Journal of Natural Fibers

ISSN: 1544-0478 (Print) 1544-046X (Online) Journal homepage: http://www.tandfonline.com/loi/wjnf20

Influence of chemical treatment on tensile

strength, water absorption, surface morphology,
and thermal analysis of areca sheath fibers

Subhakanta Nayak & Jyoti Ranjan Mohanty

To cite this article: Subhakanta Nayak & Jyoti Ranjan Mohanty (2018): Influence of chemical
treatment on tensile strength, water absorption, surface morphology, and thermal analysis of areca
sheath fibers, Journal of Natural Fibers, DOI: 10.1080/15440478.2018.1430650

To link to this article: https://doi.org/10.1080/15440478.2018.1430650

Published online: 26 Jan 2018.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2018.1430650

Influence of chemical treatment on tensile strength, water

absorption, surface morphology, and thermal analysis of areca
sheath fibers
Subhakanta Nayak and Jyoti Ranjan Mohanty
Department of Mechanical Engineering, Veer Surendra Sai University of Technology, Burla, India

ABSTRACT KEYWORDS
Proper surface modification is highly essential to improve compatibility of Areca fiber; surface
natural fibers with polymer matrix to develop eco-friendly materials. In the modification; thermal
present work, an attempt has been made to study the effect of various gravimetry analysis (TGA);
Fourier transform infrared
chemical treatments such as alkaline, acrylic acid, permanganate, sodium
spectroscopy (FTIR);
chlorite, and benzoylation on areca sheath fiber. After surface modifications, scanning electron
its density, water absorption property, mechanical property, thermal gravi- microscopy (SEM); water
metry analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and absorption
surface morphology have been thoroughly investigated. It has been
observed that benzoyl chloride-treated fiber gives better performance in 关键词
comparison to other treatments. 槟榔纤维; 表面改性; 热重
分析（TGA）; 傅立叶变换
红外光谱（FTIR）; 扫描电
摘要 子显微镜（SEM）; 水的吸
适当的表面改性对于提高天然纤维与聚合物基体的相容性，开发环保材料 收
至关重要。在目前的工作中，已尝试研究各种化学处理，如碱、丙烯酸、
高锰酸钾、氯酸钠的作用，并对槟榔鞘纤维的苯甲酰化反应。经过表面修
饰，其密度、吸水性能、力学性能、热重分析（TGA）、傅里叶变换红外
光谱（FTIR），和表面形态已经被彻底的调查。已观察到，与其他处理相
比，苯甲酰氯处理的纤维具有更好的性能。

Introduction
Recently, global warming is a major environmental issue which is a challenge to the world commu-
nity. This is mainly due to the urbanization and mechanization of life style of the people. The use of
synthetic and plastic materials is one of the important factors for this problem. Since the inception of
composite materials made of straw and mud, scientists and engineers have developed various low-
cost fiber reinforced polymer composites (FRP) by reinforcing synthetic fibers in polymeric matrices.
However, the use of synthetic fibers is being restricted due to various disadvantages like biodegrad-
ability, initial processing costs, recyclability, energy consumption, machine abrasion, health hazards,
etc. (Aziz and Ansell 2004). Therefore, the growing environmental awareness throughout the world
has triggered a paradigm shift toward the use of natural fibers as an attractive alternative to synthetic
fibers. It provides positive environmental benefits with respect to ultimate disposability and raw
material utilization (Narayan 1992).
As such, natural fibres are not a problem-free alterative to synthetic fibers for development of
FRP composites in spite of several advantages like better chemical and electrical resistance, good
thermal and acoustic insulating properties, high fracture resistance, light weight and density,
renewable character, acceptable specific strength, enhanced energy recovery, and

