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Journal of Bionic Engineering 13 (2016) 156–165

Morphological, Physical, Mechanical, Chemical and Thermal Characteriza-


tion of Sustainable Indian Areca Fruit Husk Fibers (Areca Catechu L.) as
Potential Alternate for Hazardous Synthetic Fibers

J. S. Binoj1, R. Edwin Raj1, V. S. Sreenivasan2, G. Rexin Thusnavis3


1. Department of Mechanical Engineering, St. Xavier’s Catholic College of Engineering, Nagercoil – 629003, India
2. Department of Mechanical Engineering, VV College of Engineering, Tisaiyanvilai – 627657, India
3. Department of Chemistry, St. Xavier’s Catholic College of Engineering, Nagercoil – 629003, India

Abstract
Natural fibers can play a major role in composite industry due to its renewable, biodegradable, and eco-friendly properties.
Areca Fruit Husk (AFH) is rich in fiber, but is wasted in large quantity from tobacco industries. Comprehensive characterization
of AFH fiber is done to examine its morphological, physical, mechanical, chemical and thermal properties. High cellulose
content of the fiber (57.35 wt%) provides better tensile strength (231.66 MPa) whereas the porous surface morphology (40.8 %)
ensures better bonding with the matrix. Moreover, the low density of the fiber (0.78 g·cm−3) makes it an attractive alternative for
hazardous synthetic fibers. The semi-crystalline nature and large crystalline size of the fiber reduce the water absorption char-
acteristics. The thermo gravimetric analysis confirms its stability up to 240 ˚C, which is higher than the polymerization tem-
perature. The results confirm the potential of AFH fibers as a reinforcement in bio-reinforced polymer composites for automo-
tive and structural applications.
Keywords: bio-reinforced polymer composites, Areca husk fibers, physical properties, chemical properties
Copyright © 2016, Jilin University. Published by Elsevier Limited and Science Press. All rights reserved.
doi: 10.1016/S1672-6529(14)60170-0

expensive and most importantly, potential natural mate-


1 Introduction
rials as replacement for harmful fibers in different en-
Application of natural fibers is getting momentum, gineering applications is the need for sustainable indus-
which drives us back to the golden eras of scientific trial development[9–11]. However their properties vary
inventions. Accessibility of such materials in bulk widely based on their chemical composition, aging,
quantities can alter the natural fiber market penetration. internal structure, density, micro fibril angle, cell di-
Recently, the use of biodegradable materials has been mensions, defects, etc., which need to be examined on
appreciated and attracted global attention[1]. Natural case-by-case basis.
fibers are ecofriendly, recyclable, low cost and low Areca is a monocotyledonous plant and belongs to
density with comparable mechanical properties[2–5]. palm species. This is a native of South or Southeast Asia
Fibers extracted from vegetable biomass, woodland and largely grown in India for its nuts, which are mostly
residues and farming deposits are rich in cellulose, wrapped in betel leaves for chewing and being spat out
hemicellulose, lignin, etc. and are termed as lignocellu- or swallowed[12,13]. It is a growing multi-million industry,
lose fibers[6]. Lignocellulose fibers are also called as even though there are apprehensions for its carcinogenic
plant/vegetable fibers which include fibers extracted potential. They belong to Arecaceae (arecoideae) or
from bast, foliage, fruit husk, kernel, timber, cereal Palmaceae (palms) family and have a scientific name,
straw, farmed excesses, lawn, etc.[7]. Usage of these Areca Catechu Linnaeus. They are perennial trees ex-
fibers as reinforcement for polymer matrix composites is posing attractive appearance and holding some thera-
gaining momentum due to its potential properties with peutic properties relative to cocos nucifera with a stem
sustainability[8]. Finding biodegradable, renewable, in- diameter of approximately 15 cm. They grow to a height

