. Using coupling agents reduced the water absorption of the composites but has not resulted in decreased long term performance. As described above that enzyme technology to modify the natural ber surface, is increasing substantially due to environment friendly. In addition, enzyme technology could be cost effective, improved product quality compared to mostly use maleated and silane modication. 4. Matrices for biocomposites The composites shape, surface appearance, environmental tolerance and overall durability are dominated by the matrix while the brous reinforcement carries most of the structural loads, thus providing macroscopic stiffness and strength. The polymer market is dominated by commodity plastics with 80% consuming materials based on non-renewable petroleum resources. Governments, companies and scientists are driven to nd an alternative matrix to the conventional petroleum based matrix through public awareness of the environment, climate change and limited fossil fuel resources. Therefore biobased plastics, which consist of renewable resources, have experienced a renaissance in the past few decades. Fig. 9 shows that the matrices currently used in bio ber composites depend on biobased or petroleum based plastics and also on their biodegradability. 4.1. Petrochemical based The effects of the incorporation of natural bers in petrochemical based thermoplastics and thermoset matrixes were extensively studied. Polypropylene (PP), polyethylene (PE), polystyrene (PS), and PVC (polyvinyl chloride) were used for the thermoplastic matrixes. Polyester, epoxy resin, phenol formaldehyde, and vinyl esters were used for the thermoset matrices and are reportedly the most widely used matrices for natural ber reinforced polymer composites.
Fig. 8. Tensile and exural strength of enzyme treated and unmodied abacaPP composites. Adopted from [233]. Copyright 2010. By permission from Elsevier Ltd.
modulus roughly 40% after 5 impact events and was 30% lower for composites with poor and good bermatrix adhesion, respectively. The effectiveness of MAH as coupling agent has discussed also on thermal and crystallization properties of sisal ber/PP composites [226], tensile properties of hildegardia ber/PP composites [227], wetting behavior of ax ber/PP composites [228], transcrystallinity of jute ber/PP composites [229], surface properties and water uptake behavior of ax, hemp ber reinforced PP composites [230], effects of micro-sized cellulose based corn bers as reinforcement agents in PP composites [231], and dynamic mechanical properties of ax and hemp ber/PP composites [232]. 3.2.5. Enzyme treatment The use of enzyme technology is becoming increasingly substantial for the processing of natural bers. Currently, the use of enzymes in the eld of textile and natural ber modication is also rapidly increasing. A major reason for embracing this technology is the fact that the application of enzymes is environmentally friendly. The reactions catalyzed are very specic and have a focused performance [233]. Bledzki et al. [233] investigated PP composites with enzyme treated abaca bers. The surface morphologies of enzyme treated and untreated abaca bers are shown in Fig. 7. In Fig. 7a, it was observed that the untreated ber surface is rough, containing waxy and protruding parts. The surface morphology of treated bers is observed in Fig. 7b and c. If the waxy material and cuticle in the treated surface are removed, the surface becomes smoother. Fibrillation is also known to occur when the binding materials are removed from the surface of the treated bers. Fiber surface damage was also observed for naturally digested bers which occur in natural digestion systems. The effects of enzyme treatment of abaca ber on the tensile and exural strength are shown in Fig. 8. The tensile strength of enzyme treated abaca composites was found to have increased 545% due to modication. Natural digestion system (NDS) modied abaca ber composites showed little improvement in comparison to unmodied abaca ber composites. The tensile strength of fungamix modied composites increased by 45% as compared to unmodied ber composites. A conventional coupling agent (MAPP) has a positive effect on the tensile strength. It was found
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Fig. 9. Current and emerging plastics and their biodegradability. Adopted from [1].
4.1.1. Thermoplastic 4.1.1.1. PE (polyethylene). Several mechanical properties (deformation, fracture, thermal diffusivity, thermal conductivity, and specic heat) of ax ber/HDPE biocomposites were evaluated [237,238]. Strength and stiffness improvement combined with high toughness can be achieved by varying the ber volume fraction and controlling the bonding between layers of the composite. The thermal conductivity, thermal diffusivity, and specic heat of the ax/HDPE composites decreased with increasing ber content, but the thermal conductivity and thermal diffusivity did not change signicantly at temperatures in the range (170200 C) studied. The specic heat of the biocomposites increased gradually with temperature. Traditionally the mechanism of moisture absorption is dened by diffusion theory; but the relationship between the microscopic structure-innite 3D-network and the moisture absorption could not be explained. Wang et al.
[239] introduced the percolation theory and a percolation model was developed to estimate the critical accessible ber ratio; the moisture absorption and electrical conduction behavior of composites. At high ber loading when bers are highly connected, the diffusion process is the dominant mechanism; while at low ber loading close to and below the percolation threshold, the formation of a continuous network is key. Hence, percolation is the dominant mechanism. The model can be used to estimate the threshold value which can in turn be used to explain moisture absorption and electrical conduction behavior. Fig. 10 shows the increment of electrical conductivity with the increasing moisture content of the composite with 65% rice hull ber loading. The composite started showing conductivity after it absorbed approximately 50% of maximum moisture. After this, conductivity increased quickly with further moisture absorption. The pattern of the increment of electrical conductivity suggests a diffusion process of moisture absorption.
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ber content, the crystallization activation energy of the composites decreased. Similar investigations (PE as matrix) were carried out using soya powder [244], curaua [245], rape straw [246,247], hemp [248], rice straw [249], bagasse [250] rice hull bers [251] and LDPE as matrixes with wheat straw [252], abaca, bagasse and rice straw bers [253]. (polypropylene). The thermo-mechanical 4.1.1.2. PP behavior of hemp bers was studied with focus on manufacturing high performance natural ber reinforced PP composites. Hemp bers subjected to quasi-static tensile experiments and temperature-controlled harmonic tests revealed a complex behavior, involving several mechanisms [254]. The hemp ber behavior was affected by temperature and acted not only as an activation factor, but also as a degradation factor with respect to the visco-elastic properties of the bers. It was discovered that PPhemp ber composites with relatively high performance can be achieved with some specic mechanical properties. The effect of sisal ber degradation and aging on the PP/sisal ber composites was investigated. The ber mat production method allowed the bers to avoid much of the processing degradation, which is often encountered during conventional shear mixing processes [255]. The best possible mechanical properties for the sisal ber/PP composites were achieved when the ber length was greater than 10 mm and the ber mass fraction was in the range of 1535%. The aged sisal ber showed lower tenacity, breaking strength and elongation with in comparison to fresh sisal bers. On the contrary, in sisal/PP composites, aged sisal ber composites exhibited better mechanical properties than fresh sisal ber/PP composites [256]. Rana et al. [257] observed an increase in impact strength in jute ber/PP composites as a result of ber loading. It was also found that both the impact and tensile properties showed increasing trends with the addition of compatibilizers. However, the opposite was true for the exural properties. Improvements of physico-mechanical properties achieved by post-treatment [258], and the interfacial and durability evaluation [259,260] of jute ber/PP composites were studied. The environmental performance of hemp ber reinforced PP composites based on natural ber mat thermoplastic (NMT) was evaluated by quantifying carbon storage potential and CO2 emissions. The results were compared with commercially available glass ber composites [261].
Fig. 10. The moisture absorption and electrical conductivity for HDPErice hull composite with 65% ber content. Adopted from [239]. Copyright 2006. By permission from Elsevier Ltd.
The hygrothermal weathering properties of rice hull reinforced HDPE composites were studied by Wang et al. [240]. The samples (50% rice hull and 50% HDPE) absorbed 4.5% moisture after 2000 h of exposure to a relative humidity (RH) of 93% at 40 C. The walls of the samples swelled signicantly (7.1%) in thickness and ultimately developed about 5 mm of longitudinal bowing (Fig. 11) based on 61 cm long boards. Both expansion and bowing were partially recovered after another 2000 h exposure to 20% RH at 40 C. Deformation results in increased moisture contents. Temperature also played a signicant role by causing direct thermal expansion or contraction and by affecting the rate and the amount of moisture adsorption. Sisal ber reinforced PE [241] and HDPE [242,243] composites were examined regarding their interfacial properties, isothermal crystallization behavior and mechanical properties. Sisal ber treatment with stearic acid increased the interfacial shear strength by 23% compared to untreated bers in sisal/PE composites. Permanganate (KMnO4 ) and dicumyl peroxide (DCP) roughen the ber surface and introduced mechanical interlocking with the HDPE. Sisal ber reinforced HDPE shows a stable de-bonding process with Permanganate and DCP treatment. Silane treated sisal ber reinforced HDPE exhibits an unstable debonding process. A high crystallization rate and short crystallization half time were observed for sisal/HDPE composites compared to neat HDPE. This demonstrates the strong nucleating abilities of sisal bers. With increasing
Fig. 11. Partial recovery of bowing (a) before recovery: 5.00 mm of bowing (b) after recovery: 3.00 mm of bowing. Adopted from [240]. Copyright 2005. By permission from Elsevier Ltd.
