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Materials Today: Proceedings 5 (2018) 28080–28088 www.materialstoday.com/proceedings

ICCMMEMS_2018

Tensile and flexural properties of areca sheath fibers

Ashok R. Banagara*, Srinivasa Chikkol Venkateshappab, Sakshi Shantharam Kamathc,
Basavaraju Bennehallic
a
Department of Mechanical Engineering, PES Institute of Technology, Shivamogga-577204, Karnataka, India
b
Department of Mechanical Engineering., GM Institute of Technology, Davangere-577006, Karnataka, India
c
Department of Chemistry, Alva’s Institute of Engineering and Technology, Mijar-574225, Karnataka, India
*Corresponding Author: Email: jnnashok@gmail.com

Abstract

In the current work, the effect of surface modifications of areca sheath fiber by chemical modifications such as alkylation,
permanganate treatment, benzoylation and acrylation on the tensile and flexural behavior of areca sheath was studied. Both the
surface modified and raw areca sheath fibers are studied in this investigation. It was found that the tensile and flexural strength
are greatly influenced by surface modifications. From this study, it is concluded that chemical treatment of areca sheath will
result in increasing the tensile strength and will reduce the bending strength. Further, the tensile strength increases with the
surface modification and flexural strength decreases. It is concluded that the composites utilizing areca strands are promising
elective materials, which can be effectively utilized in automobiles, packaging industry, parcel/panel boards, and so on

© 2018 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of International Conference on Composite Materials: Manufacturing,
Experimental Techniques, Modeling and Simulation (ICCMMEMS-2018).

Keywords: Areca sheath; Tensile strength; flexural strength; Surface modification;

1. Introduction

The areca nut palm, Areca catechu L. is the source of the common masticatory nut, popularly known as areca nut.
Areca is a commercial/profit-oriented crop and is mainly grown southern parts of India [1]. Areca leaf sheath is shed
intermittently from the tree and it can be conceivably utilized as dry grub in ruminants. Around four lakh hectares of
land is under Areca development and it is evaluated that 500,000 tonnes of the potential availability of areca leaf
sheaths annually [2]. Each areca leaf sheath weighs about 250 g and the total annual availability of areca sheath is
about 0.14 million tons. Few of the studies have high lightened the measurable quantity of studies on arecanut,

2214-7853 © 2018 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of International Conference on Composite Materials: Manufacturing, Experimental Techniques,
Modeling and Simulation (ICCMMEMS-2018).
 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088 28081

areca nut husk, areca leaf sheath, etc. some of the physical properties available in the previous literature on areca
sheaths are depicted in table 1 [3] and some chemical properties of areca leaf sheath are presented in table 2 [4].
Presently areca sheath is utilized for making plates/containers, fuel and in treating the soil.
Table 1. Different physical properties of areca nut sheath [3]

Physical properties of areca nut sheath

Sl. No
Particulars Mean SD C.V
1 Length (mm) 812.24 152.77 18.80
2 Width (mm) 280.21 2.76 0.983
3 Thickness (mm) 3.92 1.03 26.36
4 Bulk density (g/cc) 0.76 0.03 3.94
5 Sphere-city 0.0124 0.00 13.73
6 Surface area (mm2) 148795 523020 35.15
7 Arithmetic mean diameter (mm) 365.46 64.92 17.76
8 Geometric mean diameter (mm) 10.03 0.59 5.85
Wet 55.61 3.65 6.56
9 Moisture content (%)
Dry 11.50 1.61 14.02
Table 2. Chemical Properties of Arecanut leaf sheath [4]

Sl. No. Property Areca Leaf sheath

1 pH 6 – 6.5
2 EC 1.6 – 1.78
3 Organic carbon (%) 60 – 63
4 Nitrogen (%) 0.65
5 Lignin (%) 38.68
6 Cellulose (%) 26.40
7 Hemicellulose (%) 16 - 17