Corresponding author: R. Edwin Raj


E-mail: redwinraj@gmail.com
Binoj et al.: Morphological, Physical, Mechanical, Chemical and Thermal Characterization of Sustainable Indian Areca Fruit
Husk Fibers (Areca Catechu L.) as Potential Alternate for Hazardous Synthetic Fibers 157
of 30 m with 10 to 20 leaves on their top head side[14]. generally used for tobacco industry. However the husks
They flower in cluster and yield 30 – 50 nuts per spathe. covering the areca nuts are discarded after extracting the
They start to yield fruit after eight years and take 240 seeds. These discarded husks are collected from the
days to mature. The diameter of the nut varies from tobacco industry and soaked in water for five days. The
50 mm to 100 mm and each nut contains 2.5 g – 2.75 g of soaked husks are cleansed with running water every day
fiber on its outer shell covering. The effective life span for 5 – 10 times. Soaking process loosens the fibers and
of the tree is around 60 years[15]. The fruits are cut removes the dust particles[19–21]. They are then sun dried
opened to collect the nuts for further processing. The for three days to reduce the moisture content and
outer cover of the fruit is fairly spongy with juicy liquid brushed to extract the fiber strands for further process-
and contains coarser fibrous husk which can be easily ing[14,17]. Fig. 1 shows the collected AFH and the ex-
removed when dried[16]. Areca Fruit Husk (AFH) fiber tracted fibers.
potential is approximately estimated to be around
13,00,000 metric tons per year in India alone, which is 2.2 Characterization of AFH fiber
mostly discarded without any serious applications[17]. 2.2.1 Chemical study
Natural fibers have been used as raw materials for The major biochemical ingredients of AFH fibers
different applications and as reinforcing materials for such as cellulose, hemicellulose, lignin and wax content
polymer composite fabrication. Various researches are are determined using standard test procedures[8,18]. The
going on in natural fibers such as bamboo, coir, jute, flax, ash content is quantified as per ASTM E1755-61 stan-
sun hemp, ramie, kenaf, roselle, straw, rice husk, sugar dard, whereas the moisture content is determined by
cane, grass, raphia, papyrus, pineapple leaf, etc.[18]. They drying the sample in an oven at 104 ˚C for 4 hours.
are presented as an alternative to synthetic fibers due to
their comparable mechanical and physical properties 2.2.2 Anatomical study
along with special features such as biodegradability, Coarse and fine fibers are separated and examined
renewability, availability, low density, and low cost. by micro technique to analyze its internal structure. The
They are finding increasing applications in automotive fruit husk fiber bundles are cut into small pieces (10 mm
and packaging industries due to their specific stiffness × 10 mm) and dipped in FAA solution (5 mL formal
and strength[4]. Knowledge of the physical, mechanical, dehyde + 5 mL acetic acid + 90 mL of 70 % ethyl alcohol)
chemical and thermal properties of natural fibers is re-
quired in order to optimize the performance of polymer
composites[4].
Huge quantities of AFH fibers are discarded from
the tobacco industries without any appropriate usage
causing bad odor and environmental problems. In the
present work, the physical, anatomical, chemical, me-
chanical and thermal properties of AFH fibers are de-
termined for evaluating the feasibility of using AFH
fibers for valuable purposes. The phenomenal specific
strength of this fiber along with its thermal stability
favors this material as a viable alternate reinforcement
for polymeric matrix composites. The comprehensive
characterization of AFH fibers opens an opportunity to
use the discarded agro-waste as a replacement for haz-
ardous synthetic fibers.

