Evaluation of linden fibre as a potential reinforcement material ...

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0(00) 1–18 ! The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav DOI: 10.1177/1528083714557055 jit.sagepub.com Article Evaluation of linden fibre as a potential reinforcement material for polymer composites Yasemin Seki 1 , Yolda¸ s Seki 2 , Mehmet Sarıkanat 3 , Kutlay Sever 4 , Cenk Durmu¸ skahya 5 and Ebru Bozacı 6 Abstract The aim of this study is to characterize linden fibres as a novel cellulose-based fibre to be used as a reinforcement material in composites and to investigate the adhesion property to unsaturated polyester. Up to now, there is no report regarding the poten- tial usability of linden fibre in composite applications. Linden fibres were extracted from the stem of a plant of Tilia rubra DC. subsp. caucasica (Rupr.) V.Engl. Characterization of linden fibres was studied by Fourier transform infrared, X-ray photoelectron spectros- copy, thermogravimetric analysis, X-ray diffraction analysis, tensile and pull-out tests. Morphological properties of the fibres were observed through scanning electron and optical microscopes. Initial degradation temperature of the linden fibre was reported to be 238 C. The tensile strength and the Young’s modulus of the linden fibres were calculated to be 675.4 45.7 MPa and 61.0 9.8 GPa, respectively. The interfacial shear strength of the linden fibre with unsaturated polyester matrix was computed as 26.15 2.27 MPa via pullout test. This study offers an alternative and eco-friendly reinforcement material which may have usability potential in polymeric composites. Keywords Fibre, composite, characterization, linden 1 Department of Textile Engineering, Dokuz Eylul University Buca, Izmir, Turkey 2 Department of Chemistry, Dokuz Eylul University, Buca, Izmir, Turkey 3 Department of Mechanical Engineering, Ege University, Bornova, Izmir, Turkey 4 Department of Mechanical Engineering, Izmir Katip Celebi University, C ¸ ig ˘li, Izmir, Turkey 5 Education Faculty, Science Education Program, Celal Bayar University, Manisa, Turkey 6 Department of Textile Engineering, Ege University, Bornova, Izmir, Turkey Corresponding author: Yolda¸ s Seki, Department of Chemistry, Dokuz Eylul University, Buca, Izmir, Turkey. Email: [email protected] at PENNSYLVANIA STATE UNIV on February 19, 2016 jit.sagepub.com Downloaded from

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Article

Evaluation of lindenfibre as a potentialreinforcement materialfor polymer composites

Yasemin Seki1, Yoldas Seki2, Mehmet Sarıkanat3,Kutlay Sever4, Cenk Durmuskahya5 and Ebru Bozacı6

Abstract

The aim of this study is to characterize linden fibres as a novel cellulose-based fibre to

be used as a reinforcement material in composites and to investigate the adhesion

property to unsaturated polyester. Up to now, there is no report regarding the poten-

tial usability of linden fibre in composite applications. Linden fibres were extracted from

the stem of a plant of Tilia rubra DC. subsp. caucasica (Rupr.) V.Engl. Characterization of

linden fibres was studied by Fourier transform infrared, X-ray photoelectron spectros-

copy, thermogravimetric analysis, X-ray diffraction analysis, tensile and pull-out tests.

Morphological properties of the fibres were observed through scanning electron and

optical microscopes. Initial degradation temperature of the linden fibre was reported to

be 238�C. The tensile strength and the Young’s modulus of the linden fibres were

calculated to be 675.4� 45.7 MPa and 61.0� 9.8 GPa, respectively. The interfacial

shear strength of the linden fibre with unsaturated polyester matrix was computed

as 26.15� 2.27 MPa via pullout test. This study offers an alternative and eco-friendly

reinforcement material which may have usability potential in polymeric composites.

