Structural, Chemical, and Multi-Scale Mechanical Characterization of Waste Windmill Palm Fiber (Trachycarpus Fortunei)
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Li et al. J Wood Sci (2020) 66:8 https://doi.org/10.1186/s10086-020-1851-z Journal of Wood Science ORIGINAL ARTICLE Open Access Structural, chemical, and multi-scale mechanical characterization of waste windmill palm fber (Trachycarpus fortunei) Jing Li1,2,3, Xuexia Zhang4, Jiawei Zhu2,3, Yan Yu4 and Hankun Wang2,3* Abstract This study investigated the structural, chemical, and multi-scale mechanical properties of windmill palm (Trachycarpus fortunei) leaf sheath fber, which were frequently wasted. Signifcant variation was observed in fber diameter and cross-sectional morphology among diferent layers in a single leaf sheath, whereas the chemical composition, rela- tive crystallinity index, and the microfbrillar angle (MFA) of palm fbers were almost the same among diferent layers. Windmill palm fbers had low cellulose contents (34.70–35.5%), low relative crystallinity index (45.7–49.2%), and high MFA (38.8°–29.4°), resulting in low strength and modulus, but high failure strain under tensile load. The tensile fracture surface of windmill palm fbers was assessed through SEM studies and its ductile fracture was confrmed, which can potentially enhance the toughness of composites when used as reinforcement material. Nanoindentation was carried out among diferent leaf sheath layers, and the results showed the modulus and hardness values of windmill palm fb- ers are in the same range as other plant fbers. The experimental results may help guide selection of suitable reinforc- ing fbers for use in composites in diferent applications. Keywords: Windmill palm fber, Fiber morphology, Mechanical properties, Nanoindentation Introduction Windmill palm (Trachycarpus fortunei) is the most Over the last two decades, there has been a growing widely cultivated species at the latitudinal palm range industrial interest in the development of lignocellulosic margin, and distinguished by its large and fan-shaped natural fbers as replacements for glass or other tradi- leaves [5]. Every year, a portion of the leaves of the palm tional reinforcement materials used in composites [1]. dries out to form a mesh of coarse and brown leaf sheath Natural fbers composites ofer advantages of biodegra- fber that clasps the tree trunk, making it appear to be dability, good accessibility, fast renewability, high spe- wrapped in burlap [6] (Fig. 1a). Te palm leaf sheath fber cifc properties, and low cost [2, 3]. However, a better is considered an abundant agricultural byproduct due to understanding of the detailed morphology, structural, the necessary regular pruning process of the palm tree by and mechanical properties of natural fbers is essential removing loose mats to keep the tree attractive and safe. for evaluation of their potential as reinforcing materials Currently, due to their high durability and strength char- in composites and optimization of the service life perfor- acteristics, palm fbers are used to make a variety of by- mance of composites [4]. products such as mattresses, sofas, marine ropes, sacks, and traditional raincoats [7]. However, these applica- tions only utilize a small percentage of the total material produced, and the majority of the material is discarded *Correspondence: [email protected] directly as waste, causing serious environmental prob- 2 Department of Biomaterials, International Center for Bamboo lems [8]. Te possible use of palm fbers for composite and Rattan, Beijing, People’s Republic of China Full list of author information is available at the end of the article © The Author(s) 2020. This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creat iveco mmons .org/licen ses/by/4.0/. Li et al. J Wood Sci (2020) 66:8 Page 2 of 9 To facilitate reliable use of palm fber in composites, a detailed investigation was performed of the mechanical properties of windmill palm fbers, separated from the three layers of leaf sheath, in relationship to their chemi- cal composition and structural properties. First, the mechanical properties of palm fbers were determined at two scales: tensile tests at the fber scale and nanoin- dentation tests at the cell wall scale. Next, microscopy (SEM) observation and X-ray difraction were conducted to investigate morphology and structure (microfbril- lar angle and relative degree of crystallinity), followed by chemical composition analysis. Finally, the results were considered in a detailed assessment of the relationships between the physical, chemical, and mechanical proper- ties of the fber. Materials and methods Sample preparation Windmill palm tree trunk covered by leaf sheath