2 Materials and methods


2.1 Material collection and extraction of fibers Fig. 1 (a) Photograph of Areca fruit husk waste heap from agro
The areca palm seeds known as ‘areca nuts’ are industry and (b) photograph of extracted AFH fiber.
158 Journal of Bionic Engineering (2016) Vol.13 No.1

for 24 h in order to preserve the specimens. They are procedures. The randomly sectioned fibers embedded in
then desiccated by tertiary butyl alcohol series and em- paraffin blocks and AFH fibers are analyzed in polarized
bedded in paraffin blocks. Then the blocks are sectioned microscope to determine the diameter and cross sec-
into 10 µm – 12 µm size slices using a rotary microtome tional area through image processing software. The
rotated in clockwise direction. They are then fixed to a density of the fibers is determined on mass volume basis
glass slide and stained with safranine and toluidine blue by filling the powdered dry sample and compressed
to enhance the visibility. The slides are then examined enough to squeeze out all air in the container of known
using polarized light micrograph at PARC (Plant volume. The weight of the container is recorded before
Anatomy Research Centre) (Nikon camera, Japan) to and after filling to know the fiber weight in order to
define the fiber anatomy. compute the fiber mass density. The linear mass density
of fibers, which is the measure of fineness of the fibers,
2.2.3 FTIR analysis is estimated as per ASTM D 1577-07 standard by
Fourier Transform Infrared analysis is done on the weighing 100 fibers with each 60 mm in length. From
fibers using Perkin Elmer Spectrum RXI - FTIR Spec- the mass density and linear mass density of fibers, the
trometer (UK) with a scan rate of 32 scans per min to diameter of fibers is estimated in mm as:
define the presence of free functional groups. Extracted
Lf
fibers are sliced into smaller units using scissors and Df = , (1)
crushed to fine powder using mortar and pestle. The fine 9000 × M d × 0.7855
particles are then mixed with potassium bromide (KBr) where Df represent the diameter of fiber, Lf represent the
and pelletized by applying pressure. FTIR spectrum is linear mass density of fiber, which is in denier (mass in
applied at normal conditions under transmittance mode grams per 9000 m length of fiber) and Md is the mass
with resolution of 2 cm−1 and in the wave number range density which is in grams per cubic centimeters.
from 500 cm−1 to 4000 cm−1. Porosity is the ratio of total surface area of the fiber
lumens to the entire surface area of the fiber in sectional
2.2.4 Morphological study view[8]. It is determined by processing the polarized light
The surface morphology of AFH fiber is examined micrograph image using ‘Image J software’ at randomly
in CARL ZEISS SMART (MA and LS series) scanning selected 10 sectional views and averaged. Similarly, the
electron microscope, (EVO 18.15.66, Germany) with an cell dimensions such as thickness of middle lamellae,
accelerated voltage of 20 kV. The AFH fibers are fixed primary wall, secondary wall and fiber lumen are also
on aluminum stubs by steel tape and coated with gold to estimated using image analysis.
make the surfaces conductive, so as to avoid electron The mechanical properties of the fiber is estimated
charge gathering. by conducting tensile test as per ASTM D3822-07
standard in INSTRON (5500R) universal testing ma-
2.2.5 XRD Analysis chine with computer interface for data acquisition and
Areca powdered fibers are exposed to X-ray dif- control at 28 ˚C and relative humidity of 65%. Tests are
fraction to measure the crystallite size and to identify the conducted at a constant cross head speed of 5 mm·min-1
crystalline index. It is done in P-Analytical Xpert PRO for different Gauge Lengths (GL) varying from 10 mm
MPD diffractometer (UK) with monochromatic CuKα to 40 mm in steps of 10 mm. 20 samples are tested for
radiation for 2θ range from 10˚ to 80˚ with goniometer every gauge length to nullify the variation of results due
speed of 5˚·min−1. The settings of the generator read to uneven structure of natural fibers.
30 mA, 40 kV using Cu anode materials at a temperature
of 25 ˚C. 2.2.7 TGA analysis
The behavior of fibers for high temperature appli-
2.2.6 Physico-mechanical study cation is assessed by thermo gravimetric (TG & DTA)
The physical properties of the fiber such as di- analysis using Jupiter simultaneous thermo gravimetric
ameter, cross section area, density, porosity, and average analyzer (STA 409 PC, Netzsch, Germany) at Netzsch,
length are determined using appropriate ASTM standard Chennai. 10 mg to 20 mg of accurately measured
Binoj et al.: Morphological, Physical, Mechanical, Chemical and Thermal Characterization of Sustainable Indian Areca Fruit
Husk Fibers (Areca Catechu L.) as Potential Alternate for Hazardous Synthetic Fibers 159
crushed fibers are kept in alumina crucible and carefully tion capacity[24]. Lignin improves the rigidity and stiff-
instrumented using thermocouple to record the variation ness of the fiber by bonding the cell wall structures to-
in temperature with respect to time using Proteus ther- gether. It also helps in bonding with polymers when used
mal analysis software. To avoid oxidation effects, the as a reinforcement in polymer matrix composites[23].
process is done under nitrogen atmosphere with a flow Wax will affect the interfacial bonding of fibers
rate of 20 mL·min−1. The temperature is raised from with polymer matrix, but AFH fibers contains only
32 ˚C to 550 ˚C at a rate of 10 ˚C·min−1. 0.12 wt% of wax. Voids are present due to dimensional
disparity leading to moisture absorption which in turn
3 Results and discussion
affects the mechanical properties[24]. Moisture also in-
3.1 Chemical properties of AFH fibers creases the weight of the fiber and induces degradation.
Chemical composition of plant fibers varies among The moisture content of the fibers is very low at
species, and may even varies within different portions of 7.32 wt%. However, the ash content is 5.08 wt%, which
the same plant[22,23]. The chemical composition of the provides better firefighting ability and blocks sensitive
fiber influences its mechanical, moisture absorption, chemical groups from reaction, thereby improves its
morphological and bonding characteristics, which have thermal stability[24,25]. The chemical analysis shows the
direct impact on its application as reinforcement for absence of any environmental friendly content, which is
polymer composite fabrication[24,25]. The properties of needed for cleaner production practices in industries.
AFH fibers are listed and compared with other natural
fibers in Table 1[17,22–28]. AFH fibers are rich in cellulose 3.2 Anatomical analysis of AFH fibers
content with 57.35 wt%, which is higher than most of the The optical microscopic images of the sectioned
commonly used natural fibers. Lower hemicellulose AFH fibers are shown in Fig. 2, where fibers are em-
content is desirable, because higher content will degrade bedded in parenchymatous tissue. The thick and thin
its thermal stability and increases the moisture absorp- fibers are dispersed in the fruit husk with scattered