Keywords

Fibre, composite, characterization, linden

1Department of Textile Engineering, Dokuz Eylul University Buca, Izmir, Turkey2Department of Chemistry, Dokuz Eylul University, Buca, Izmir, Turkey3Department of Mechanical Engineering, Ege University, Bornova, Izmir, Turkey4Department of Mechanical Engineering, Izmir Katip Celebi University, Cigli, Izmir, Turkey5Education Faculty, Science Education Program, Celal Bayar University, Manisa, Turkey6Department of Textile Engineering, Ege University, Bornova, Izmir, Turkey

Corresponding author:

Yoldas Seki, Department of Chemistry, Dokuz Eylul University, Buca, Izmir, Turkey.

Email: [email protected]

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Introduction

Currently, finite petroleum resources, the increasing concern towards environmen-tal issues, moreover regulations about carbon dioxide emissions, the availability ofimproved data on the properties and morphologies of natural fibres and recyclabil-ity of the materials have led to an increase in the use of natural fibre reinforced orfilled polymer composites in the many industries such as automotive and construc-tion [1–4].

Recent trends towards environmentally friendly polymer composites have beenfocusing on the use of cellulose-based natural fibres such as flax, jute, hemp, ramie,and sisal as reinforcement in the composites instead of glass fibres [5–7]. The nat-ural fibres have advantageous properties such as lightweight, high specific modulus,low density, low cost, non-toxicity, biodegradability, less health hazards, no abra-sion during processing, and absorbing CO2 during their growth [8,9]. The densityof natural fibres is lower (1.2–1.6 g cm�3) compared to glass fibre (2.4 g cm�3). Thisensures the production of lighter composites [10]. The use of large volumes ofsynthetic fibre-reinforced polymer composites in different industries despite theirhigh cost has led to disposal problems [4]. They are also very abrasive materialsthat lead to an increased wear of processing equipment such as extruders andmoulds. Glass fibres can cause problems with respect to health and safety. Forexample, natural fibres, unlike glass fibres, have less impact on the health of com-posite manufacturers (irritation of the skin, lung cancer) [11]. Glass fibres give skinirritations during handling of fibre products, processing and cutting of fibre-rein-forced parts [6]. These advantages and the disadvantages make natural fibres apotential reinforcement material in polymer composites.

As a result, natural fibres have attracted growing interest for industrial appli-cations, technical textiles, composites, pulp and paper, as well as for civil engin-eering and building activities [12]. Approximately 43,000 tonnes of natural fibreswere utilized as reinforcement in composites in the European Union (EU) in 2003[13]. The amount increased to around 315,000 tonnes in 2010, which accounted for13% of the total reinforcement materials (glass, carbon and natural fibres) in fibre-reinforced composites. It is forecasted that about 830,000 tonnes of natural fibreswill be consumed by 2020 and the share will go up to 28% of the total reinforce-ment materials [14].

Growing environmental awareness leads to focusing on new plant fibre forpolymeric composites. A fibre which can be used as a reinforcement in compositemanufacturing should have high tenacity, high flexural and impact strength basedon the application area. The main scope of using fibres as a reinforcement materialis to enhance mechanical performance of polymers. Additionally, the surface chem-istry and the surface morphology of the fibres should be compatible with polymersto provide high interfacial adhesion in composite system. Thus, many natural fibreshave been investigated. In recent times, the use of artichoke fibres extracted fromthe stem of artichoke plant was investigated as a potential reinforcement in poly-mer composites. The microstructure, chemical composition, and mechanical

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properties of artichoke fibres were studied and these fibres were represented asan alternative to synthetic fibres (i.e. glass) as reinforcement in composites [15].Besides, the potential of okra fibres extracted from the stem of a plant ofthe Malvaceae family as reinforcement in polymer composites was alsoexamined [16].

Ethnobotanically, linden fibres have been used for centuries in Turkey.Traditionally, it is used especially for rope making due to durability properties.In the Northeast part of Turkey, many villagers occupy with traditional beekeepingand they used big carved wooden barrel as a hive. They use linden ropes forcarrying these heavy hives. Scientifically, there has been no report on the Lindenfibres. Therefore, the purpose of this research is to characterize and to investigatethe mechanical performance of the Linden fibre as a novel cellulose-based fibre tobe used as a reinforcement material for composite materials. According to thisscope, the linden fibres were characterized by thermogravimetric analysis (TGA),Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS) andX-ray diffraction (XRD). The chemical composition and the fibre tensile propertieswere determined and also pull-out test was performed. Additionally, surfacemorphology of the linden fibres was observed by using scanning electron (SEM)and optical microscopes.