CONTACT Subhakanta Nayak [email protected] Department of Mechanical Engineering, Veer Surendra Sai
University of Technology, Burla, Sambalpur 768018, India.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/wjnf.
© 2018 Taylor & Francis
2 S. NAYAK AND J. R. MOHANTY

biodegradability. The major problem relating to the use of natural fibres in FRP composites is
their moisture-absorption property. It is mainly because of hydrophilic nature of natural fibers
which is incompatible to hydrophobic polymer matrices leading to poor bonding and ineffective
stress transfer throughout the interface of the composites. The properties of these fibers are
greatly influenced by the crystal-structure, the degree of crystallinity, the spiral angle of the
fibrils, the degree of polymerization, the porosity content, the size of the lumen (center void),
and the chemical composition which controls the overall property of FRP composites. In order
to enhance the property of natural fiber reinforced polymer composites, the properties of fibers
have to be optimized (Mohanty, Misra, and Hinrichsen 2000). It is achieved by proper chemical
treatments of the fiber surface to improve compatibility and interfacial bond strength which is
one of the challenging areas of today’s composite research. Although these additional processes
required to reduce the moisture sensitivity of natural fibers raise their cost, these may still be
affordable to get overall cost-effective products.
Among all the natural fibers, areca appears to be a promising reinforcing material because it
is inexpensive, abundantly available, and a very high-potential perennial crop. It belongs to the
species Areca Catechu L., under the family Palmecea and originated in the Malaya peninsular,
East India (Rajan and Kurup 2005). In India, this perennial crop is mainly grown in the states of
Kerala, Tamil Nadu, Assam, Andaman & Nicobar Islands. Areca leaf sheath is shed periodically
from the tree and used for making plates/cups, fuel, and composting. This highly hemicellulosic
material can be potentially used as reinforcing fiber in FRP composites if its property is properly
explored in details. Till now, several studies have been conducted which deal with the chemical
treatments of natural fibres in order to modify not only the interphase, but also produce
morphological changes on the fibers (Aziz and Ansell 2004; Cyras et al. 2001; Khalil and
Rozman 2000; Rong et al. 2001; Stocchi et al. 2007). As far as areca sheath fiber is concerned,
few works have been done pertaining to surface modification. The effect of alkali-treatment and
acetylation on water-absorption characteristics of single areca fiber was studied by Sampath
kumar et al., 2012. They found that the acetylation of areca fibers drastically reduces the water
absorption; whereas, alkali treatment of areca fibers improves the water absorption. The effect of
alkali treatment on impact behavior of areca fibers reinforced polymer composites has been
conducted by (Srinivasa and Bharath 2013). They have observed that the alkali-treated areca
fiber reinforcement increases the impact strength of composite. Composites made of alkali-
treated areca fiber shows improved tensile strength, thermal stability, and acoustic property in
comparison to untreated one (Jayamani et al. 2014). Most of the studies on surface modification
of areca fibers deal with alkali treatment which more or less improves various properties of
fibers. However, there are other chemical treatments available in the literature which can be used
in areca fiber in order to improve its property. Therefore, the aim of this research work is to
investigate the effect of other chemical treatments like benzoylation, permanganate, acrylic acid,
sodium chlorite in addition to alkali treatment on tensile, thermal, and water-sorption properties
of areca fiber. The treated and untreated areca fibers have been characterized by Fourier trans-
form infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric
analysis (TGA), and tensile testing to ascertain the productive use of those fibers in FRP
composites.

Materials and methods

Materials
Areca leaf sheath have been collected from rural areas of Odisha, India. The chemicals such as
sodium hydroxide, benzoyl chloride, potassium permanganate, acrylic acid, and sodium chlorite of
analytical grades have been used without any further purification. All solutions are made in double-
distilled water.
 JOURNAL OF NATURAL FIBERS 3

Methods
Fiber extraction
Dried areca sheath has been soaked in water for about 10 days which loosened the fiber for easy
extraction. The fibers have been separated from the sheath by using metal wire brush and dried at
room temperature. The extracted fibers are designated as untreated fibers.

Surface modification of areca fibers

Alkali treatment. The untreated areca sheath fibers have been treated in 5% sodium hydroxide
(NaOH) solution for 1 h at a temperature of 80°C. Then, the fibers have been cooled to room
temperature and washed in running water to remove any trace of sodium hydroxide solution
adhered on the surface of the fibers so that the pH level of fiber is approximately 7 (neutral).
Then, they have been dried in an oven at a temperature of 60°C for 24 h. The areca sheath fibers
obtained at this stage have been designated as alkaline pretreated fibers.