Table 1 AFH fiber properties are listed in comparison with other natural and synthetic fibers[17, 22–28].
Chemical properties Physical properties Mechanical properties
Fiber Hemi Tensile Young’s
Cellulose Lignin Wax Moisture Diameter Density Length Elongation
cellulose Strength modulus
(wt%) (wt%) (wt%) (wt%) (µm) (g·cm−3) (mm) (%)
(wt%) (MPa) (GPa)
Areca fiber 57.35–58.21 13–15.42 23.17–24.16 0.12 7.32 396–476 0.7–0.8 10–60 147–322 1.124–3.155 10.23–13.15
Coconut fiber 32–43.8 0.15–20 40 – 45 - 8 100–460 1.15–1.46 20–150 95–230 2.8–6 15–51.4
Palm fiber 60–65 - 21 – 29 - - 150–500 0.7–1.55 - 80–248 0.5–3.2 17–25
Cotton 82.7 5.7 - - - 10–20 1.5–1.6 15–56 287–800 5.5–12.6 7–8
Bagasse 55.2 16.8 25.3 - 8.8 10–34 1.25 0.8–2.8 290 17 1
Bamboo 26–43 30 21 – 31 - 8.9 14 0.6–1.1 2.7 140–230 11–17 -
Flax 71 18.6–20.6 2.2 1.5 7 10–25 1.5 10–65 345–1035 27.6 2.7–3.2
Kenaf 72 20.3 9 - - 1.4–11 - 12–36 930 53 1.6
Jute 61–71 14–20 12 – 13 0.5 12 25 – 200 1.3 0.8–6 393–773 26.5 1.5–1.8
Hemp 68 15 10 0.8 9 25 – 35 1.48 5–55 690 70 1.6
Ramie 68.6–76.2 13–16 0.6–0.7 0.3 9 10–25 1.5 18–80 560 24.5 2.5
Abaca 56–63 20–25 7–9 3 15 - 1.5 - 400 12 3–10
Sisal 65 12 9.9 2 11 7–47 1.5 0.8–8 511–635 9.4–22 2–2.5
Banana 60–65 19 5 – 10 - - 13–16 1.35 0.17 355 33.8 5.3
Pine apple 81 - 12.7 - 13 20–80 0.8–1.6 3–9 400–627 1.44 14.5
Curaua 73.6 9.9 7.5 - - - 1.4 - 500–1150 11.8 3.7–4.3
E-glass - - - - - 8 – 15 2.5 - 2000–3500 70 2.5
Carbon - - - - - 5 – 100 1.7 - 2400–4000 230–400 1.4–1.8
Aramid - - - - - 15 1.4 - 3000–3150 63–67 3.3–3.7
S-glass - - - - - - 2.5 - 4570 86 2.8
160 Journal of Bionic Engineering (2016) Vol.13 No.1