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Fig. 12. CO2 emissions per ton composite and reduction in emissions by substituting glass ber with hemp bers. Adopted from [261]. Copyright 2003. By permission from Elsevier Ltd. Fig. 14. TGA curves of wheat straw bers prepared by different processes. Adopted from [262]. Copyright 2006. By permission from Elsevier Ltd.
Fig. 12 shows CO2 emissions in ton/ton of composite for both natural and glass bers. These values are estimated by converting energy into CO2 emissions using standard conversion factors for different fossil fuels. The heat energy liberated by incineration of hemp ber and PP is also added in non-renewable energy requirements to make calculations simpler. The results demonstrate a net reduction in emissions of 3 ton CO2 /ton of product if glass bers are substituted by hemp bers. The potential of wheat straw bers to be used as reinforcing additives for PP prepared with the inuence of different processes (mechanical and chemical processes) was investigated [262]. Fibers prepared by mechanical and chemical processes were characterized with respect to their chemical composition, morphology, physical, mechanical and thermal properties. The bers prepared by chemical processes exhibited better mechanical, physical and thermal properties. The morphology of the wheat straw ber surfaces processed by mechanical and chemical means is shown in
the SEM photomicrographs (Fig. 13). The surface of the chemically processed bers was more uniform and homogeneous while the bers processed mechanically exhibit more surface irregularities. Mechanically processed bers still contained the cellular residues such as lignin and hemicellulose, which cement the bers together. The inuence of chemical and mechanical processes on the TGA of the wheat straw bers is shown in Fig. 14. The onset of degradation of wheat straw bers prepared by mechanical and chemical processes were 217 C and 242 C respectively indicating the suitability of these bers for processing with thermoplastics, especially polyolens. The higher onset of degradation temperature indicates the improved thermal stability of the bers prepared by chemical processing. Similar to PE, PP is also widely used as a matrix in combination with different natural bers: such as hemp [263,264], ax [265267], kenaf [268,269], oil palm [270],
Fig. 13. Surface of wheat straw bers by different methods (a) mechanical processing and (b) chemical processing. Adopted from [262]. Copyright 2006. By permission from Elsevier Ltd.
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date palm [271], coir [272,273], bamboo [274,275], abaca [276,277], rice hull [278280], jute [281,282], and wheat straw [283]. 4.1.1.3. PS (polystyrene) and PVC (polyvinyl chloride). Only limited studies were reported regarding the usage of PS and PVC as matrixes for natural bers. The thermal and dynamic mechanical behavior [284], as well as the rheological [285] and mechanical properties [286] of PS composites reinforced with sisal bers were studied. The PS composites reinforced with agave ber were also studied regarding their ber surface modication [287]. The impact properties of PVC composites reinforced with bamboo bers [288], the interfacial modication of bagasse ber [289] and the thermal degradation of abaca ber [290] reinforced PVC composites were also evaluated. 4.1.2. Thermosets 4.1.2.1. Polyester. The possibility of using date palm bers as reinforcement in polyester composites was investigated [291]. Flexural properties and impact strength of date palm ber/polyester composites were found to be inuenced by ber content and ber treatment method. Soda treated bers exhibited higher mechanical properties compared to untreated ber/polyester composites. The ber fraction and ber length for this system were optimized for 9 wt% and 2 cm, respectively. Water absorption was lightly affected by surface modication of the bers and was relatively low. The hybrid effect on the mechanical properties of abaca and sisal ber reinforced polyester composites was evaluated [292]. A positive hybrid effect was observed for the exural properties. The tensile strength was found to be increased when the volume fraction of banana was increased. A negative effect was observed for the impact properties. Recent works regarding sisal and jute ber [293], sisal [294], abaca [295], abaca and sisal [296], ax [297], jute bers [298], sisal, abaca and bamboo ber [299] reinforced polyester composites have been developed. 4.1.2.2. Epoxy. The excellent properties of epoxy (good adhesion, mechanical properties, low moisture content, little shrinkage, and processing ease) make it one of the best matrix materials for composites. The effect of ber treatment on the mechanical properties of unidirectional sisal/epoxy composites was reported [300]. Ganan et al. [301] evaluated the mechanical and thermal properties of sisal/epoxy composites as a function of ber modication. Kenaf [302], hemp and ax [303], oil palm [304], sisal [305,306], ax [307], sisal and hemp [308], ax, hemp and kenaf [309], lantana camara ber [310] and sugar palm ber [311] were reinforced with an epoxy matrix. Their mechanical properties, processing methods, water absorption, and fracture toughness were evaluated. 4.1.2.3. Phenolic. Phenolic resins show superior re resistance to other thermosetting resins. Sreekala et al. [312316] extensively investigated oil palm ber reinforcement in phenolic resins. The ber surface modication [312], a comparison of mechanical properties to glass ber/phenolic resin composites [313], the dynamic
mechanical properties regarding the ber content and hybrid ber ratio [314], the water absorption [315] and stressrelaxation behavior [316] of oil palm/phenolic resin composites were evaluated. Bamboo [317], jute [318,319], date palm ber [320], and grewia optiva ber [321] were also investigated with phenol formaldehyde resin as a matrix. 4.2. Bio-based Public concern about the environment, climate change and limited fossil fuel resources are important driving forces, which motivate researchers to nd alternatives to crude oil. Bio-based plastics may offer important contributions by reducing the dependence on fossil fuels and, in turn the related environmental impacts. Biopolymers have experienced a renaissance in the recent years. Many new polymers were developed from renewable resources, such as starch, which is a naturally occurring polymer that was re-discovered as a plastic material. Others are poly lactic acid (PLA) that can be produced via lactic acid from fermentable sugar and polyhydroxyalkanoate (PHAs), which can be produced from vegetable oils next to other bio-based feed stocks. 4.2.1. PLA (polylactide acid) Kenaf ber reinforced PLA composites were studied extensively. Investigations have been undertaken concerning chemical modications such as alkylation [322] and silane treatments [323], the biodegradability [324] and the mechanical and dynamic mechanical properties [325]. The alkali treated ber reinforced composites, followed by silane-treated ber reinforced composite possessed signicantly improved mechanical properties. The heat deection temperature (HDT) of the kenaf reinforced PLA composites was signicantly higher than that of neat PLA resin. The biodegradability of kenaf/PLA composites corresponds to the weight of the composites, which decreased approximately 38% after four weeks of decomposition. Youngs modulus (6.3 GPa) and the tensile strength (62 MPa) of the kenaf/PLA composites (ber content = 70 vol%) were comparable to those of traditional composites. In addition, the storage modulus of the composite remained unchanged until the melting point of PLA was reached. The interfacial characterization of ax ber/PLA composites was performed on a micro-scale using the microbond testing method [326]. The interfacial mechanisms of ax/PLA biocomposite were exposed to varying thermal treatments (i.e., different cooling rates and annealing to release thermal stress). The treatments resulted in different micro-structures and residual stress states inside the material. Cooling kinetics is shown to modify the interfacial properties and when the cooling rate is slow, the interfacial properties improve. In addition, a high degree of crystallinity was measured, including transcrystallinity around the ax ber. The higher crystalline morphology of the PLA results in an improvement of the tensile and shear properties and higher residual compressive stress. Bledzki et al. [327] investigated PLA biocomposites with abaca and man-made cellulose bers and compared these
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200
(a)
Tensile strength Flexural strength
160
[MPa]
120
80
40
0 PLA PLA/abaca PLA/cellulose PP PP/abaca PP/cellulose
10000
(b)
8000
Tensile modulus Flexural modulus
[MPa]
6000
4000
2000
0 PLA PLA/abaca PLA/cellulose PP PP/abaca PP/cellulose
Fig. 15. Tensile and exural properties [(a) strength and (b) modulus] of PLA and PP composites (ber content 30 wt%). Adopted from [327]. Copyright 2009. By permission from Elsevier Ltd.