Benzoylation treatment. The alkaline pretreated areca sheath fibers have been treated with 10%
NaOH and benzoyl chloride solution for 15 min. The resulting fibers have been dipped in ethanol
for 1 h to remove benzoyl chloride sticky to the fiber surface. Then, the fibers have been washed with
distilled water and put in an oven maintaining 80°C temperature for 24 h for drying purpose.

Permanganate treatment. The alkaline pretreated fibers have been soaked in potassium permanga-
nate solution maintaining a concentration of 0.003% in acetone for 1 min. Similar to the previous
treatment, the resulting fibers have been rinsed with distilled water and oven dried at a temperature
of 80°C for about 24 h.

Acrylic acid treatment. The alkaline pretreated fibers have been first soaked in a solution of water
and benzene (45:5 cm3). The temperature and time during this process are maintained at 85°C and
15 min, respectively. After that the fibers have been treated with 0.3 M acrylic acid. The resulting
fibers have been rinsed first with an alkaline solution of NaOH and NaCl for 15 min and then with
distilled water for 1 h. Similar procedure has been followed as per previous treatments to dry and
cool the fibers for further use.

Sodium chlorite treatment. The alkali-treated areca fibers have been treated with sodium chlorite
solution (Sodium chlorite: water = 1:25) at 70°C for 2 h. Then the fibers have been washed with
distilled water and oven dried as discussed earlier.

Characterization of fibers
Density. The density of areca sheath fibers has been determined by measuring the mass and volume
of a bunch of fibers. Each bunch of fibers has been weighed to an accuracy of 0.001 g by using an
analytical balance. The mass of each bunch has been calculated by taking the arithmetic mean of the
mass of all the test samples. The dimensions of each fiber have been measured using a sliding caliper
having accuracy of ±0.02 mm, in accordance with BS EN 325:1993. The volume of the fiber has been
calculated by multiplying the length and cross-sectional area of the fiber. Diameters of the fiber
varied from 0.285 to 0.899 mm and the length varied from 18 to 29 mm. The density of the fiber has
been determined as per BS EN 323:1993 for untreated and treated fibers (Srinivasa and Bharath
2011).

Single fiber tensile test. The mechanical properties (tensile strength, Young’s modulus, and elonga-
tion at break) of single areca sheath fiber have been performed as per ASTM D3379-75. To hold the
specimen in the machine, a tab has been prepared from a thick sheet of paper. A slot has been cut in
the middle of the tab having length equal to the gage length (50 mm) of the specimen. A single
4 S. NAYAK AND J. R. MOHANTY

filament of areca fiber has been pasted by gluing both ends (about 20 mm) of the fiber in the slot.
The specimen to be tested is mounted on INSTRON 3382 machine with a 100 g load cell. A gauge
length of 50 mm and crosshead speed of 0.2 mm/min are maintained. During the test, both sides of
the tabs have been cut carefully at the mid-gage without disturbing the setup as a whole. The full-
scale load has been applied by the testing machine till the specimens failed. From each chemical-
treated fiber bundles, a total of 25 filaments have been tested one after another and the averages of
the readings have been recorded.
For untreated areca fiber, tests in gage lengths of 10, 20, 30, 40, 50 and 60 mm have been
performed to determine the machine compliance and study the influence of gage length on the fiber
tensile behavior. The compliance of the loading and gripping system has been determined by
obtaining the force versus displacement behavior of the fiber at various gauge lengths as per
ASTM D3379. The total cross-head displacement during fiber testing, Δl has been determined by
the following equation:
Δl l
¼ þc (1)
F EA
Where, ‘c’ is the machine compliance, ‘F’ is the applied force, ‘E’ is the Young’s modulus of the fiber,
and ‘A’ is the cross-sectional area of the fiber.