Material and methods

Materials

Linden tree, which is a member of Tiliaceae family, grows naturally in manyregions of Turkey. The used materials were collected from Efeler Village ofArtvin district located in the northeast part of Turkey. Plant materials were iden-tified according to Flora of Turkey and East Aegean Island [17]. Linden fibres(close, general and detailed views) used in this study were extracted from Tiliarubra DC. subsp. caucasica (Rupr.) V.Engl (Figure 1a–c). Polipol polyester 383-T (specific gravity: 1.11 g/cm3, viscosity brookfield: 950 cP), which is isophthalicacid type resin, was used as resin in the pull-out test.

Extraction process

The linden fibres are held together in the stems of the plant and in order to freethe fibres, fermentation process called water retting was applied [18]. Aftercollecting the fresh plant, the stems of the plants were retted for six weeks intap water without any enzyme. The fibres extracted from the stems of the plantswere washed with distilled water, combed, and dried in open air for aboutone week after the retting process. The average L/D ratio of the retted fibreswas 25/0.13 (mm/mm). The wettability of the fibres was determined by waterdrop test. Average disappearance time of water drops of linden fiber is43.85� 3.54 s.

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TGA experiment

TGA was conducted by using Perkin–Elmer Diamond TG/DTAanalyzer from 30�C to 600�C at a heating rate of 10�C/min under dynamicnitrogen flow.

FTIR analysis

FTIR analysis was carried out by using Perkin Elmer Spectrum BX-II. Prior toanalysis, KBr was dried at 80�C for 1 h. In order to prepare pellets for FTIRanalysis, 1mg of linden fibres was mixed with 100mg of KBr. After drying at80�C for 2 h, pellet was produced.

Determination of chemical composition

The fibre samples were oven-dried at 105�C for 4 h and kept in a desiccator beforethe chemical analysis for cellulose, hemicelluloses, and lignin. The details of meth-ods are given elsewhere [19,20].

Tensile testing

In order to determine the tensile properties (the tensile strength, the Young’smodulus, elongation at break) of the linden fibre, single fibre tensile tests wereperformed by using a universal testing machine (Shimadzu AUTOGRAPH AG-IS Series) with 100N loadcell at a contact speed of 0.1mm/min. The single fibrehaving a gauge length of 20mm was mounted on cardboard end tabs via aquicksetting polyester adhesive. The test was repeated eight times and the resultswere averaged.

Figure 1. The picture of the plant: (a) a close view, (b) a general view, (c) a detailed view.

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SEM observation

The surface morphology of the linden fibres was examined via SEM analysis byusing Quanta FEG 250 SEM (at an accelerating voltage of 7 kV). Before observa-tion, the fibres were gold-coated via Emitech K550X automatic sputter coater.

XPS analysis

It is known that XPS is utilized to investigate the surface chemistry of materials. Inorder to determine distribution of chemical elements and the amount of functionalgroups on the surface of linden fibres, XPS analysis of the linden fibres was carriedout by using Techno Scientific Al-Ka X-Ray Photoelectron Spectroscopy. Thedevice was calibrated according to gold 4f7/2 and a 10�8mbar of vacuum wasapplied. Pass energy and energy step size were determined as 150 eV and 1 eV,respectively.

Pull-out testing

In order to characterize fibre–matrix adhesion, the bonding strength betweenmatrix and fibre was determined via pull-out test using ShimadzuAUTOGRAPH AG-IS Series universal testing machine. Pull-out test was per-formed after embedding of the fibres in the matrix for 180min at room tempera-ture. The gauge length was kept as 10mm with a cross-head speed of 0.1mm/min.The tests were carried out for five times and an average value was taken intoconsideration. The debonding force Fmax, the diameter d, and the embeddedlength of the fibres le were measured and the interfacial shear strength (IFSS) �dwas calculated from the following equation [21]

�d ¼Fmax

d�leð1Þ

Optical microscopy studies

Longitudinal and cross-sectional views of the linden fibres were taken by usingOlympus CX 21 optical microscope under 400�magnification to examine themorphology.