to PP composites. The composites were processed using combined molding technology: rst a two-step extrusion coating process was carried out and consecutively an injection molding was completed. With man-made cellulose of 30 wt%, the tensile strength and modulus increased by factors of 1.45 and 1.75 times in comparison to neat PLA. Reinforcing with abaca bers (30 wt%) enhanced both the E-modulus and the tensile strength by factors of 2.40 and 1.20, respectively (Fig. 15). The bers length distribution in pellets after compounding and in samples after injection molding is depicted in Fig. 16. The measurement was evaluated using approximately 500 bers. A signicant decrease in the ber length after compounding on the single-screw extruder can be observed, from the cut length of 15 mm to about 12 mm. Moreover, the injection molded samples show merely an insignicant drop in length, when put side by side to pellets. This indicates to massive ber length reduction during extrusion processes. Processing on the single-screw extruder already affected the length significantly. Compounding on twin-screw extruders, which is often carried out during composite processing, can exceedingly inuence the ber length even more. The minimal ber length achieved during compounding is not being affected during the injection molding process; however, the occurrence of the ber length seems to be more uniform. As a result, most of the bers, which remain longer than 2 mm after compounding, are shortened less than 2 mm during injection molding. PLA as a matrix for biocomposites reinforced with biober was extensively investigated for jute ber [328331], ax ber [332,333], kenaf [334,335], coir [336], bamboo [337] and cellulose bers [338,339]. Special attention was paid to the inuence of chemical treatments,
processing techniques, coupling agents, micro-brillated ber bundles, and reinforcement using man-made cellulose bers. The mechanical properties of PLA reinforced with ax bers [340], the inuence of the additives on the interfacial strength [341], as well as the effects of recycling [342] and sea water aging [343] on the mechanical properties was investigated. It was found that the composite strength is about 50% better compared to similar PP/ax ber composites, which are used in many automotive panels today. The different additives signicantly inuenced the interfacial strength of the PLA/ax ber composites while extraction with acetone had no effect compared to the untreated bers. The use of TDP (4,40-thiodiphenol) imparted the most signicant increase in interfacial shear strength whilst HBP (Hyper Branched Polyester) had an opposing effect. The repeated injection molding cycles were inuenced by many parameters; i.e., the reinforcement geometry, the molecular weight of PLA and, the thermal and rheological behavior. The tensile stiffness of PLA is hardly affected by seawater at temperatures approximately of 40 C, but the composite does loses stiffness and strength. The interfacial adhesion weakens more due to wet aging. Cracks also appear in the PLA and ax bers after longer periods of time. Huda et al. [344,345] examined the effect of reinforcing recycled newspaper, the addition of silane and talc on the thermal and mechanical properties of PLA/recycled newspaper ber composites. The results indicated that the addition of bers increased the thermal stability of the composites compared to neat PLA. The heat deection temperature of the PLA/recycled newspaper ber composites was found to be comparable to that of the glass ber-reinforced PLA composites. The silane treated talc reinforced PLA/recycled newspaper ber hybrid composites exural and impact strength was found to be signicantly higher than that of those made without silane treated composites. The silane treated hybrid composites showed improved properties such as a exural strength of 132 MPa and a exural modulus of 15.3 GPa, while the untreated composites exhibited exural strength and modulus values of only 77 MPa and 6.7 GPa, respectively. PLA and PHBV were compounded with man-made cellulose; jute and abaca bers and their mechanical performance were studied and compared to PP based composites [346]. It is clearly seen in Table 7 that the tested biopolymer based composites clearly show better or comparable mechanical characteristic values than the common natural ber reinforced PP composites. 4.2.2. PHB (polyhydroxybutyrate) The biopolymer polyhydroxybutyrate (PHB) was also reinforced with ax ber. Barkoula et al. [347] investigated the effects of ber and copolymer HV (hydroxyvalerate) contents, the biodegradability, and the inuence of manufacturing methods (compression molding of non-woven mats and injection molding of short ber compounds) and processing conditions (cooling temperature and annealing) on the mechanical properties of the composites. It can be concluded that the addition of ax bers, along
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Fig. 16. The ber length of abaca/PLA composites after different processes. Adopted from [327]. Copyright 2009. By permission from Elsevier Ltd.
with controlled processing conditions, is a convenient technique to toughen the PHB matrix. The injection molded composites exhibited lower impact strength than other manufactured composites. The tensile strength dropped signicantly in the initial stage of degradation and was more gradual in later stages of biodegradation. The interfacial improvement of PHB/ax composites was also evaluated. The addition of TDP at various concentrations (up to 10% v/v) brought advantageous changes in the dynamic exural properties and thermal stability (favorable shift of degradation temperatures to higher values). With increases of the TDP content, improvements were observed in the bermatrix bonding and a change in the matrix from brittle to ductile [348]. Zini et al. [349] illustrated that composites prepared by compression molding using long ber mats showed better mechanical properties
compared to composites obtained by batch mixing bers with molten polymer. Chemically modied (by acetylation or by short-chain-PEG grafting) bers exhibit better adhesion and the best results were obtained with acetylated bers. Several lines of transgenic ax were produced by overexpressing the PHB synthesis genes [350]. It was revealed that the cellulose in bers from the transgenic plants was more highly structured than in bers from the control plants and PHB was strongly bound to the cellulose of the bers by covalent ester and hydrogen bonds. The PHB/ax composite with bers from transgenic plants was signicantly stronger and stiffer than the composites with bers from the control plants. Polyhydroxybutyrate-co-valerate (PHBV) bioplastic was reinforced with hemp [351], coir [352], and bamboo
Table 7 Mechanical properties of PLA, PHBV and PP based natural ber reinforced composites. Matrix PLA Fiber Man-made cellulose Abaca Jute Man-made cellulose Abaca Jute Man-made cellulose Abaca Jute Tensile E-modulus (GPa) 3.4 5.8 8.0 9.6 2.14 4.4 4.4 7.0 1.5 3.7 4.9 5.8 0.23 0.15 0.34 0.36 0.07 0.34 0.06 0.26 0.03 0.11 0.11 0.47 Tensile strength (MPa) 63.5 92.0 74.0 81.9 27.3 41.7 28.0 35.2 29.2 71.6 42.0 47.9 0.4 4.7 0.7 2.9 0.3 3.8 1.3 1.3 0.4 2.7 0.5 2.7 Tensile elongation-at-break (%) 3.3 0.5 1.9 03 1.44 0.1 1.8 0.0 7.0 1.1 2.3 1.0 0.9 0.1 0.8 0.0 >50 3.5 0.5 1.7 0.2 1.4 0.1
PHBV/ecoex
PP
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[353] bers. The mechanical, thermo-mechanical and morphological properties were evaluated. 4.2.3. Starch Alvarez et al. [354356] developed composites by mixing biodegradable starch matrixes with sisal bers. The thermal, melt rheological and creep properties were investigated extensively. It was reported that the shear rate is the most inuential processing condition regarding the material structure. The intercalation effectiveness of the matrix in the bers is directly linked to the rheological behavior. The addition of sisal bers to the polymeric matrix promotes a signicant improvement of the composite creep resistance and thermal properties. Investigations were carried out using starch as the matrix of composites with kenaf, bagasse [357], curaua [358], coir [359], bamboo [360], sisal [361], hemp [362,363], abaca and bagasse [364] bers, wheat straw bers [365], and kenaf bers [366]. 4.2.4. Others A soy based biodegradable resin matrix was applied to cellulose from papers [367], ax [368], sisal [369] and pineapple leaf [370] ber reinforced composites. Biodegradable resins have been tested, including cashew nut shells [371,372] with hemp and kenaf bers, polybutylene succinate (PBS) with jute bers [373,374] bamboo bers [375], and hemp bers [376], and polycaprolactone (PCL) with ax bers [377] and bamboo bers [378]. 4.3. Summary The petroleum derived thermoplastics PP and PE are the two most commonly employed thermoplastics in natural ber reinforced composites. Day by day, there is great interest in developing biocomposites with a thermoplastic rather than thermoset matrix, mainly due to their recyclability. Also the choice of a thermoplastic matrix ts well within the eco-theme of biocomposites, but there are some important limitations on the recyclability and mechanical performance of thermoplastics. Generally, the mechanical properties of thermosets exhibit higher than the thermoplastic (lower modulus and strength). In addition, a dramatic loss in properties is observed above the glass transition temperature, which leads to decrease in other thermally sensitive properties such as creep resistance. On the contrary, thermoplastics show greater fracture toughness than thermosets and thus are more useful in resisting impact loads. Another remarkable change was the introduction of biopolymers in recent years with the aim of decreasing reliance on petroleum-based thermoplastics. The availability and outstanding mechanical properties of biopolymer PLA has led to this matrix system being one of the most thoroughly investigated in the biocomposites research area. 5. Processing techniques Generally, natural ber reinforced plastic composites are manufactured by using traditional manufacturing techniques (designed for conventional ber reinforced polymer
Fig. 17. Water absorption of HDPE composites with and without compatibilizers. Adopted from [380]. Copyright 2007. By permission from Elsevier Ltd.