(a)
vascular bundle at the peripheral portion of a fiber
(Fig. 2a). The fiber diameter varies from 396 µm to Fiber cells
476 µm. Vascular bundle consists of xylem and phloem
distributed in the pericarp surrounded by sclerenchy-
matous fiber called bundle sheath, which is a protective Phloem
layer, which enhances the mechanical property. Vascular bundle
AFH Fiber has a honeycomb structure with thin
Xylem
lignified walls and fairly wide lumen (Fig. 2b). The cell Thick and thin fibers
structure consists of primary cell wall, secondary cell
[-----250µm-----]
wall, middle lamellae and cell lumen (Fig. 2d). The (16×)
dimensions of cell wall are measured by image proc-
essing technique using Image J software and are tabu-
lated in Table 2. Primary cell walls are made of cellulose
and the secondary cell walls contain lignin, which gives
the hardness to the fibers. Middle lamellae is the inter-
cellular layer which joins the adjacent cells. They are
made up of hemicellulose and lignin, whereas the central
portion of each cell contains free space to store water,
called as lumens. The density of the fiber is low to pro-
vide light weight structures with high specific strength.
(c)

3.3 FTIR analysis of AFH fibers


Fig. 3 illustrates the FTIR spectrum of AFH fibers.
Sharp and prominents known spectra are obtained in the
wavelength range from 1031.49 cm−1 to 3354.29 cm−1.
Fine and strong peaks are seen at 1031.49 cm−1, 1238.55
cm−1, 2852.01 cm−1, 2921.62 cm−1 and 3354.29 cm−1
indicating the presence of strong and broad -C-OH
stretching vibration of cellulose, which are raised due to
the presence of polysaccharide components (i.e. largely
cellulose)[29]. These peaks are also an indication of the (10×)
occurrence of strong and broad -C-O stretching, which is (d)
the alcohol groups of cellulose[30,31]. Similarly, they also
suggest the existence of strong carboxylic acid with
-C=O stretch[31]. Peaks formed between 1512.83 cm−1 Cell lumen

Primary
Table 2 Tested physical properties of AFH fiber wall

Property Value
Primary wall thickness (nm) 1074±113 Secondary wall
Secondary wall thickness (nm) 402±74
Middle
Middle lamellae thickness (nm) 671±53 lamellae
Cell lumen thickness (nm) 3462±223
[-----70µm-----]
(50×)
Diameter of the fiber (µm) 396–476
Fig. 2 Anatomical and physical characterization of AFH fibers. (a)
Colour of the fiber Dark brownish
Sectional view of AFH fibers using optical microscope (16×); (b)
Fineness of the fiber (tex) 125 fiber diameter calculation using Image J software in sectional
Density of the fiber (g·cm−3) 0.7–0.8 position (10×); (c) fiber diameter calculation using Image pro
software in longitudinal position (10×) and (d) cell wall dimen-
Porosity of the fiber (%) 38.5–43.2 sion measurement using Image J software (50×).
Binoj et al.: Morphological, Physical, Mechanical, Chemical and Thermal Characterization of Sustainable Indian Areca Fruit
Husk Fibers (Areca Catechu L.) as Potential Alternate for Hazardous Synthetic Fibers 161