Many of the naturally available fibers are used in many applications like housing insulation, manufacture of
significant worth included items, for example, cushion pads, handcrafts, and non-woven textures etc. as a raw
material, it is very difficult to use natural fibers in any products. The major drawback of utilizing raw natural fiber in
composites is an incompatibility between the hydrophilic natures of natural fiber. Many surface modification
methods have been investigated to alter the natural fiber surfaces, so as to improve the compatibility of the natural
fibers [3].
Some of them are alkali treatment [5-14, 18, 19], Potassium permanganate treatment [9, 10], Benzoyl chloride
treatment [9, 10], Acrylic acid treatment [9, 10], Peroxide Treatment [11], sugar treatment [15], potassium hydroxide
[16, 17], hydrogen peroxide [20]. These treatment methods are implemented to determine the tensile strength [5-7, 8, 9,
12, 15-18, 19], flexural strength [12-19], moisture absorption [12], impact strength [12, 17, 18] and some other
mechanical and chemical properties of the natural fibers and its composites.

2. Materials and Methods

2.1 Materials

Areca sheaths were collected in and around the Shivamogga, collected sheaths were washed in water and dried till
the moisture is removed from the sheaths. Tensile and flexural test specimens were prepared as per ASTM standards
D3039 [22] and D790 [23] respectively. The analytical grade chemicals were purchased from Pal Scientific and
Surgicals, Davangere, Karnataka.
28082 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088

2.2 Chemical modification of areca sheath fibers

Lignin, holocelluloses, α-cellulose and hemicellulose content and chemical modifications of fibre; alkylation,
benzoylation, acrylation, peroxide and permanganate treatments were determined according to methods described by
Dhanalakshmi et.al. [10].

2.3 Mechanical Tests

Tensile and flexural tests were conducted using a Universal testing machine with the capacity of 1N to 2.5kN. As per
the ASTM standard maximum of five specimens were prepared and all are tested and average values were presented.

1. Tensile tester 2. Converter (Load Master Series III) 3. Computer system

a. Experimental setup

b. Tensile specimen held between a pair of grips c. Three-point bending test specimen
Fig. 1. Experimentation

Initially, untreated and chemical treated specimens were dried carefully, specimens were prepared according to
ASTM D3039 and D790 standards (Fig. 1). For tensile test, specimens length considered was 250 mm, width 15
mm and thickness 1 mm, and a pair of aluminum tabs of length 56 mm was used at both the ends of the specimen to
 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088 28083

facilitate the proper grip for the areca sheath specimens in the tensile test. Fig. 1 (a) shows the different elements of
the experimental setup; it mainly consists of three elements, 1. Universal testing machine, 2. Converter (Load Master
Series III), 3. Computer system. Universal testing machine (maximum capacity 1N to 2.5kN), interconnected to
indicator (Load Master Series III) to store the Load, displacement and other parameters history automatically with
RS 232 connection. Test specimen was installed between two grips is shown in Fig. 1 (b). Similarly, for flexural
strength test, areca sheath specimen with gauge length 88.6mm, width 25.4mm, and thickness 2.36mm were used.
Fig. 1 (c) clearly exhibits the three-point bending specimen held in the test rig. Both tensile and bending specimens
were loaded in the computerized universal testing machine with the loading rate of 1 mm/min until the failure of
specimen occurs at laboratory conditions (temperature - 30±5 0C: Relative Humidity - 60%).

3. Results and Discussions

3.1 Density of areca sheath

The density of areca sheath was determined in accordance with BS EN 323:1993/ASTM D 3800-99 and the result
were taken as the average of ten samples. The areca sheaths were classified into dry, medium dry, medium wet and
wet sheath according to percentage of moisture content. The densities of areca sheath with 10 (dry), 25 (medium
dry), 43 (medium wet), and 64% (wet) moisture were found to be 0.4062, 0.5605, 0.6816 and 0.6580 g/cm3
respectively.

3.2 Chemical Composition of areca sheath fibers:

Natural fibres are made up cellulose, hemicellulose and lignin. In natural fibers, semi-crystalline cellulose is the
main reinforcement material which is held together by amorphous hemicelluloses whereas lignin acts as plant cell
adhesive which helps in cementing the fibres together. All the natural fibres possess similar properties such as
flammability, thermo-plasticity, swelling and shrinking, chemical reactivity due to variation of moisture content in
cell wall, in spite of having different chemical composition which results in designing specific application-oriented
composites. The chemical composition of areca sheath is compared with other natural fibres in Table 3.