was obtained from Anhui province, China (Fig. 1a). Te leaf sheath fbers were mechanically separated from the Fig. 1 Photograph of a windmill palm tree covered with leaf sheath; b leaf sheath; c a small piece of leaf sheath showing the petiole (Fig. 1b), and then washed with distilled water arrangements of diferent layers of fber bundle, with inserted images to remove impurities and dust and further air-dried to showing the schematic view of fber arrangement remove excessive water and moisture. Ten, the cleaned leaf sheath was sorted into three layers, namely the outer, middle, and inner layers, according to their diameters reinforcement may provide a strategy for the efcient uti- and orientations (Fig. 1c). Comparison of sample prepa- lization of these waste fbers. ration of diferent plant fbers is summarized in Addi- Each palm leaf sheath is composed of a middle layer tional fle 1: Table S1. of coarse fbers which is sandwiched between two layers of fbers with smaller diameters. Tere have been only preliminary studies of palm leaf sheath fbers. Zhang Morphological and chemical analysis et al. [9] revealed a unique structure of palm fber with Te longitudinal and transverse surface morphology of sub-cylindrical shape containing abundant fber cells in the palm fber were investigated through SEM (XL30, the cross section and Si-dots on the surface. Previously, FEI, USA) operating at 7 kV. Te tensile fracture surface the mechanical properties of palm fber were mainly of the palm fbers was also analyzed. Before SEM obser- determined through monotonic tensile tests. Palm fber vation, the samples were sputter-coated with a thin layer exhibits excellent elongation properties, which is able to of Pt using an Edwards Sputter Coater. tolerate signifcantly higher stain than other natural fb- Te diameter and length of each palm fber and ele- ers [10]. Chen et al. [11] investigated the infuence of the mentary fber were measured with a digital biological chemical treatment of windmill palm fbers on its ten- microscope (XTS20G, Fukai Ltd., China). In order to sile properties, and found that alkalized fbers possessed extract elementary fber, palm fbers were chemically higher tensile properties than untreated fbers. Neverthe- treated using a mixture solution of hydrogen peroxide less, none of these studies examined the potential vari- and glacial acetic as described by Yu et al. [13]. For meas- ation in the physical and mechanical properties of palm urement of elementary fber cell wall thickness, sam- fber from diferent layers of the leaf sheath. Since there ples were embedded with Spurr resin and cut to obtain are three layers in each sheet of palm leaf sheath with smooth transverse section for SEM observation. some diferences in terms of fber morphology and tensile Te chemical composition (α-cellulose, hemicellulose, properties [12], it is important to assess the properties of lignin, and ash content) of the palm fbers in diferent leaf these individual layers for a more comprehensive evalua- sheath layers was analyzed in accordance with the Tech- tion of the use of palm fber as composite reinforcement nical association of Pulp and Paper industry (TAPPI) material. standards, as described by Khalil et al. [14]. Li et al. J Wood Sci (2020) 66:8 Page 3 of 9 X‑ray difraction and then measured with an image-processing software A Philips X-ray difraction system (X’pert Pro, PANa- (Image-ProPlus 5.0, Media Cybernetics, USA). lytical B.V., Almelo, NL) was used to evaluate both the microfbrillar angle (MFA) and relative crystallinity index Nanoindentation testing (CrI) of palm fbers. Before measurement, palm fbers of For nanoindentation testing, palm fbers were embed- the same layer were arranged closely to form a mat. Here, ded in Spurr resin and cured in a fat mold as previous evaluation of the entire fber was performed instead of described [13]. After curing, the embedded samples were examination of the powder samples that are commonly polished with a glass knife and a diamond knife to pre- used in order to preserve the internal structure of the fb- pare a smooth surface exposing a transverse section. Te ers [15]. Using Eq. (1), MFA of the palm fbers was deter- nanoindentation experiments were performed using a mined by application of the widely used 0.6T method Triboindenter (Hysitron Incorporation, USA) with a dia- [16]: mond Berkovich indenter (tip radius less than 100 nm). MFA = 0.6 × T, Te indentation procedure was performed under load (1) control using a three-segment load ramp: reaching the where T-value was determined as half the width of the peak load of 150 μN within 6 s, holding at the peak load peak obtained in azimuthal distribution (Additional for 6 s, and then unloading within 3 s.