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Binoj2016 PDF
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
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)
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
Kλ
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.
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)]
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
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INSPIRE fellowship to pursue his PhD study. [13] Lai W L, Mariatti M, Mohamad Jani S. The properties of
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