102
100
98
96
94
92
90
88
86
84
82
3500 3000 2500 2000 1500 1000
Wavenumber (cm−1)
Fig. 3 FTIR spectrum of the given AFH fiber.

and 1547.79 cm−1 belong to lignin[8] and the one formed is determined for five samples using SEM image with
at 1642.52 cm−1 confirms the existence of hemicellu- image analysis technique by Image J software and the
lose[18]. The peak at 2852.01 cm−1 indicates the strong average value is 7.36˚ ± 0.54˚ (Fig. 4d). The MFA (α) is
alkyl saturated C-H stretching vibrations and (CH2) also estimated using common arc Eq. (2) for verification
methylene group[30]. The peak found at 2921.62 cm−1 and confirmation as 7.15˚ ± 0.73˚[29].
denotes the reduction of C-H stretch of alkyl and me- ΔL
thylene (CH2) group. Higher transmittance intensity ε = ln[1+ ]= − ln(cosα ), (2)
L0
between 3633.69 cm−1 and 3889.58 cm−1 predicts the
presence of hydrogen bonds and O-H stretching[18]. where ε is the strain, ΔL / L0 deformation in length and α
Fourier Transform Infrared (FTIR) spectra confirm the micro fibril angle (degree).
existence of chemical composition such as cellulose, MFA plays a major role in determining the me-
hemicellulose and lignin in the AFH fiber. chanical properties of the fiber where increase in prop-
erties are reported for lower MFA[35,36]. The microfibril
3.4 Morphological properties of AFH fibers is also a primary factor which ensures smooth stress
Surface disparities may occur on fibers due to har- transfer from matrix to fiber in composite structure[29].
vesting technique, removal process, fiber maturity, eco-
logical influence, nature of soil variety, etc. Therefore, 3. 5 XRD analysis of AFH fibers
utmost care is given in sample preparation. The Scan- Fig. 5 shows the typical X-ray diffraction pattern of
ning Electron Microscopic (SEM) image of the extracted powdered AFH fiber sample. A single broad feature with
AFH fibers is shown in Fig. 4c. The surface of the fiber incoherent scatter is obtained for AFH fiber at
looks very rough with numerous slots and grooves, 2θ = 20.12˚ indicates that the fiber is semi-crystalline in
which enhances wettability and promotes bonding when nature[5,8,29,34,37]. This may be attributed to the interac-
it is used as an reinforcement for polymer composites tion between hydroxyl and carbonyl groups present in
(Figs. 4 a and 4b)[32]. fiber structure which could have led to intercalation of
The lignocellulosic fiber surface at higher magni- cellulose in it[38]. The Crystallinity Index (CI) of AFH
fications shows the presence of micro fibrils with the fiber is calculated using Eq. (3) and valued as
binding material (lignin) and parenchyma cells[33,34] 55.5%[39,40].
(Figs. 4b and 4c). The perforated deep structure on the
I c − I am
fiber surface called as trichomes also enhances me- CI = × 100%, (3)
Ic
chanical bonding between the fiber and the matrix[16].
Micro Fibril Angle (MFA) is the angle between direc- where Ic and Iam are the intensity of crystalline and
tions of helical winding of cellulose microfibrils in S2, amorphous peaks respectively. The CI value of AFH
secondary layer and axis of cell wall. Micro fibril angle fibers is somewhat near to that of other reported natural
162 Journal of Bionic Engineering (2016) Vol.13 No.1

fibers such as oil palm fruit fiber (34.1%)[41], cotton fruit


fiber (60%) and wrighitia tinctoria seed fiber (49.2%)[8].
The crystallite size (L) of AFH fibers is estimated
using Scherrer’s Eq. (4) and found to be 7.9 nm[8].