composites and thermoplastics). The processing techniques includes compounding, mixing, extrusion, injection molding, compression molding, and resin transfer molding (RTM) and above mentioned techniques have been well developed and accumulated experience has proofed their successability for producing composites with controllable quality. Innovative technologies and process solutions should be intensively researched to get the high strength engineering composites which is related to their new applications area. 5.1. Factors inuencing processing 5.1.1. Moisture The moisture content at a given relative humidity can have a great effect on the biological performance of a composite made from natural bers and therefore ber drying before processing is a signicant step. A composite made from pennywort bers would have much greater moisture content (57%) at 90% RH humidity than would a composite made from bamboo bers (15%). The pennywort product would be much more prone to decay as compared to the bamboo product. Moisture content of natural bers with time under different conditions (relative humidity) and for different ber treatments were analyzed [379]. It was evident that the moisture content as well as the rate at which it accumulates is directly related to the ambient relative humidity. Fiber treatment can reduce both the moisture content level and the rate of absorption very signicantly. It should be noted that bio based polymers can be more sensitive to moisture than natural bers. Panthapulakkal and Sain investigated the effect of compatibilizer on the water absorption behavior of HDPE composites with different llers (wheat straw, cornstalk, and corncob). This is shown in Fig. 17 [380]. Presence of compatibilizer had no effect on the water absorption of
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Fig. 18. Compounding methods for injection molding of natural ber reinforced thermoplastics. Adopted from [383]. Copyright 2006. By permission from Institute for Materials Technology of the University of Kassel, Germany.
corncob lled composites. Wheat straw and cornstalk lled composites showed a decrease in the water uptake with the incorporation of compatibilzers. This indicates that, the aws and gaps at the interface of the ller and HDPE are the main factors for moisture diffusion in the composites without compatibilizer. As observed in mechanical properties, the observed reduction in water uptake is higher in wheat straw lled composites compared to cornstalk lled composites. After 40 days of water absorption, percentage reduction in the water uptake of composites is 19%, 12% and 0% respectively for wheat straw, corn stalk and corncob lled composites. It is already seen that the enhanced water content can drastically affect mechanical properties (such as, compression, exural and tensile) of the composites [381]. Nowadays new extruder screw design (higher L/D ratio) allows better degassing and, consequently, lower moisture content. In addition, the machines barrel must be redesigned.
5.1.2. Fiber type and content The natural ber type and content is generally essential for furthering the sustainability of the composite. In addition, natural bers length (short or long), aspect ratio (length/diameter), chemical compositions (such as rice husk contains higher silicates than ax or jute ber) have an great inuence on the processing and therefore processing parameters and accessories should be developed. The compounding process signicantly inuences the shortening, brillation, as well as the thermal deterioration of the bers in early stages; the nal properties of the product are already determined at the beginning of the production process [382]. Fig. 18 shows the different compounding processes for injection molding of natural reinforced thermoplastics [383]. 5.1.3. Inuence on composites properties As described above, the natural ber type has strongly inuence on the performance of the composite. There are
Fig. 19. Inuence of different natural bers on the tensile and Charpy notched impact strength (+23 C) of PLA biocomposites (ber content 30 wt%). Adopted from [387]. Copyright 2008. By permission from Woodhead Publishing Ltd.
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Fig. 20. Inuence of abaca ber content on odor concentration of abaca/PP composites. Adopted from [387]. Copyright 2008. By permission from Woodhead Publishing Ltd.
numerous types of natural bers, which differ regarding their chemical structure [384386]. The inuence of the type of natural ber on some mechanical parameters of PLA biocomposites is presented in Fig. 19 [387]. In general, increasing ber content in the composites increases the composites stiffness signicantly. Additionally its strength is increased through the addition of natural bers [388,389]. Higher ber content improves the impact strength. Unfortunately, increased ber content increases the composites odor (Fig. 20) as well as the water uptake [387]. Moreover, the composites ductility can be affected. The ber length and its geometry also play a decisive role in composites. Usually, most mechanical properties of a ber can be enhanced by increasing the aspect ratio [390]. In addition, the use of one appropriate additive (coupling agents, lubricants, light stabilizers, colorants, ame retardants, foaming agents, odor reduction agents, and biocides) in very small quantities (0.55%) can signicantly improve most of physical, chemical or mechanical properties of natural ber composite material [391]. 5.2. Semi-nished product manufacturing Mat production is one of the initial steps in seminished product manufacturing. Fiber mats (ber eece) from natural bers could be manufactured by carding method, aerodynamic eece making, the ber spreading process, and wet eece production. The other step is the production of slivers and ber yarns. The ber preparation (opening, mixing, and carding) is similar to eece production. Granule production is the other important step in the manufacture of semi-nished products. Natural ber granules can be produced via pelleting, compounding, pultrusion and the pull-drill process regarding the homogeneity of the granules and the desired ber lengths. 5.3. Processing technologies for natural ber reinforced thermoplastics 5.3.1. Compression molding The pressure method is very popular in the manufacture of natural ber composites because of its high reproducibility and low cycle time. The two methods in use are compression and ow compression molding. The
processes differ concerning the kind of semi-nished product used and its cutting. In the compression molding process, at semi-nished products or hybrid eeces are usually used that are either larger than the form or are cut exactly to the size of the desired part. Whole and split wheat straws with lengths up to 10 cm were used with PP to make lightweight composites by means of the compression molding process [392]. The effects of the wheat straw concentration, length, and split conguration (half, quarter, and mechanically split) on the exural and tensile properties of the composites were investigated. Compared with whole wheat strawsPP composites, mechanically split wheat strawPP composites have a exural strength that is higher by 69%. They also have a 39% higher modulus of elasticity, 18% higher impact resistance properties, 69% higher tensile strength and a 26% higher Youngs modulus. Compared with jutePP composites, mechanically split wheat strawPP composites have a 114% higher exural strength, 38% higher modulus of elasticity. In addition, they also have a 10% higher tensile strength, 140% higher Youngs modulus, a 50% lower impact resistance and better sound absorption properties. The compression molding process was tested for jute ber with PP [393], an ethylene propylene co-polymer [394] and, baggase bers with PET composites [395]. Also the abrasive wear behavior, interfacial adhesion, and degradability were evaluated. 5.3.2. Extrusion The extrusion process is used by the plastics industry for the production of granules and also in the continuous production of semi-nished products or components. Single screw as well as twin-screw extruders that run either co- or counter-rotating may be used for this process. Single screw extruders are used when the mixing effect does not have to be very high. Owing to the excellent mixing effect of the twin-screw extruder the natural ber materials can be homogenously distributed and wetted in the thermoplastic melt. HDPE composites with bagasse [396] and curaua [397] bers reinforced HDPE composites were obtained by extrusion process. The effects of coupling agents on the mechanical and thermal properties of those composites were investigated and evaluated. Curaua bers were also reinforced with PA-6 by using a co-rotating twin-screw extruder [398]. The ber contents of 20 wt%, 30 wt% or 40 wt% and ber lengths of 0.1 or 10 mm were studied. Fibers were treated with N2 plasma or washed with NaOH solution, to improve their adhesion to PA-6. The tensile and exural properties of this composite are better than unlled, but are still lower than those of glass ber reinforced polyamide-6. 5.3.3. Injection molding It is possible to produce complex geometric components with functional elements fast and also in great numbers by injection molding. It offers a number of advantages (economics of scale, minimal warping and shrinkage, high function integration, use of recycled materials) as compared to compression molding [399] and hardly any nishing needed.