Table 3. Chemical composition (wt%) of natural fibers

Fiber Cellulose Hemicellulose Lignin Moisture Ash
Areca sheath 34.82 25.68 16.58 12.06 10.86
Bagasse 32-48 19-24 27-32 -- 1.5-5
Bamboo 26-43 21-31 15-26 -- 1.7-5
Rice 28-48 12-16 23-28 -- 15-20
Coir 36-43 0.15-0.25 41-45 8.0 --
Wheat 29-51 -- 16-21 -- 4.5-9
Oat 31-48 -- 16-19 -- 6-8
Kenaf 31-39 15-19 21.5 -- 4.7

3.3 Chemical treatment of areca fibers

Chemical treatment of areca sheath fibres facilitates proficient coupling with polymeric matrix by uncovering more
responsive groups on the fiber surface. Areca sheath fibres are pretreated with sodium hydroxide (Scheme 1) which
results in increase of amorphous cellulose at the expense of crystalline cellulose, which increases the moisture
resistance property of the fibre. Benzoylation (Scheme 2) of alkali pretreated fibers further reduces the
hydrophilicity and enhances the chemical interlocking at the interface. The replacement of hydrophilic hydroxyl
groups by hydrophobic ester groups occurs due to acrylation (Scheme 3), permanganate treatment (Scheme 4)
results in physically rough surface of fibres which effectively reduces the moisture absorption and increases the
surface area of the fibre respectively. Benzoyl peroxide treatment removes the surface and subsurface
contaminations. Hence, effective increase in the adhesion between the resin and matrix is been expected [9, 20, 21].
28084 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088

3.4 Morphological study

SEM images of the areca sheath before and after the alkali treatment is presented in Fig. 2. From Fig. 2(a) it can be
observed that the surface of the areca sheath is not even, spread with nodes and irregular strips. The fiber surface is
covered with a layer of substances, which may include pectin, lignin and other impurities. The image of alkylated
fiber (Fig. 2(b) displays a large number of globular fatty deposits, pin holes on the surface; which are due to the
elimination of fatty deposits from the fiber. This designates a very fresh surface of fibers and appears to be
moderately roughened by the chemical treatments

Fig. 2. SEM image of areca sheath (a) Untreated, (b) Treated with 5% NaOH

3.5 Mechanical Tests

3.5.1 Tensile Test

Tensile strength of untreated and chemically treated areca sheath specimens was carried out according to ASTM
D3039 standard procedure at a standard laboratory atmosphere of 30±2 0C. A rectangular shape specimen with the
total length of 250 mm, gauge length of 150 mm, the width of 15 mm, and a constant thickness of 1.0 mm [22], is
considered for the test. The specimen was stacked in the universal testing machine until the failure of the specimen
occurs. Average results of 5 specimens of untreated and chemically altered areca sheath fibers under 5%, 10%, 15%
and 20% chemical concentrations was presented in Table 4.

Table 4. Tensile strength values (Experimental) for untreated and treated areca sheath fibers
Tensile Strength (N/mm2)
Chemical
Alkali Benzoylation Acrylation Permanganate Peroxide
Concentrations Untreated
Treatment Test Test Test Test
5% 21.54 9.84 19.46 15.69 12.57
10% 7.37 8.33 9.08 12.69 4.81
16.45
15% 7.36 10.47 11.19 7.66 12.48
20% 10.26 12.17 11.64 6.88 3.79

Generally, chemically altered natural fiber composites exhibits higher tensile strength than the untreated fiber
composites. The effect of artificial treatment on the tensile strength of areca sheath fibers is depicted in Fig. 3. It is
observed that the tensile strength of 5% alkali treated areca sheath fibers have shown good tensile properties than the
untreated, followed by 5% acrylic acid treated fibers. Except alkali and acrylation treatment, areca sheath fibers
have shown downfall in the tensile strength as compared to untreated fibers. It is also noticed that 25% and 41%
reduction in the tensile strength values for the peroxide treated and benzoyl treated fibers.
 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088 28085

Fig. 3. Tensile strength of areca fiber with different concentrations and different chemicals