L= , (4)
β cosθ
where K is the dimensionless shape factor (0.89), β the
peak’s Full Width Half Maximum (FWHM), λ the
wavelength of the radiation (m) and θ is the Bragg angle
(deg). The crystalline size of AFH fiber is higher than
other natural fibers such as cotton (5.5 nm), corn stalk
(3.8 nm) and flax (2.8 nm)[8]. Large crystalline size will
reduce the water and chemical absorption capacity of the
fibers when reinforced in polymer composite.

3.6 Physico-mechanical properties of AFH fibers


Physical properties of the fibers such as diameter,
density, fineness and porosity are determined before
subjecting them to mechanical testing. The embedded
AFH fiber samples in sectional position are observed in
optical microscopy to determine the average diameter
and porosity of the fiber using Image J software (Fig. 2b).
The average diameter of the fiber obtained through op-
tical microscopy of samples is (0.4285±0.018) mm. AFH
fibers are also observed in longitudinal position using
polarized light micrograph to determine the average
diameter by Image-pro software (Fig. 2c). The average
diameter of the fibers obtained through polarized light
microscopy is (0.4349±0.034) mm. Randomized fiber
samples are powdered and filled in a known volume
container of cylindrical shape and weighed to determine
the mass density as (0.7839 ± 0.021) g·cm−3. The fineness
of the fibers or otherwise denoted as linear mass density
Fig. 4 SEM image of AFH fiber : (a, b) Horizontal view (100×,
500×), (c) Vertical view (250×) and (d) Micro fibril angle calcu-
of the given sample is 1125 grams per 9000 m length of
lation using Image J software. the fibers. From these densities the diameter of the fibers
is determined for cross verification using Eq. (1) as
450
0.4505 mm. The surface porosity of the samples are
400
analyzed by image processing using Image J and found
350
that the porosity varies from 38.5 % to 43.2 %, with
Intensity (cps)

300 average porosity of 40.8 %.The physical properties of the


250 fiber is tabulated in Table 2.
200 Low density fibers with better mechanical proper-
150 ties are favored for light weight composite applications in
100
10 15 20 25 30 35 40
automobiles and aviation sectors. The mechanical prop-
2θ (deg) erties of any natural fiber depend on its species, growing
Fig. 5 XRD spectrum of the given AFH fiber. condition and its chemical composition such as the
Binoj et al.: Morphological, Physical, Mechanical, Chemical and Thermal Characterization of Sustainable Indian Areca Fruit
Husk Fibers (Areca Catechu L.) as Potential Alternate for Hazardous Synthetic Fibers 163
presence of cellulose, hemicellulose and lignin[16,23,42]. 20 Table 3 Tabulation of mechanical properties of AFH fiber tested
with ASTM standard procedures
samples are tested for each gauge length ranging from 10
mm to 40 mm in steps of 10 mm using INSTRON Gauge Tensile Young’s
Strain to Diameter
length strength modulus
failure (%) (mm)
(5500R) universal testing machine and the results are (mm) (MPa) (GPa)
tabulated in Table 3. It can be noted that, as the gauge 10 147.923±32 1.124±0.86 13.15±1.31 0.476±0.013
20 196.544±41 1.596±1.13 12.31±2.52 0.431±0.016
length increases, the physical structure of any natural
30 259.363±54 2.273±1.87 11.41±3.63 0.412±0.015
fiber also varies and the same has been reflected with
40 322.829±67 3.155±2.31 10.23±2.75 0.395±0.017
larger variation in tensile strength. The higher strain
value and lower modulus provide better toughness to the and a mass reduction of 60% is occurred up to
fibers to resist failure. The physical and mechanical 360 ˚C[24,43]. Afterwards some small peaks are observed
properties of AFH fibers are compared with other natural in DTG curve at 390 ˚C, 420 ˚C and 440 ˚C which relate
and synthetic fibers and are presented in Table 1. The to pyrolysis, decomposition and degradation of lignin
average specific strength of AFH fibers is 289.6 kJ·kg−1. respectively[44].
The physical and mechanical properties of AFH fibers The apparent activation energy Ea is calculated to
are significant enough to be used as a reinforcement in know the kinetic parameter of AFH fibers using the
polymer composites. Broido’s Eq. (5)[8,45,46].