Water absorption. The study of water-absorption properties of untreated and treated areca fibers
has been conducted in pond and bore well water whose pH values are 8.30 and 7.20, respectively.
The specimens (fiber bundles) have been dried in hot air oven at 60°C for 24 h, weighed in a balance
accurate to 4 decimal places (±0.1 mg), and then placed in the humidity chamber (desiccators)
maintained at room temperature. Each fiber bundle is taken out from the humidity chamber after 24
h and the excess water is removed by filter paper. The weight of the fibers has been measured and
the process is repeated after different interval of time for a period of 105 days. The percentage gain at
any time t, Mt as a result of water uptake, has been calculated as per Eq. 2 (Jimenez and Bismarck
2007).
Wt  W0
Mt ð%Þ ¼  100 (2)
Wt
Where Wt is the mass of the sample after immersion (g) and W0 is the mass of the sample before
immersion (g).

Thermogravimetric analysis (TGA). The thermal stability of areca fibers is characterized using a
thermogravimetric analyzer (TA instrument, Q50 V20.13 Build 39). About 10 mg of areca fiber is
exposed to atmospheric air with a heating rate of 10°C min−1 from room temperature to 400°C.

Fourier transform infrared spectroscopy. The FTIR spectra of untreated and surface-treated areca
fibers have been recorded in a Nicolet 6700 spectrophotmeter in the form of KBr Pellets. The test
apparatus is equipped with Germanium Attenuated Total Reflectance (ATR). About 200 scans have
been collected for each measurement over the spectral range 4000–375 cm−1 with a resolution of
4 cm−1.

Surface morphology. Microscopic examinations have been performed using a HITACHI SU3500
scanning electron microscope (SEM). All specimens are sputtered with a 10 nm layer of gold and
mounted on aluminum holders using double-sided electrically conducted carbon adhesive tabs prior
to SEM observations.
 JOURNAL OF NATURAL FIBERS 5

Results and discussion

Density
Generally, natural fibers contain pores and voids. Hence, the problem in determining the reliable
value of density is related to their porous nature. The apparent density is the density of natural fiber
including voids which are inherent in the vegetable fibers. Batra (Batra 1998) has measured an
apparent density of fibers as 1.38 g/cm3 and a true density as 1.54 g/cm3. In the present case, the
apparent densities of areca fibers have been measured for both treated and untreated fibers to have
an overview about the change in densities, if any, during chemical treatments. The apparent densities
of areca fibers have been measured as per the procedure described earlier and found to be 1040 ± 30,
1245 ± 20, 1160 ± 10, 1190 ± 20, 1210 ± 30 kg/cm3 for untreated, alkali-treated, benzoylation-treated,
permanganate-treated, acrylic acid-treated, and sodium chlorite-treated fibers, respectively. The
measured densities are in the range of 1040 to 1245 kg/cm3 which is consistent with the earlier
results (Srinivasa et al. 2011), i.e. 1.05 to 1.25 g/cm3. From the results, it has been observed that the
fiber densities are almost unaffected by surface modifications. However, they increase after alkali
treatment, may be, due to the destruction of cellular structure of the areca fiber which reduces the
void contents. For other surface modifications, the reactions mainly occur on the fiber surface and
do not affect the internal structure of the fibers. The SEM results of cross-section of untreated and
alkali-treated areca fibers have been shown in Figure 1.

Figure 1. SEM image of cross-section of areca fiber (a) untreated and (b) alkali treated.
6 S. NAYAK AND J. R. MOHANTY

Tensile strength
Table 1 presents the tensile test results of untreated areca fiber for different gage lengths. A total of
25 fibers have been randomly selected from a given batch and tested. Young’s modulus has been
calculated in the elastic portion of the stress-strain curve and then corrected for compliance by
measuring force versus displacement at various gage lengths using Eq. 1. From the results, the gage
length does not seem to influence the Young’s modulus of the fiber. The variability in Young’s
modulus is probably related to the variability in microstructure of the areca fiber. The tensile
strength does not seem to be a function of gage length. The obtained tensile strength varied for
different gage length from 32.67 to 65.72 MPa with standard deviation ranging from 2.81 to 5.02
MPa. Strain-to-failure results seem to be higher for the 20-mm gage length and do not show
significant variation for the lengths of 30 mm and higher. Similar behavior has been reported for
other chemically treated fibers and the final results have been shown in Figure 2 in the form of a bar
chart in order to compare the effect of chemical treatments on the tensile properties of areca fibres.
By comparing the tensile strengths (σ) of untreated areca fibers (Figure 2 a) with the treated ones,
it is observed that the strength values of all the treated fibers are found to increase in comparison to
untreated one. Particularly, in case of benzoyl chloride-treated fibers, the value is considerably
higher. This may be due to the removal of waxes, gums, and cement materials leading to an increase