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Table 8 Tensile strength and modulus of PP and PP/hemp ber/glass ber hybrid composites before and after aging (A. 0 wt% glass ber, B. 5 wt% glass ber, C. 10 wt% glass ber, D. 15 wt% glass ber). Sample designation Tensile strength (MPa) Original PP A B C D 30.1 52.5 53.7 57.9 59.5 0.1 0.5 1.6 0.7 0.9 Wet sample 29.9 34 34.8 34.9 35.5 0.5 0.6 1.6 0.9 0.5 Retention (%) 99 65 65 60 65 Tensile modulus (GPa) Original 1.10 3.77 4.07 4.25 4.4 0.03 0.05 0.05 0.04 0.01 Wet sample 0.89 1.64 1.74 2.04 2.32 0.03 0.04 0.03 0.05 0.12 Retention (%) 81 44 43 48 53
Pickering and his co-workers [400403] extensively investigated hemp ber reinforced PP composites used in the injection molding process. Their investigations included ber treatments and modications, model predictions of micro-mechanics and strengths, the optimization of hemp ber quality, and the inuence of bag retting and, white rot fungal treatments. The effect of surface treatment on the injection molded pineapple leaf ber reinforced polycarbonate composites was evaluated [404]. The modied pineapple leaf bers composite produces enhanced mechanical properties. The results from the thermogravimetric analysis showed that the thermal stability of the composites is lower than that of neat polycarbonate resin and that the thermal stability decreased with increasing pineapple leaf ber content. Injection molded jute [405] and sisal [406] ber reinforced PP composites were also investigated regarding their thermal, hydrothermal and, dynamic mechanical behavior. The introduction of the pre-impregnation technique was also examined. Panthapulakkal and Sain investigated the inuence of water absorption on the tensile properties of injection molded short hemp ber/glass ber-reinforced polypropylene hybrid composites [407]. Tensile tests were performed on wet samples after the saturation level (3624 h) is reached (Table 8). A signicant reduction in strength and stiffness is observed for all composites because of the changes to the bers, mainly natural bers, and the interface between the matrix and ber, as the effect of water absorption on PP matrix is only secondary. Swelling of natural ber as a result of prolonged exposure to water, leads to at reduction in the stiffness of the bers. The loss in strength and modulus values of the hemp ber composites are believed to be the inability of the swelled natural ber to carry the stress transferred from the matrix through the disrupted interface as a result of water absorption. Despite the reduction in the equilibrium moisture content in hybrid composites, glass bers did not alter the degradation of the hemp ber composites.
Injection molded ax, hemp, core hemp, bleached kraft pulp (BKP) and wood our reinforced PP composites were prepared and the effect of MAPP on the mechanical properties was investigated [408]. Table 9 clearly indicated that the BKPPP composites have the highest tensile and exural strength and unnotched impact strength. Flax and hemp-lled PP composites have similar strength properties. In comparison, wood our-lled PP composites have the lowest mechanical strength. Such a trend can be attributed to the actual ber length in the composites. It has been observed that after compounding, the ber length of ax and hemp decrease signicantly, whereas that of BKP bers dose not change much. This is possibly due to the fact that the ax and hemp bundles are prone to being torn down to very small size by the high-shear force from the melted PP. To preserve the ber length, less severe treatment is necessary but at the cost of poor dispersion of bers in the resin matrix. The poor strength of wood our reinforced composites is due to the low aspect ratio of wood our particles, which is far below the critical ber length required for reinforcement. Bledzki et al. [409] investigated the different separation processes (mechanical, rener and enzymatic separation) with injection molded hemp and partially with ax and wheat straw reinforced PP composites. It was found that thermomechanical processed hemp berPP composites possessed better mechanical properties compared to other process and composites. 5.3.4. Long ber thermoplastic-direct (LFT-D) method Different methods [410] to directly process natural bers with the LFT-D-process are shown (Fig. 21). Express method, which is the basic thought of the combined extrusion and press method to combine the natural ber mats with the polymer melt directly in the pressing tool. A lm of molten polymer is placed into the pressing tool with the help of an adjustable extruder and a natural ber eece is added to the molten mass and the layers are pressed together. Another possibility to process natural bers with
Table 9 Effect of ller type on mechanical strength performance of lledPP composites (40% ller, 2% compatibilizer). Fiber type Tensile (MPa) Tensile modulus (GPa) Flexural (MPa) Flexural modulus (GPa) Notched Izod (J/m) U-notched Izod (J/m) BKP 50 3.0 78 3.3 40 205 Flax 42 3.2 67 3.4 44 150 Milled hemp 42 3.0 70 3.5 42 145 Core hemp 29 2.3 52 2.6 20 100 Wood hour 35 2.9 59 3.0 28 105
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Fig. 21. Express method and direct extrusion of natural bers. Adopted from [410]. Copyright 2002. By permission from Institute for Materials Technology of the University of Kassel, Germany.
the LFT-D-method is to directly feed off ber yarns or slivers into either a twin screw extruder or directly into an injection molding machine. Research has shown that it is possible to retain the long ber structure through an optimal conguration of the screws; however, the handling of slivers is rather problematic in an industrial application (extrusion with high throughput). 5.4. Processing technologies for natural ber reinforced thermosets 5.4.1. Resin transfer molding Resin transfer molding (RTM) is a method for the production of component parts made of ber-plastic composites. During the RTM procedure, dry semi-nished ber parts are streamed and consequently soaked with reaction resin by a pressure gradient within a closed vessel. The following methods can be distinguished with regard to the admission by the pressure gradient: high pressure injection, twin wall injection, vacuum injection, and differential pressure injection. Hemp ber-unsaturated polyester composites were manufactured using a resin transfer molding (RTM) process [411]. RTM composites with various ber contents, up to 20.6% by volume, were manufactured. The wetting of the bers was very good. The resin injection time was observed to increase dramatically at high ber contents due to the low permeability of the mat. Keeping a constant mold temperature is the key to obtain fast and homogeneous curing of the part. The cure of the resin in the mold was simulated. The results given by the modied model are presented in Fig. 22. The predicted temperatures were in very good agreement with the experimental data. The model predicted the degree of cure and the rate of cure of the resin with time as well. The hemp ber composites manufactured with RTM process were found to have a very homogeneous structure with no noticeable defects [412]. The tensile, exural and impact properties of these materials was found to increase linearly with increasing ber content (Table 10). It was observed that the optimum properties were not reached in this study and that ber content higher than 35 vol% should yield better mechanical properties. When compared to a glass ber composite however these natural ber composites had much lower performances. Hemp ber reinforced polyester [413] and phenolic resin [414] composites were prepared using RTM process
Fig. 22. Comparison of RTM experiment and corrected model for a pure resin system. Adopted from [411]. Copyright 2004. By permission from Elsevier Ltd.
and their cure simulation, interfacial adhesion, and ow visualization were evaluated. The effects of ber surface modication [415] were evaluated. A comparison of the RTM process to the compression molding process [416] of sisal ber reinforced polyester composites was made. Composites containing ax and hemp ber with bio-resin [417], ax and jute ber with epoxy and polyester resin [418], and jute ber with polyester resin [419] were also prepared using the RTM process. 5.4.2. Sheet molding compound The sheet molding compound (SMC) material made of natural bers and a special resin based on vegetable oil and carbohydrates represents an effective alternative to the established systems within the technically specialized sector. Procedural modications are not necessary in comparison to conventional SMC production of component
Table 10 Mechanical properties of 20 vol% glass ber, 20 vol% hemp ber and 35 vol% hemp ber-reinforced unsaturated polyester composites. 20 vol% glass bers Tensile strength (MPa) Tensile modulus (GPa) Flexural strength (MPa) Flexural modulus (CPa) Impact strength (kJ/m2 ) 85.0 1.719 175.9 7.74 60.8 20 vol% hemp bers 32.9 1.421 54.0 5.02 4.8 35 vol% hemp bers 60.2 1.736 112.9 6.38 14.2
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Fig. 23. Thermoset mat compression process and ready component part; raw and covered by all functional and decorative details. Adopted from [423]. Copyright 2006. By permission from Institute for Materials Technology of the University of Kassel, Germany.