XRD analysis

XRD analysis of the linden fibres was performed by Rigaku D/MAX 200 XRDusing CuKa radiation. The diffraction intensity of the powdered sample was

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recorded between 3� and 90� (2y) at a scan speed of 4o/min. The crystallinity indexof the linden fibres was calculated by following Segal empirical method [22,23]

CI ¼ðI002 � IamÞ

I002� 100 ð2Þ

where I002 indicates the maximum intensity of diffraction of the (002) lattice peak ata 2y angle between 22� and 23�, which represents both crystalline and amorphousmaterials. Iam is assigned to the intensity of diffraction of the amorphous material,which is taken at a 2y angle between 18o and 19o where the intensity is at a min-imum value [22,24].

Results and discussion

TGA

Thermal decomposition profile for the linden fibres is given in Figure 2. TGAparameters are obtained by using TG, DTG, and D2TG curves, as revealed byYao et al. and Grønli et al. [25,26]. The weight loss up to 110�C due to waterevaporation is less than 1% due to which linden fibres contain low water content. Itis known that hemicellulose in the fibres is mainly responsible for moisture absorp-tion; but accessible cellulose, amorphous cellulose, and lignin also contribute tothis process [27]. From the chemical analysis, it is observed that hemicellulose

Figure 2. TGA curves; weight loss, 1st and 2nd derivative of the weight loss vs. temperature for

the linden fibre.

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content of the Linden fibre is quite low. The initial degradation temperature(Tinitial) is presumed to correspond to a solid mass fraction equal to 0.975 [26].

Initial degradation temperature for linden fibre is obtained to be 238�C. As canbe seen from DTG curve of the linden fibres, a shoulder around 300�C is seen(weight loss is 17% until 300�C). This may mainly correspond to the thermaldepolymerization of hemicellulose and the cleavage of glycosidic linkages of cellu-lose [16]. It is probable that decomposition of high content of lignin (34%) in thelinden fibres takes place within the whole temperature range. The temperatureTpeak (Tp), at which the maximum decomposition rate is reached, is determinedas 337�C. From TG curve, it is obtained that the weight loss percentage corres-ponding to Tp is 42%. The extrapolated onset temperature of decomposition (To) isdescribed by extrapolating the slope of the DTG curve (up to zero level of the DTGaxis) in correspondence with the first local maximum in D2TG curve [25,26]. Finaldecomposition temperature was obtained to be 425�C. Besides, weight loss corres-ponding to major decomposition step until 600�C is about 64%. This step is mainlydue to decomposition of a-cellulose available in the linden fibres. Table 1 shows acomparison of thermal properties of some cellulose-based fibres. The linden fibresexhibit higher extrapolated onset temperature of decomposition than jute, hemp,bamboo, kenaf, cotton stalk, bagasse, and wood-pine fibres. Besides, the Lindenfibres also have a greater maximum decomposition temperature than the otherfibres as presented in Table 1. Weight loss value for the linden fibre is relativelylow in comparison with those of the other fibres in Table 1. In terms ofresidual char of the fibres in Table 1, the linden fibre has the greatest value. As aconclusion, it is worth reporting from TGA that the Linden fibres are stable untilaround 240�C.

Table 1. Thermal characteristics of the selected fibres and the linden fibre.

Sample To (�C) Tp (�C)

Weight loss

until Tp (%)

Residual char

(wt) (%) Reference

Jute 205 283 44 25.2a [25]

Hemp 205 282 38 24.6a [25]

Bamboo 214 286 45 20.5a [25]

Kenaf 219 284 43 22.4a [25]

Cotton stalk 222 293 50 17.1a [25]

Bagasse 222 299 54 20.4a [25]

Wood-Pine 230 312 59 14.9a [25]

Linden 243 337 42 36b In this study

aUntil 800�C.bUntil 600�C.