Table 1. Summary of average tensile test results and standard deviation of areca sheath fibers.
Strain-to-failure Area
Gage length (mm) Tensile strength (MPa) Young’s modulus (MPa) (%) Weibull modulus (mm2)
10 55.77  4.80 748.62  26.50 0.91  0.3 1.49 0.235  0.15
20 58.22  4.80 694.03  27.21 0.92  0.3 2.25 0.244  0.20
30 42.71  2.81 725.10  15.75 0.65  0.2 3.68 0.228  0.15
40 32.67  3.30 807.09  20.18 0.78  0.2 2.79 0.223  0.10
50 65.72  5.02 826.18  22.87 0.68  0.2 2.06 0.264  0.21
60 39.88  3.81 789.74  22.90 0.79  0.2 2.31 0.232  0.17

Figure 2. Effect of chemical treatments on (a) tensile strength, (b) Young’s modulus, and (c) elongation at break of areca fiber.
 JOURNAL OF NATURAL FIBERS 7

in the ratio of cellulose content which increases the mechanical properties of fibres. The reason of
highest value of tensile strength for benzoyl chloride-treated fibers is that the exposed hydroxyl (OH)
groups of pretreated fibers are further replaced by benzoyl group and it is attached to the cellulose
backbone which increases the surface roughness of fibers.
Considering the Young’s modulus (E) of fibers (Figure 2 b), it is observed that the chemical
treatments used increase the stiffness of fibers, highest for acrylic acid-treated fiber. This may be due
to the fact that volatile substance, lignin, and other unwanted materials that ensure cohesion between
cellulose microfibrils are partially eliminated by chemical treatments. However, in case of acrylic
acid-treated fibers, the surprising high value of E could be due to the esterification of cellulosic fiber.
The esterification increases the surface roughness of fiber which enhances the amount of cellulose
exposed on the fiber surface as well as in the reaction sites. As far as percentage elongation before
break (Figure 2 c) is concerned, its value is more in case of alkaline-treated fibers showing its ductile
behavior.

Figure 3. Comparison of water absorption of untreated and treated areca fibers: (a) bore well water and (b) pond water.
8 S. NAYAK AND J. R. MOHANTY

Water-absorption property
The experimental results of percentage of water absorption as a function of the square root of
immersion time (√t) for each immersed specimen in two different sources for a period of 105 days
has been shown in Figure 3. The relationship of the water absorption with the square root of
immersion time appeared to obey non-Fickian’s behavior (Nosbi et al. 2011) mostly in the first phase
of the measurement. It has been observed that for both untreated and treated areca fiber immersed
in bore well (Figure 3 a) and pond water (Figure 3 b), the percentage of water absorption increases
nonlinearly with √t in the first phase of the curve till 25 root square hours. Then, the percentage of
water uptake decreases with immersion time in almost all cases except for acrylic acid- and
benzoylation-treated fibers in pond water (Figure 3 b). In those cases, the saturation stage occurs
approximately after 30 root square hours. The first absorption phase of all the fibers may be due to
wetting of fibers and the capillary absorption process where the water diffuses into the fibers until
reaching a maximum absorption. When the immersion time becomes significant, a decreasing trend
in water absorption occurs which may be due to the presence of physical damage, chemical or
material hydrolysis.