parts [420]. The middle bumper part for a city bus was manufactured with standard tools. The risk potential for the fabricator is lower, both during production and treatment of the prepregs which are made of natural bers and vegetable oil. Emissions do not occur; hence, there is no need for breathing protection [421]. Flax ber reinforced SMC material was developed and the processing parameters regarding the physico-mechanical properties were optimized [422]. 5.5. Other processes 5.5.1. Thermosets compression molding The thermosets compression process uses mats made of natural bers. As shown in Fig. 23, the mats are just sprayed, not moistened, with resin and compressed into their nal contour in a hot tool; due to the air-permeability the parts can be covered easily in a vacuum covering process [423]. The dynamic and static mechanical properties of short abaca/sisal hybrid ber reinforced polyester composite achieved using the thermoset compression molding process were determined [424]. Dynamic properties, such as the storage modulus, damping behavior and static mechanical properties (i.e., tensile, exural and impact properties) were investigated as a function of the total ber volume fraction and the relative volume fraction of the two bers. The storage modulus was found to increase with ber volume fraction above the glass transition temperature (Tg ) of the matrix. A maximum value was obtained at a volume fraction of 0.40. The tensile modulus and exural strength were found to be the highest at a volume fraction of 0.40, which indicates effective stress transfer between the ber and the matrix. Sisal/polyester composites displayed the best damping behavior and highest impact strengths compared to abaca/polyester and hybrid composites. However, maximum stress transfer between the ber and the matrix was obtained in composites with a volume ratio of banana and sisal equal to 3:1. The tensile strength and exural modulus reached their maximum at this volume ratio, while the impact strength reached its minimum. The thermal conductivity, diffusivity and specic heat of thermoset compression molded polyester/natural ber (abaca/sisal) composites were investigated for several ber surface treatments as functions of the ller concentration [425]. The thermo-physical behavior of hybrid pineapple leaf ber (PALF) and glass ber reinforced polyester
composites were also evaluated regarding the constant total ber loading equal to 0.40 volume fraction by varying the ratio of PALF and glass. The results show that the chemical treatment of the bers reduces the composite thermal contact resistance. Hybridization of natural bers with glass allows a signicantly better heat transport ability of the composite. The thermal conductivity, which is measured in the direction transverse to the plane of composite plate, could be well represented by a series prediction model. 5.5.2. Pultrusion Fibers are pulled from a creel through a resin bath and then on through a heated die. The impregnation of the ber controls of the resin content and curing of the materials into their nal shape is completed using the die. Although pultrusion is a continuous process, which produces a prole of constant cross-sections, a variant known as pulforming allows for some variation to be introduced into the crosssections. Flax ber reinforced PP composites were developed by means of the thermoplastic pultrusion process and their physic-mechanical properties were evaluated [426]. The water absorption behavior of pultruded jute ber reinforced unsaturated polyester composites was found to follow so-called pseudo-Fickian behavior [427]. The exural and compression properties were found to decrease with the increase in water uptake in percentage. These exural and compression behaviors were attributed to the plasticization of the matrix-ber interface and the swelling of the jute bers. Pultruded kenaf ber [428], jute ber [429] and hybrid jute/glass and kenaf/glass ber [430] composites were investigated and their exural behavior using acoustic emission, dynamic properties and degradation of compressive properties were evaluated. 5.5.3. Summary In recent years the processing and production technologies for biocomposites have also advanced. To date, injection molding, extrusion, compression molding, sheet molding and resin transfer molding are the major manufacturing processes for natural ber reinforced plastic composites. But new downstream and auxiliary equipment has been designed. Such as: unique heating and single or dual venting systems for in-line drying, high-intensity
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spray-cooling tanks, a variety of new congurations of feeding (gravimetric or vertical crammer) systems, combinations of extrusion-injection molding or extrusioncompression molding as well as screw, die, and mold design. Although the majority of biocomposites produced today by the processes mentioned above, the manufacturers are improving the feasibility of using other processes like pultrusion and so on. 6. Performance of biocomposites It is important to be knowledgeable of certain mechanical properties of each natural ber in order to be able to exploit the highest potential of it. Among these properties are the tensile, exural, impacts, dynamic mechanical and creep properties. In general, natural bers are suitable for reinforcing plastics, due to their relatively high strength, stiffness and low density. 6.1. Tensile properties The tensile properties are among the most widely tested properties of natural ber reinforced composites. The ber strength can be an important factor regarding the selection of a specic natural ber for a specic application. A tensile test reects the average property through the thickness, whereas a exural test is strongly inuenced by the properties of the specimen closest to the top and bottom surfaces. The stresses in a tensile test are uniform throughout the specimen cross-section, whereas the stresses in exure vary from zero in the middle to maximum in the top and bottom surfaces. The comparison of the tensile properties of the HDPE/hemp ber composites showed that the silane treatment and the matrix-resin pre-impregnation of the ber produced a signicant increase in tensile strength, while the tensile modulus remained relatively unaffected [431,432]. The longitudinal tensile strength increased from 71.8 MPa to 79.3 MPa for the silane treated bers, which equals an increase of approximately 10%. The increase in the transverse tensile strength from 2.75 MPa for the untreated bers to 3.95 MPa for the treated bers is higher, representing an increase of 43%. It is evident that the behavior is ber dominated, as the longitudinal ber direction, is 1900% higher compared to transverse direction. Fiber surface modication has little impact. However, the improvement in the bermatrix interactions plays a more important role for the matrix and/or interphase dominated behavior. Rice husk reinforced PP composites with ller loadings of 10 wt%, 20 wt%, 30 wt% and 40 wt% were designed [433]. Six test temperatures (30, 0, 20, 50, 80 and 110 C) and ve levels of crosshead speed (2, 10, 100, 500 and 1500 mm/min) were designed during tensile testing. The tensile strengths of the composites decreased slightly as the ller loading increased. The tensile modulus improved with increasing ller loading. As the crosshead speed increased, the composite became more brittle. At lower test temperatures (30 and 0 C), the composites exhibited strong and brittle properties similar to glass ber, but the tensile strength and modulus decreased due to the glass
transition of the matrix polymer PP as the test temperature was increased from 0 to 20 C. A study on the effect of alkaline treatment on tensile properties of sugar palm ber reinforced epoxy composites was investigated [434]. The treatment was carried out using different concentrations of sodium hydroxide (NaOH) solutions and varying soaking periods. It was observed that as the alkali concentration and the length of soaking periods increased, the tensile strength decreased. However, the tensile modulus results are much higher than those of untreated ber composite specimens, thus proving the effectiveness of the treatment. Composites consisting of aliphatic polyester (Bionolle) with ax bers were prepared via batch mixing [435]. The effects of processing conditions on the ber length distribution and the dependence of the composite tensile properties on the ber content were investigated. The tensile modulus changes with the amount of ber content according to the modied rule-of-mixture equation. The tensile strength of Bionolle/ax composites tends to decrease with ber loading, showing that there is no adhesion between the matrix and the bers. Flax bers with chemically modied surfaces were also tested as reinforcing agents. An increase in tensile strength of 30% was observed when ax bers (25 vol%) were substituted with bers containing acetate groups. No signicant strength changes were observed in composites containing bers with valerate groups or polyethylene glycol chains grafted at the surface. The following investigations were completed with thermoplastic matrices; the effect of moisture absorption of sisal ber/PP composites [436], the inuence of surface treatment (NaOH solution) of coir ber/PP composites [437], the surface esterication of bagasse/LDPE composites [438], the surface modication of olive husk/PP composites [439], the performance of hybrid jute/betel nut ber reinforced PP [440], and the effects of surface treatments of luffa ber/PP composites [441]. It was observed that the tensile properties were inuenced by all the mentioned factors. The tensile properties of natural ber reinforced thermosets were investigated regarding the siloxane treatment of jute ber/polyester and epoxy composites [442], the temperature and loading rate effects of kenaf ber/epoxy composites [443], the effects of a differing geometry of abaca ber/epoxy composites [444], the inuence of moisture absorption of bamboo/vinylester composites [445], the effect of oil palm bers volume fraction of oil palm/polyester composites [446], and the inuence of the ber orientation and the volume fraction of alfa ber/polyester composites [447]. The effects of hybridization and the chemical modication of oil palm/sisal ber reinforced natural rubber composites [448,449], the effects of high temperature on ramie ber/biodegradable resin composites [450], effect of biodegradable matrix type (PLA, PHBV, PBS) on regenerated cellulose ber/biopolymer composites [451], the inuence of bio based coupling agent on bamboo ber/PLA and PBS composites [452], preparation of sandwich composite panels for building applications from jute/polyester [453], and the structural and mechanical characterization of sugar
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beet pulp/PLA composites [454] on the tensile properties were evaluated. Rao et al. [455] investigated the tensile properties of bamboo, date palm, abaca, oil palm, sisal, coir and vakka bers regarding their ber cross sections, atmospheric moisture content and density.
6.2. Flexural properties The exural stiffness is a criterion of measuring deformability. The exural stiffness of a structure is a function based upon two essential properties: the rst is the elastic modulus (stress per unit strain) of the material that composes it; and the second is the moment of inertia, a function of the cross-sectional geometry. Zampaloni et al. [456] focused on the fabrication of kenaf ber reinforced PP sheets that could be thermoformed for a wide variety of applications with properties that are comparable to existing synthetic composites. The optimal fabrication method determined for these materials was determined to be a compression molding process which utilized a layered sifting of a microne PP powder and chopped kenaf bers. When comparing the exural strengths of the kenaf ber/PP composite materials, 40% kenaf/PP composites performed signicantly better than the 30% kenaf/PP composites. The exural strength of 40% kenaf/PP was equivalent to the ax/PP, larger than the hemp/PP and almost doubles that of the coir/PP and sisal/PP composites. The exural strength of 30% kenaf/PP composites showed results equivalent to those of the 40% hemp/PP composites, while also outperforming the coir/PP and sisal/PP composites. Composites of PP and HDPE reinforced with 20 wt% curaua bers were prepared and the effect of screw rotation speed was evaluated by measuring the exural properties of the composites [457]. The yield stress in exural tests for the composites with PP and HDPE matrixes, decreased with the increase in screw rotation speed. For HDPE a higher rate of decrease was shown. However, the exural modulus was not affected by the screw rotation speed. The elongation at break exhibited different behavior; this effect strengthened HDPE at screw rotations above 300 rpm, and slightly increased for PP composites above 350 rpm. The effect of acetylation [458] on the exural properties of bagasse/PP composites (properties decreased due to acetylation), and the effect of different maleated coupling agents (exural properties increased above 60% with optimum loading of coupling agent) on jute and ax ber reinforced PP composites [459] have been evaluated. Composites were fabricated using abaca ber with varying ber lengths and ber loading [460]. The analysis of the exural properties revealed the optimum length of abaca bers required for abaca ber/phenol formaldehyde resin composites. The exural strength and modulus values increased with ber length for composites with short bers. Furthermore, the maximum exural strength and modulus values were obtained for 40 mm bers. Due to ber loading up to 45%, the exural modulus increased to about 25%. The exural strength also showed good enhancement, because of increasing ber loading.