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FTIR analysis

The lignocellulosic fibre compounds containing cellulose, hemicelluloses, and ligninconsist of some oxygen containing functional groups (ester, ketone, and alcohol),alkenes, and aromatic groups [16,28]. As shown in Figure 3, a strong absorptionband was observed at 3418 cm�1 due to OH stretching and hydrogen bonds. Thebands at 3418 cm�1, 1265 cm�1 (due to C-O-C), and 1056 cm�1 (C-OH stretchingvibration of the cellulose backbone) indicate the polysaccharide components, lar-gely cellulose. C-H bending and OH deformation bands of alcohol group of cel-lulose are located at 1377 cm�1 and 1321 cm�1, respectively [29–31]. The band at2926 cm�1 and a shoulder at about 2850 cm�1 correspond to C-H stretching vibra-tion from CH and CH2 in cellulose and hemicelluloses [32]. This weak shoulderconfirms low content of hemicellulose in the linden fibres. C¼O stretching vibra-tion of linkage of carboxylic acid in lignin or ester group in hemicellulose is cen-tered at 1736 cm�1 [33]. C¼C stretching of aromatic ring of lignin appears at1506 cm�1. The band at 1654 cm�1 is assigned to the antisymmetric COO� stretch-ing or presence of water [30]. The band at 1428 cm�1 may be attributed to the CH2

symmetric bending in cellulose [34]. The absorption band at 1261 cm�1 may beindicative of C-O stretching vibration of the acetyl group in hemicellulose [35,36].A weak band detected at 1161 cm�1 corresponds to the antisymmetrical deform-ation of the C-O-C band. b-glycosidic linkages between the monosaccharides showa band at 893 cm�1 [16,35]. The aromatic C-H out-of-plane vibration in lignin islocated at 833 cm�1 [30]. The lateral crystallinity index of the fibres is obtained byusing absorption values at 1428 cm�1 and 893 cm�1 attributed to the CH2 symmet-ric bending mode and C1 group frequency, respectively [30,37]. The baseline-cor-rected absorptions at 1428 cm�1 and 893 cm�1 correspond to crystalline andamorphous cellulose structures, respectively [32,38–40]. The Lateral order index(LOI) shows the order of crystallinity rather than the amount of crystalline

Figure 3. FTIR spectrum for the linden fibre.

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cellulose relative to the amorphous components [40]. LOI for the linden fibre wascomputed as follows

LOI ¼a1428 cm�1

a893 cm�1ð3Þ

where a1428cm�1 and a893cm�1 correspond to the absorbencies at 1428 cm�1 and893 cm�1, respectively [37]. The LOI value for the linden fibre was calculated as0.96. This value is greater than those of althaea and ferula fibres (althaea fibre:0.79, ferula fibres: 0.70).

Chemical composition

The contents of basic constituents of the fibres such as cellulose, hemicelluloses, andlignin were obtained to be 61.8%, 4.2%, and 34.0%, respectively. Cellulose contentof the linden fibres is comparable with those of abaca, agave Americana, and flaxfibres [19,41,42] However, lignin content of the linden fibres is higher than those ofthe other cellulose-based fibres. The lignin contents of abaca, agave Americana,hemp, and jute fibres are revealed to be 4.9%, 8.5%, 4%, and 8%, respectively[19,20,41,43]. The high amount of lignin may explain moisture resistance behaviourof the Linden fibres [44]. This result is in accordance with TGA shown in Figure 2.

XPS analysis

Table 2 gives the atomic concentrations and O/C ratio of the linden fibres withrespect to XPS analysis. As can be seen in Table 2, C and O concentrations of theLinden fibres are 85.63% and 10.70%, respectively. O content of the Linden fibresis very low in comparison with luffa cylindrica and jute fibres which have O con-tents of 34.9% and 29.7%, respectively. O/C ratio of the linden fibres is calculatedto be 0.13, which is lower than the other fibres such as flax (0.156) [45], jute (0.46)[20], and luffa cylindrica (0.54) [46]. A low O/C ratio can be used as an indicative ofhydrophobicity of the fibres [47]. Therefore, moisture resistance property of thelinden fibres can be confirmed by relatively low O/C ratio.