An effective impact on the tensile strength of areca sheath fiber was observed with chemical modifications. The
tensile strength values of untreated areca sheath fibers are 16.45 N/mm2.
The tensile strength values of alkali (NaOH) treated areca sheath fibers with chemical concentrations from 5%, 10%,
15%, 20% are 21.54 N/mm2, 7.37 N/mm2, 7.36 N/mm2, and 10.29 N/mm2 respectively.
The tensile strength values of alkali treated areca sheath fiber with 5% concentration have shown 30.94% increment
compared with the untreated and decreases to 44.8%, 44.75%, and 62.5% for 10%, 15%, and 20% alkali treatment.
For 20% alkali treatment, a small increment in the tensile strength was observed that is because of the removal of all
hydroxyl groups from the sheath and load was directly taken by the fibers.
The tensile strength values of benzoyl chloride treated areca sheath fibers with 20% concentration have shown good
results as compared to other concentration treatments. But benzoylation of areca sheath fiber has shown that the
greater amount of decrement in the tensile properties of fibers. Obtained tensile strength values for 5% to 20%
benzoyl chloride treated fibers have shown 9.84 N/mm2, 8.33 N/mm2, 10.47 N/mm2 and 12.19 N/mm2 values
respectively and these values are in downfall trend with 40.15%, 49.3%, 36.34% and 25.98% compared to untreated
areca sheath fibers.
The tensile strength values of acrylic acid treated areca sheath fiber with 5% concentration have shown an increment
of 18.34% as compared with the untreated fibers. And sudden fall in the tensile strength was observed for 10%
acrylic acid concentration. The slight increment was observed for 15% and 20% concentrations. Obtained tensile
strength values for acrylic acid treated fibers are 14.66 N/mm2, 9.08 N/mm2, 11.19 and 11.63 N/mm2 for 5%, 10%,
15% and 20% acrylic acid treated fibers.
The tensile strength values for permanganate treated areca sheath fibers are 15.69 N/mm2, 12.697.66 N/mm2 and
6.88 N/mm2 for the concentrations 5%, 10%, 15% and 20% respectively. 5% permanganate treated fiber have shown
close results with the untreated areca sheath fibers but very minute decrement in the tensile strength was observed at
4.6%. And the results for other concentrations are 22.85%, 53.45%, 58.15%, which are gradually decreasing in order
when compared with the untreated fiber.
The tensile strength values for peroxide treated areca sheath fibers have shown a considerable decrement in the
tensile strength for all the concentrations. Least value 3.79 N/mm2 is recorded for 20% peroxide treated specimen
among all available specimens for all the categories.
28086 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088

3.5.2 Flexural Test

The flexural test measures the force required to bend a beam under three-point loading conditions. The flexural test
is also known as bending test and applying a concentrated load (point load) at the center of the specimen until it
fractures and breaks. The testing was done as per ASTM D790 with the help of computerized UTM at a crosshead
speed of 1mm/min and at room temperature. The standard specimen size for ASTM D790 is 88.9 mm x 25.4 mm x
2.36mm [23]. Five samples were tested for each case and average flexural load was reported in N. The flexural
load values of untreated and treated areca sheath fibers under 5%, 10%, 15% and 20% chemical concentrations were
given in table 5.

Table 5. Flexural load values for untreated and treated areca sheath fibers
Flexural Strength (N)
Chemical
Alkali Benzoylation Acrylation Permanganate Peroxide
Concentrations Untreated
Treatment Test Test Test Test
5% 24.47 15.49 32.49 16.99 8.98
10% 20.87 35.07 27.84 12.89 25.39
41.71
15% 9.12 20.70 14.54 8.76 17.90
20% 11.78 17.23 14.69 20.53 28.95

It is observedIthat chemical treatment of areca sheath fiber has no effect on flexural load. The effect of chemical
treatment on flexural load for untreatedIand chemically treated areca sheath fibers with different chemical
concentrations is depicted in Fig. 4.