The exural properties of coir ber/polyester composites were evaluated [461]. Composites were prepared using two molding pressures and with amounts of coir ber up to 80 wt%. When the ber amount equaled up to 50 wt%, rigid composites were obtained. Higher ber amounts resulted in composite performances similar to that of exible agglomerates. The results obtained for the exural strength made it possible to compare the technical performance of the composites with that of other conventional materials. The exural properties of thermoset resins, such as cardanol reinforced with hemp, ramie, jute and ax bers [462], epoxy resin with coir bers [463], and hemp, kenaf, ax and henequen bers [464], polyester resin reinforced bagasse bers [465], coir and oil palm bers [466], hemp and kenaf bers [467], were also investigated. Biocomposites were fabricated from chopped hemp ber and cellulose ester biodegradable plastic via two different processes: powder impregnation by compression molding and an extrusion process followed by an injection molding process [468]. Fabricated through process extrusion followed by injection molding process of hemp (30 wt%) ber reinforced cellulose acetate biocomposite exhibited exural strength of 78 MPa and modulus of elasticity of 5.6 GPa as contrast to 55 MPa and 3.7 GPa for the corresponding hemp ber/PP based composite. The corresponding biocomposites showed superior exural strength and modulus values during the extrusion and ensuing injection molding processes, as compared to biocomposites powder impregnated through compression molding process. Biodegradable composites were prepared with the melt blending technique using PCL and oil palm empty fruit bunch ber [469]. Since oil palm ber is not compatible with PCL, a binder (polyvinyl pyrrolidone), was used to improve the interaction between PCL and the bers. The composites produced were irradiated with the aid of an electron beam to improve the mechanical properties. The exural strength and modulus of the composites were improved by an additional 1% by weight of poly(vinyl pyrrolidone) and irradiated with a 10 kGy electron beam.
6.3. Impact properties Impact strength is the ability of a material to resist fracture under stress applied at high speed. Biober reinforced plastic composites have properties that can compete with the properties of glass ber thermoplastic composites, especially concerning specic properties. However, one property, namely the impact strength is often listed among the major disadvantages of biober reinforced composites. In recent years, the development of new ber manufacturing techniques and improved composite processing methods along with enhancement of ber/matrix adhesion has improved the current situation somewhat. Jute ber was treated with o-hydroxybenzenediazonium salt (o-HBDS) in alkaline media [470]. Treated and untreated jute ber reinforced PP composites were prepared with different weight fractions (20, 25, 30, and 35%) of jute ber. The increase of Charpy impact strength was
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found to be exceptionally high (in some cases 200%) as compared to those of literature values. Composite panels consisting of virgin and recycled HDPE and four types of rice straw components including rice husk, rice straw leaf, rice straw stem, and whole rice straw were made via melt compounding and compression molding [471]. Composite panels with rice husk exhibited better impact strength than composites panels made of other straw bers. Minor differences concerning the impact properties existed among leaf, stem, and whole straw bers. The recycled HDPE resin and its composites possessed a signicantly better impact strength compared to the virgin HDPE systems. This was attributed to the additives used during initial processing. Recycled HDPE composites were reinforced with bagasse bers and the inuence of coupling agent types/concentrations on the composite impact properties were studied [472]. The addition of maleated polyethylene (MAPE), carboxylated polyethylene (CAPE), and titanium-derived mixture (TDM) improved the compatibility between the bagasse ber and recycled HDPE. The impact properties of the resultant composites were comparable with those of virgin HDPE composites. The better impact strength of the composites was achieved, when a MAPE coupling agent was used. The impact strength increased with increasing MAPE content. Oil palm empty fruit bunch ber reinforced composite was studied. The effects of ber loading and impact modiers, namely chlorinated polyethylene (CPE) and acrylic, on the impact properties of oil palm ber lled-PVC composites were of particular interest [473]. The results from the impact test showed that the unlled PVC samples of both impact modiers change from brittle to ductile with increasing impact modier concentration. The incorporation of bers into unmodied PVC and modied PVC resulted in the reduction of the impact strength. As the ber content increased from 10 to 40 phr, the impact strength reduced about 40% and 30% for acrylic-modied PVC and CPE-modied PVC, respectively. The impact strength reduction was only marginal for unmodied PVC composites. The impact modier enhanced the impact strength of ber reinforced PVC composites. However, the effectiveness decreased with increased ber loadings. The impact strength of CPE-modied PVC was higher than acrylicmodied PVC at ber contents of 20 phr and higher. The impact properties regarding the inuence of the ber microstructure of sisal, abaca, jute and ax ber reinforced PP composites [474], the processing methods for ax ber/PP composites [475], and the effect of impact modiers (natural rubber and ethylene propylene diene monomer) on grass ber/PP composites [476] were investigated. Hemp ber reinforced unsaturated polyester composites were subjected to low velocity impact tests in order to study the effects of non-woven hemp ber reinforcement on their impact properties [477,478]. The composite specimen containing 0, 0.06, 0.10, 0.15, 0.21 and 0.26 ber volume fractions (Vf ) were prepared and their impact responses were compared with samples containing an equivalent ber volume fraction of chopped strand mat E-glass ber reinforcement. A signicant improvement in
the load bearing capability and impact energy absorption was found after the introduction hemp ber as reinforcement. The results indicated a clear correlation between ber volume fractions, stiffness of the composite laminate, impact load and total absorbed energy. Unreinforced unsaturated polyester control specimens exhibited brittle fracture behavior with a lower peak load, lower impact energy and less time until failure occurred than hemp reinforced unsaturated polyester composites. The impact test results showed that the total energy absorbed by 0.21 ber volume fraction (four layers) of hemp reinforced specimens is comparable to the energy absorbed by the equivalent ber volume fraction of chopped strand mat E-glass ber reinforced unsaturated polyester composite specimens. The effects of the bi-dimensional orientation of leaf stalk bers from peach palms (peach palm powder and weave) on the impact strength behavior of polyester/ber reinforced composites were studied [479]. The Izod impact data obtained for the composites with only woven material was considerably superior to that of composites containing only powder, suggesting that the reinforcement in the form of powder is inefcient, independent of the size range of the particles used. The impact strength of the bamboo ber/PLA composites decreased after addition of bamboo ber [480]. The impact strength of treated ber reinforced composites improved after the addition of treated bers. Good ber/matrix adhesion provides an effective resistance to crack propagation during impact tests. The impact strength increased signicantly (33%) for silane treated bamboo ber/PLA composites compared to untreated bamboo ber/PLA composites with 30 wt% ber content. The toughness of the short ber reinforced composites can be inuenced by a number of factors, such as the intrinsic properties of the matrix, the ber volume fraction, and interfacial bond strength. Therefore, strong interactions between the hydroxyl groups of biobers and the coupling agents are needed to overcome the incompatibility problem. In doing so, the impact, tensile and exural strengths of biober reinforced composites can be increased. 6.4. Summary Tensile, exural and impact properties are the most commonly investigated mechanical properties of natural ber reinforced plastic composites. Impact strength is one of the undesirable weak points of these materials in terms of mechanical performance. Besides these tensile, exural and impact properties, the long-term performance (creep behavior), dynamic mechanical behavior, compressive properties are also investigated for natural ber composites. To improve performance to the desired level, still much work is to be done considering ber processing, non-linear behavior, bermatrix adhesion, ber dispersion, composite manufacturing with optimized processing parameters. 7. Development and future trends of biocomposites The advanced natural ber reinforced polymer composite contributes to enhancing the development of