Deconvulation analyses of C1s and O1s were performed to determine the func-tional groups and their concentrations on the surface of the linden fibres. The peakassignments and the concentrations of related functional groups are given inTable 3 and their curves are presented in Figure 4. As can be seen in Table 3,the high proportions for the linden fibres belong to C-C/C-H and O-C groups. It is

Table 2. Surface chemical composition of the linden fibre.

C (%) O (%) Ca (%) O/C

Linden fibre 85.63 10.70 3.7 0.13

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noteworthy that proportion of C¼O groups is 36.2% and this value is relativelyhigh as compared with jute (6.1%) and luffa cylindrica fibres (4.6%). Carbonylgroups mainly exist in lignin and also present in hemicellulose components inlignocellulosic fibres. This high concentration of carbonyl groups can confirm thehigh amount of lignin.

Tensile properties

Figure 5 shows tensile testing results, in terms of tensile strength versus strain, forlinden fibre. Tensile properties of linden fibre were determined and a comparisonwith the other plant fibres was made, as shown in Table 4. In this study, the tensilestrength and the Young’s modulus of the linden fibre were obtained as675.4� 45.7MPa and 61.0� 9.8GPa, respectively. Besides, the elongation atbreak of the linden fibres was determined as 2.95%� 0.20. It is interesting to notethat, the linden fibres have close values to hemp fibres for related tensile properties.The tensile strength, tensile modulus, and elongation at break of hemp fibres havebeen given as 690MPa, 70GPa, 2.0–4.0%, respectively [50]. It can also be empha-sized that the tensile strength and the Young’s modulus for the linden fibre are betterthan those for ferula communis and coir, as presented in Table 4.

Interfacial shear strength

The properties of fibre-matrix interface affect the mechanical properties of com-posite materials due to the role of fibre-matrix interface in transferring stress

Table 3. The concentration of functional groups on the surface of the linden fibre

[20,48,49].

C-C, C-H C-O C¼O O-C O¼C O-H

C1s O1s

eV 284.5 286.3 287.6 533.5 532.2 530.7

% 45.2 18.6 36.2 54.3 23.5 22.2

Figure 4. XPS spectra showing the deconvoluted C1s (a) and O1s (b) envelope for the linden

fibre.

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Figure 5. The stress–strain curve of the linden fibre.

Table 4. Tensile properties of linden fibre and other natural fibres.

Fibre

Tensile

strength (MPa)

Tensile

modulus (GPa)

Elongation

at break (%) Reference

Ferula 475.6� 15.7 52.7� 3.7 4.2� 0.2 [22]

Althaea 415.2� 11.5 65.4� 7.2 3.9� 0.1 [51]

Luffa 385� 11 12.2� 1.0 2.65� 0.05 [49]

Jute 400–773 10–30 1.5–1.8 [52]

Pineapple 180–748 25–80 1.6–3.2 [53]

Ramie 400–938 61.4–128 3.6–3.8 [22,52]

Flax 500–1500 27.6 2.7–3.2 [54]

Kenaf 930 53 1.6 [55]

Hemp 690 70 2.0–4.0 [56]

Banana 700–800 27–32 2.5–3.7 [52]

Abaca 756 31.1 2.9 [57]

Sisal 511–635 9.4–22 2.0–2.5 [58]

Piassava 76.9 2.93 10.45 [59]

Coir 95–220 2.5–6.0 13.7–51.4 [60]

Linden 675.4� 45.7 61.0� 9.8 2.95� 0.20 In this study

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between the fibre and the matrix. In order to transfer the load from matrix to fibre,which is also required for good performance, a strong fibre-matrix adhesion isnecessary [61]. Interfacial shear strength of the linden fibre-unsaturated polyestermatrix was obtained to be 26.15� 2.27MPa. Seki et al. [62] have determined IFSSvalue of Ferula Communis/unsaturated polyester as 16.21MPa. The IFSS valueobtained in the study is about 1.6 times greater than that of Ferula Communis/unsaturated polyester.