3.7 Thermal properties of AFH fiber 1 E 1


ln[ln[ ]]= − ( a )[( )+k ], (5)
TG and DTG curve of the powdered AFH fiber y R T
samples is shown in Fig. 6a. Minor weight loss is ob- where R is universal gas constant (8.314 J·mol−1K−1), T
served up to 100 ˚C due to the evaporation of moisture temperature in Kelvin, y normalized weight (wt/wo), wt
content in the fibers. No appreciable drop in weight is weight of the sample at any time t, w0 initial sample
witnessed until 240 ˚C, which signifies good thermal weight and k Boltzmann’s constant (1.3806×10−23J·K−1).
stability of the fibers up to that temperature. As the The kinetic activation energy for the given AFH
temperature increases beyond this value, depolymeriza- fibers is calculated from Broido’s plot (Fig. 6b) drawn
tion and degradation of hemicellulose and cellulose start with ln[ln(1/y)] against (1/T) K as Ea = 64.54 kJ·mol−1,
which is within the specified range for natural materials
(60 kJ·mol−1 – 170 kJ·mol−1). This value is lesser than
that of Prosopis juliflora bark fibers (76.72 kJ·mol−1) and
DTG (%·min−1)

Cissusquadrangularis root fibers (74.18 kJ·mol−1), which


TG (%)

indicates AFH fibers have better thermal stability to


withstand polymerization process temperature in poly-
mer composite manufacturing[29,46].

4 Conclusion
Finding viable alternate reinforcement for harmful
carcinogenic synthetic fibers in polymer composite in-
dustry is essential for eco-friendliness. In this work,
novel, AFH fibers discard from tobacco industrial waste
ln[ln(1/y)]

are comprehensively characterized. The presence of rich


cellulose (57.35 wt%) confirmed through FTIR analysis
and low wax (0.12 wt%) content with rough surface
morphology ensures better strength and bonding. The
low density of AFH fibers (0.78 g·cm−3) and moderate
tensile strength provide enough specific strength for
Fig. 6 (a) TG – DTG curve of the given AFH fibers and (b) light weight applications. The high crystalline index and
Broido’s plot of the given AFH fibers. crystalline size of the fibers ensure better water and
164 Journal of Bionic Engineering (2016) Vol.13 No.1

chemical absorption characteristics. The thermo-gra- natural product based agents derived from industrial plants
vimetric analysis confirms the fibers ability to withstand in textile applications-a review. Journal of Cleaner Produc-
polymerization process temperature without degradation, tion, 2013, 57, 2–18.
thus bringing hope for AFH fibers as a potential rein- [11] Kidalova L, Stevulova N, Terpakova E, Sicakova A. Utili-
forcement in polymer composites. zation of alternative materials in lightweight composites.
Journal of Cleaner Production, 2012, 34, 116–119.
Acknowledgment [12] Lai W L, Mariatti M. The properties of woven betel palm
The first author thanks Department of Science and (areca catechu) reinforced polyester composites. Journal of
Technology, Government of India for providing Reinforced Plastics and Composites, 2008, 27, 925–935.
INSPIRE fellowship to pursue his PhD study. [13] Lai W L, Mariatti M, Mohamad Jani S. The properties of
woven kenaf and betel palm (areca catechu) reinforced un-
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