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biocomposites in regards of performance and sustainability. Biocomposites have created substantial commercial markets for value-added products especially in automotive sector. However, in order to be able to expand into other markets, such as commercial construction and consumer goods, composites need to achieve high-quality performance, serviceability, durability, and reliability standards. In recent years, the major advancement lies within the establishment of nanotechnology (i.e., reinforcing as well as producing nanocrystalline cellulose from natural bers). Natural bers consist of approximately 3040% cellulose and about half of that is crystalline cellulose. The nanocrystalline cellulose may be only one-tenth as strong as carbon nanotubes but it costs 501000 times less to produce. Wood pulp has often been used as the starting material for research on nano cellulose production. In the literature there are reports of cellulose nano/microbril extraction from diverse non-wood sources including hemp bers [481,482], sugar beet pulp [483,484], potato pulp [485], swede root [486], bagasse [487491], sisal [492,493], algae [494], stems of cacti [495,496], banana rachis [497], ax bers [498,499], plantain [500], water hyacinth [501], bamboo [502], coir [503], pea hull [504], pineapple leaf [505], and wheat straw [506]. Alemdar and Sain investigated the reinforcing potential of composites comprising a starch-based thermoplastic polymer and cellulose nanobers obtained from agroresidues [507]. Cellulose nanobers were isolated from wheat straw by a chemi-mechanical technique and determined to have diameters in the range of 1080 nm and lengths of several thousand nanometers. Fig. 24 shows the structure of the wheat straw bers after the chemical treatment. These images visually suggest the partial removal of hemicelluloses, lignin and pectin after chemical treatment, which are the cementing materials around the ber-bundles. It is clear from the image that the average diameter of the bers is about 1015 m, which is lower than the average size of the ber bundles, 25125 m before chemical treatment. TEM image (Fig. 24b) for the nanobers obtained after the chemi-mechanical treatment. The mechanical treatment of the bers resulted in debrillation of nanobers from the cell walls and the TEM image of the nanobers shows the separation of these nanobers from the micro-sized bers. Alemdar and Sain [508] extracted MFC from wheat straw and soy hulls via mechanical treatment involving cryocrushing followed by disintegration and brillation. These authors found that almost 60% of the nanobers had a diameter within a range of 3040 nm and lengths of several thousand nanometers. Cryocrushing is an alternative method for producing nanobers in which bers are frozen using liquid nitrogen and high shear forces are then applied. When high impact forces are applied to the frozen bers, ice crystals exert pressure on the cell walls, causing them to rupture and thereby liberating microbrils. The cryocrushed bers may then be dispersed uniformly into water suspension using a disintegrator before highpressure brillation. A blend containing 10% cellulose nanobers obtained from various sources, such as ax bast bers, hemp bers,
kraft pulp or rutabaga and 90% poly(vinyl alcohol) was used for making nanober reinforced composite material by a solution casting procedure [509]. Both tensile strength and Youngs modulus were improved compared to neat PVOH lm, with a pronounced four- to ve-fold increase in Youngs modulus observed. Similarly, Wang and Sain [510,511] reported that soybean stock-based nanober-reinforced PVOH lms (up to 10% nanober content) demonstrated a two-fold increase in tensile strength when compared with lms without ller. With a higher loading of MFC, the relative enhancement of mechanical properties was even more remarkable. They also applied solid phase melt-mixing followed by compression molding to produce MFC-reinforced composites. In their study nanober was directly incorporated (up to 5 wt%) into PE and PP matrix using a Brabender mixer and an ethylene-acrylic oligomer emulsion was used as a dispersant. This work demonstrated that coating MFC bers with the dispersant improved the cellulose dispersion in these polymers. As a consequence, the mechanical properties of PP and PE nanocomposites were slightly improved when compared to pure matrices; however, this enhancement was not considered signicant. Sain and Bhatnagar [512] invented a method to obtain MFC from renewable feedstocks such as natural bers and root crops via cryocrushing of the pre-treated pulp with liquid nitrogen. The pulp was hydrolyzed at a moderate temperature of 5090 C and then both acidic and alkali extractions were performed. Taniguchi [513] utilized natural cellulose bers derived from different sources (such as cotton, hemp, wood pulp, seaweed, cereals, sea squirts, bacteria, etc.) for the production of MFC by brillating raw materials between rotating twin disks while adding shear stress in the vertical direction of ber long axes. Joseph et al. [514516] investigated the effect of microbrilation of oil palm ber on the dynamic mechanical properties of oil palm ber reinforced rubber composites. As technology improves for biocomposites reinforced with natural bers to provide enhanced material and product characteristics, the products will become more diverse and enter markets that as of yet are unexplored. Today natural ber reinforced biocomposites are found extensively in automotive sectors [517521]. By the time, biocomposite materials and associated design methods are sufciently mature to allow their widespread use, issues related to construction materials. The development of methods, systems and standards could see biocomposite materials at a distinct advantage over traditional materials. There is a signicant research effort underway to develop biocomposite materials and explore their use as construction materials, especially for load bearing applications. Burgueno et al. manufactured cellular beams and plates as load bearing structural components from hemp, jute and ax bers with unsaturated polyester resin [522525] for housing panel applications. The material and structural performance was experimentally assessed and compared with results from short-ber composite micro-mechanics models and sandwich analyses. It was demonstrated that cellular biocomposite components
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Fig. 24. SEM images of the wheat straw microbers (a), and TEM image (magnication 15,000) of the wheat straw nanobers (b). Adopted from [507]. Copyright 2008. By permission from Elsevier Ltd.
can be used for load-bearing components by improving their structural efciency through cellular material arrangements. Furthermore, it was veried that they could compete with components made from conventional materials. This research should continue in conjunction with development of conventional composite materials in order to provide a solution in the future to allow wider use of the bio composite materials by civil engineering applications. In the future, these biocomposites will see increased use in structural applications. Various other applications depend on their further improvements. But there are still a number of problems that have to be solved before biocomposites become fully competitive with synthetic ber composites. Biocomposites are sustainable and could be fully recyclable, but could be more expensive if fully bio-based and biodegradable and they are extremely sensitive to moisture and temperature. If a proper matrix is used, biocomposites could be 100% biodegradable, but their biodegradation can difcult to control. Biocomposites exhibit good specic properties, but there is high variability in their properties. Biocomposites showed non-linear mechanical behavior, poor long-term performance and low impact strength. Many of these weaknesses can and will be overcome with the development of more advanced processing of natural bers and their composites. However fully environmental superiority of biocomposites compared to synthetic ber composites is still questionable because of their relatively excessive processing requirements, which in turn consume more energy. Therefore, careful life-cycle assessment of biocomposites is essential in order to retain the main advantage in the process of developing high performance biocomposites. New markets will develop when these biocomposite products are more durable, dimensionally stable, moisture proof, and re resistant. Nanotechnology shows numerous opportunities for improving biocomposite products by providing nanotechnology-based coatings to increase water uptake, reduce biodegradation and volatile organic compounds and even ame resistance. The use of nanocrystalline cellulose is being explored for a variety of uses since it is
stronger than steel and stiffer than aluminum. Nanocrystalline cellulose reinforced composites could soon provide advanced performance, durability, value, service-life, and utility while at the same time being a fully sustainable technology. 8. Conclusions Biocomposites reinforced with natural bers and/or biopolymers have developed signicantly over the past years because of their signicant processing advantages, biodegradability, low cost, low relative density, high specic strength and renewable nature. These composites are predestined to nd more and more application in the near future, especially in Europe, where pressure from both legislation and the public is rising. Interfacial adhesion between natural bers and matrix will remain the key issue in terms of overall performance, since it dictates the nal properties of the composites. Many studies are examined, reviewed and highlighted in this review paper regarding the importance of the interface, the inuence of various types of surface modications, different types of matrices used for the composites, as well as fabrication methods, and the performance of composites. Further research is required to overcome obstacles such as moisture absorption, inadequate toughness, and reduced long-term stability for outdoor applications. In particular, different weathering conditions, such as temperature, humidity, and UV radiation all affect the service life of the product. The major detrimental effect of hygrothermal and UV exposure are property deterioration, discoloring and deformation. Signicant research is currently underway around the world to address and overcome the obstacles mentioned above. This effort to develop biocomposite materials with improved performance for global applications is an ongoing process. References
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Progress in Polymer Science 37 (2012) 15521596

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Progress in Polymer Science

Biocomposites reinforced with natural bers: 20002010

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

Notched charpy impact strength [mJ/mm]

4 3 2 1 0 Abaca-PP Flax-PP Jute-PP

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

Tensile strength Flexural strength

0 PLA PLA/abaca PLA/cellulose PP PP/abaca PP/cellulose

Tensile modulus Flexural modulus

0 PLA PLA/abaca PLA/cellulose PP PP/abaca PP/cellulose

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

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O. Faruk et al. / Progress in Polymer Science 37 (2012) 15521596

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