Optical microscopy studies

Figure 6 shows the longitudinal and the cross-sectional optical views of the lindenfibres. It can be seen from Figure 6 that impurities and non-cellulosic materials arepresent on surface of the linden fibres. In addition, the linden fibres exist as abundle of elementary fibres or cells because one elementary fibre seems to beseparated from the bundle in longitudinal view of the linden fibres in Figure 6.The linden fibres have polygonal cross-sectional shape which can vary notablyfrom irregular shape to reasonably circular.

SEM observation

SEM micrographs of the linden fibres are depicted in Figure 7(a and b). Figure 7(a)shows that the structure of the linden fibres includes several elementary fibres (orcells) bonded with non-cellulosic materials along the fibre axis, which is also deter-mined in optical images of the fibres. It is clearly seen that surface impurities arepresent on the surface of the linden fibres (Figure 7a). The diameter values of thelinden fibres vary in the range of 40–300 mm (Figure 7b). The average diameter ofthe linden fibres were roughly measured as 131.75 mm. This result is a consequence

Figure 6. Optical microscopy images of the linden fibres (400�): (a) the longitudinal image,

(b) the cross-sectional image.

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of the measurement of several ultimate fibres that exist in a bundle of the lindenfibres. As can be seen from SEM micrograph of the fracture surfaces of the lindenfibre (Figure 7c–d), the fibre showed brittle fracture behavior. The tensile strengthversus strain curve (Figure 5) shows brittle behavior of the linden fibre, with a lowstrain (3–5%), similar to other fibres, such as sisal [63], pineapple [64], andbanana [65].

XRD analysis

The XRD pattern of the linden fibres is shown in Figure 8. As can be seen fromFigure 8, the major crystalline peak of the linden fibres occurred at 2y¼ 16.7�. It isalso found that the linden fibres have diffraction peaks at 13.9�, 14.8�, 22.0�, and25.2�, which can be assigned to the typical diffractions of cellulose I. The crystal-linity index of the linden fibres is 53% (Figure 8). As compared with the other

Figure 7. SEM micrographs of the linden fibres: (a and b) general view and (c and d) fracture

surfaces.

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commonly used cellulose-based fibres, this value is higher than wrighitia tinctoriaseed fibre (49.2%) but lower than coir fibres (57%), ramie (58%), cotton (60%),jute (71%), flax (80%), and hemp fibres (81%) [22,35]. The cystallinity index of thelinden fibres is also lower than recently developed potential plant fibre, Althaeafibres (68%) [51]. This may be due to the high content of non-cellulosic materials ascompared with the other cellulosic-based natural fibres [50].

Conclusion

The contents of cellulose, hemicelluloses, and lignin of the linden fibres wereobtained to be 61.8%, 4.2%, and 34.0%, respectively. LOI value for the lindenfibres, obtained from IR analysis, was calculated as 0.96. XRD analysis showedthat the crystallinity index of the linden fibres was calculated as 53%. O/C ratio ofthe linden fibres was obtained to be 0.13 from XPS analysis. It may be said that thesurface of linden fibres contains non-polar components. The tensile strength andthe Young’s modulus of the linden fibres were 675.4� 45.7MPa and61.0� 9.8GPa, respectively. Interfacial shear strength of the linden fibre-unsatu-rated polyester matrix was computed as 26.15� 2.27MPa. Although the maximumdecomposition temperature of the linden fibres is obtained to be 337�C, the lindenfibres are stable until around 240�C. It is probable that linden fibres may be used asa reinforcement material for unsaturated polyester due to relatively good adhesionproperties and high thermal stability.

Funding

This research received no specific grant from any funding agency in the public,commercial, or not-for-profit sectors.

Figure 8. XRD pattern of the linden fibres.

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