Thermogravimetric analysis
To use a natural fiber as reinforcement in polymer matrix, its thermal stability has to be
analyzed to have a clear picture on curing and extrusion temperature of thermosets and
thermoplastic matrix composites, respectively. The TG curves of both untreated and treated
areca fibers are shown in Figure 4. As evident from the curves, all the fibers have been degraded
mostly in two major steps. The first step corresponds to 24% weight loss which occurs at 250°C
for untreated fiber. Whereas for other treated fibers, it occurs in the temperature range from
260°C to 270°C. The second step corresponds to 60% weight loss and may be considered as
major degradation in the process. This major weight loss occurs at 345°C for treated fiber; for
others, it falls in the range of 350°C to 352°C. It should be noted that the end temperature values
for both the steps are referred to as benzyolation-treated fibers which show better thermal
stability in comparison to other treated fibers.

Figure 4. TGA curves of untreated and treated areca fibers.

 JOURNAL OF NATURAL FIBERS 9

Figure 5. FTIR of untreated and treated areca fibers: (a) untreated, (b) alkaline, (c) sodium chlorite, (d) permanganate, (e) acrylic
acid, and (f) benzoylation.

Fourier transform infrared spectroscopy

A comparison of FTIR spectra of areca fibers before and after chemical treatments has been
presented in Figure 5. The region 3500–2500 cm−1 is mainly due to OH and CH/CH2 groups. As
observed in the figure, compared to untreated spectrum, the peak area at 3372 cm−1 has been
increased considerably indicating the presence of an increased number of OH groups arising due to
the cleavage of alkali-sensitive bonds. The peak observed at 2931 cm−1 is pronounced in treated
fibers compared to untreated one which may be due to –CH– group formation. The carbonyl
(C = O) stretching vibration at 1743 cm−1 corresponds to hemicellulose; whereas, the peak at
1618 cm−1 is associated with the absorbed water, due to the hydrophilic character of the cellulose
fibers. The C–OH stretching vibration of the cellulose backbone at 1060–1033 cm−1 (ν C–O
secondary alcohol) arises from the polysaccharide components (i.e. largely cellulose) and this is
more predominant in chemically treated fibers.

Surface morphology
The surface morphology of untreated and treated areca fibers is shown in Figure 6. From SEM image
of untreated areca fiber (Figure 6 a), it is observed that the longitudinally oriented unit cells are
oriented in parallel directions in which the fibrils are bound together by hemicelluloses and lignin.
The intracellular gap is filled with lignin and fatty substances. In case of alkali-treated areca fibers
(Figure 6 b), a large number of pinholes or pits is clearly observed and the fiber surface is rough and
irregular in comparison to untreated one. This may be mainly due to the removal of impurities, waxy
epidermal tissue, adhesive pectin, and hemicelluloses thereby causing fibrillation. Figures 6 (c-f)
show further removal of fatty deposits that occurs in case of other chemical treatments which make
the fibers curved, their surfaces become more rough, and diameters decrease.

Conclusion
The potential of using natural fiber as reinforcing material in polymer matrix is based on the interfacial
properties and good compatibility between the fiber and matrix. This can be achieved by giving proper
surface modification of natural fibers with different chemicals and to characterize their properties. In
10 S. NAYAK AND J. R. MOHANTY

Figure 6. Surface morphology of areca sheath fibers: (a) untreated, (b) alkaline, (c) sodium chlorite, (d) permanganate, (e) acrylic
acid, and (f) benzoylation.

this direction, an attempt has been made in the present work to study the effect of various chemical
treatments on areca sheath fiber to be used as reinforcing material in polymer matrix.
From the detail analysis, it has been observed that the densities of areca fibers are almost
unaffected by surface modifications. As far as water-absorption property is concerned, different
chemical treatments reduce the water absorption irrespective of the sources. However, benzoyl
chloride- and sodium chlorite-treated fibers have better resistant to water absorption in comparison
to other treatments. The tensile strength of areca fibers is improved by chemical treatments being
better in case of benzoyl chloride treatment. The Young’ modulus shows better values for all treated
fibers as compared with untreated fibers. However, the acrylic acid-treated fibers shows highest
value. The thermal stability is also improved by various chemical treatments. Comparing overall
properties of areca fibers, it has been found that benzoyl chloride-treated fiber gives better perfor-
mance in comparison to other treatments.
 JOURNAL OF NATURAL FIBERS 11

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