Fig. 4. Flexural load for areca fiber with different concentrations and different chemicals

Alkali (NaOH) treatment of areca fibers takes out a certain portion of hemicelluloses, lignin, adhesive pectin, waxy
epidermal tissue, and oil covering materials and reduced fiber geometry [15], as a result of this alkali treated areca
sheath fibers have shown decreased flexural (bending) strength values when compared to untreated fibers. The
flexural load for alkali treated areca sheath fibers decreased by 41.36%, 50%, 78.05% and 71.7% for 5%, 10%, 15%
and 20% concentrations compared to untreated fiber.
Benzoylation treatment results in an establishment of ester linkage with areca sheath fibers and it improves chemical
interlocking between the fibers cells, as a result of this the fibers treated with benzoyl chloride showed slightly
higher flexural load values, when compared with that of alkali treated. Among four chemical concentrations, 10%
 Ashok R Banagar / Materials Today: Proceedings 5 (2018) 28080–28088 28087

benzoyl chloride treated areca fiber has shown good results of 35.07N which is higher than that of alkali treated
fibers and is comparative value with the untreated areca sheath fibers.
During acrylic acid exploration, most of the hemicelluloses and lignin are expelled out and there is the substitution
of hydroxyl group by hydrophobic ester groups in the areca fiber. Hence as the concentration of acrylic acid
increases like flexural load is decreased. The flexural load for acrylic acid treated areca sheath fiber with 5%
treatment have shown 21.9% decrement when compared with untreated, similarly, 33.09% for 10% treated, 65.1%
for 15% treated and 64.7% for 20% treated areca sheath fiber.
Permanganate ions carved the fiber surface due to the reaction with the lignin ingredients and as a result, areca fiber
surface became uneven and brittle. This will reduce the load-bearing capacity of areca sheath fibers, as a result,
flexural load decreases. The flexural load for permanganate treated areca sheath fibers is reduced by 54.3%, 69.06%,
78.99%, and 50.75% for 5%, 10%, 15% and 20% concentrations when compared to untreated areca sheath fiber.
Here a slight increment was observed for 20% concentration that is because of high roughness and brittleness of the
fibers.
The peroxideItreatment was carried out on an alkali pre-treated areca sheath fiber. Pre-treated areca sheath fibers
were treated with different concentration benzoylIperoxide in acetone for 30min. AfterItreatments, fibers were
thoroughly washed with distilledIwater and dried at 80 ℃ for 24Ih. Since peroxide is a bleaching agent, it will clean
the alkali treated surface of the fiber, as a result, decreased flexural load values are noticed for 5% treated fibers. As
the concentration of the benzoyl peroxide increases, it will take away the alkali content and other materials from the
areca sheath fiber, this will increase the flexural load of the fibers (for 10%, 15%, and 20%). As compared to
untreated fiber values, this treatment will also exhibit the same trend as of other chemicals.

Conclusions

As a result of surface modification of areca sheath fibers, some of the chemically active group coatings is considered
on the surface of the fiber. Also, some of the naturally available impurities in the areca fiber will be removed. From
the study, it is concluded that, in connection with the surface modification of the fibers, the surface roughness is
achieved, this will affects the performance of the areca sheath fiber in many tests.
Reduction in the hydrophilic property of fibers enhances the proper natural bonds between the areca sheath cells,
which will, in turn, increases the mechanical properties or loss of bonds between the cells will reduce the
mechanical properties. Tensile strength values of areca sheath fibers are increased after surface modification for 5%
alkali treatment and 5% Acrylation test. The highest value of tensile strength is observed for 5% alkali treated areca
fibers. And no further improvement in the flexural load property for areca sheath fibers after surface modification is
observed. Among all type of surface modification processes, untreated areca sheath fibers have shown good results
for flexural load tests. Even though the benzoylation test and Acrylation tests have shown considerable increment in
the flexural load values as compared to alkali-treated and another type of chemical treatments.
Hence, the areca sheath fibers can be considered as a very promising material for tensile load applications in
lightweight materials and can be adequately utilized as a part of industrial division like locomotive parts, office
furniture, packaging industry, partition panels, etc. and in its raw format areca sheath fibers can be used in some of
the flexural load application.

Acknowledgements

The authors are thankful to the Vision Group on Science & Technology, Department of IT, BT and Science &
Technology, Government of Karnataka for financial support in the form of sanctioning a Research Project for the
proposal titled: “Establishment of Green Engineering Research Center and Research on Bio-Based Sandwich
Composite Structures”, to carry out the present investigation (Grant Ref. No: PɸÉÖ¥ïì / «vÀAzÁ¸À / ವಿತಂದಾ¸À / 05 / K-
FIST / 2015-16, Dt.: 20.06.2016, GRD No: 486)

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