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Materials Today: Proceedings 2 (2015) 3149 3155

4th International conference on material processing and characterization

Effect of Fiber Chemical Treatment on Mechanical Properties of Sisal


Fiber/Recycled HDPE Composite
Mohit Sooda, Dharmpal Deepakb , V.K Guptac
a

Post Graduate Student, Punjabi University, Patiala 147002, India


b*
Astt. Professor, Punjabi University, Patiala 147002, India
c*
Professor, Punjabi University, Patiala 147002, India

Abstract
The present study investigates the effect of chemical treatments on tensile and flexural properties of polymer composites fabricated by reinforcing
treated sisal fibers into 50-50 mixture of fresh and recycled HDPE matrix. The sisal fibers are treated with NaOH + Maleic Anhydride (MA) and
NaOH + Benzoyl Peroxide (BP) + MA. The effect of chemical treatments on mechanical properties of composites is compared at two different
contents (7.5 wt.% and 30 wt.%) of treated sisal fibers. It is observed that the composites containing 30 wt.% of NaOH + BP + MA treated sisal fiber
shows higher tensile strength than that observed for NaOH + MA treated sisal fiber composites. However at lower fiber content of 7.5 wt.% , both
the treated fibers composites exhibits almost comparable tensile strength. The flexural strength of NaOH + BP + MA treated sisal fibers composites
is significantly higher at 30 wt. % of sisal fibers but relatively lower at 7.5 wt.% of sisal fibers when compared to the corresponding composites with
the same amount of NaOH + MA treated sisal fibers.SEM images reveal that in both the composites the primary failure mechanisms responsible for
tensile failure is fiber pull-out apart from some other secondary mechanisms like fiber breakage and fiber delamination.
2015
2014 The
Authors.

Published
by Elsevier
ElsevierLtd.
Ltd.All rights reserved.
Selection and peer-review
peer-review under
underresponsibility
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conference
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Keywords: Sisal fiber; HDPE; Maleic Anhydride; Benzoyl Peroxide; SEM

1. Introduction
The interest in natural fiber reinforced composite material is rapidly growing both in term of their application and research. The
primary benefits in the broad use of natural fibers commercially are biodegradability, low cost and density, recyclability, good

Corresponding author. Tel: +91-98156-09794


E mail address: deepakbass@yahoo.com

2214-7853 2015 Published by Elsevier Ltd.


Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing
and Characterization.
doi:10.1016/j.matpr.2015.07.103

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mechanical properties, ability to withstand processing temperatures up to 230 oC, which make them an attractive ecological alternative
to synthetic fibers used for fabrication of composites [1]. Moreover, natural fibers are lighter than glass fibers which revert as fuel
reduction when this material is used by the automotive industry.
Sisal, a ligno-cellulosic natural fiber, is recently gaining attention as diversified reinforcing applications in composite industry,
housing, railways and aerospace applications on account of its low cost and density, high specific strength and stiffness, and good
range of aspect ratio [2, 3]. High density polyethylene (HDPE) is one of the synthetic polymers which possess outstanding properties
like low density and cost, good flex life and surface hardness, scratch resistance and excellent electrical insulating properties [4].
However in natural fiber reinforced composite the fiber matrix interface has reaction zone in which fibers are chemically
and/or mechanically combined [5]. During fabrication of composite with injection moulding, sisal fibers have tendency to absorb
water form environment thereby reducing efficiency of interface bonding which adversely affect the mechanical properties of the
fabricated composite. The stress transfer from the matrix to the fiber depends on fiber-fiber and fiber-matrix interactions [6]. To
create effective interface bonding between fiber and matrix, the fiber surface needs to be modified with different chemical treatments,
reactive additives and coupling agents that expose more reactive groups on the fiber surface and facilitate efficient coupling with
matrix [7]. The increased commercial use of HDPE is posing a serious environmental threat and thus the researchers are motivated to
undertake studies concerning recycling of polymer waste.
In the light of these facts, it is decided to study the effect of NaOH and benzoyl peroxide treatment, in the presence of maleic
anhydride, on the tensile and flexural properties on sisal fiber-HDPE composites, with varying fiber contents. The matrix selected in
this study comprises of 50-50 mixture of fresh and recycled HDPE, with a view to emphasis on the worldwide practice of recycling of
plastics to avoid the garbage accumulation and decomposition of the organic matter.
2. Materials and methods
2.1 Materials
In this study sisal fibers are used as reinforcement in HDPE matrix (both fresh and recycled). For chemical treatments; chemicals
used are sodium hydroxide (NaOH), benzoyl peroxide (BP); maleic anhydride (MA) used as coupling agent and acetone used as
solvent. Sisal fibers were purchased from Chandra Parkash and Company, Jaipur, Rajasthan. HDPE (both fresh and recycled) of
moulding grade was procured from Goyal polymers, Chandigarh. Chemicals used for treatment viz. NaOH, BP, MA and acetone was
procured from Vivek chemical Industries, Ambala Cantt.
2.2 Alkali treatment
Before the chemical treatments, sisal fibers were prepared by chopping them (0.5 and 1.0 cm length ) and then washed with distill
water at 80 for 1 hr followed by drying in oven at 100C for 5 hrs [8]. The alkali treatment of dried sisal fibers was carried out by
soaking them into 10 wt. % solution of NaOH for 4 hrs at room temperature. After this process the fibers were thoroughly washed
with distilled water and dried in hot air oven at 80C for 24hrs [9].
2.3 Benzoyl peroxide treatment
The peroxide treatment (BP) was carried out on NaOH treated fibers. The fibers were treated with 5% benzoyl peroxide solution in
acetone for 40 - 45 minutes. After treatment, the fibers were thoroughly washed with distilled water and dried in hot air oven at 80C
for 24 hrs [10].
2.4 Treatment with maleic anhydride
Maleic anhydride (MA) is used as coupling agent in the treatment [11]. For the purpose of treatment with maleic anhydride (MA)
sisal fibers were soaked in a solution of maleic anhydride (10 wt. %) in acetone for 2 hrs at 55C. Following this the fibers were
rinsed to obtain pH=7 and dried at 105C until a constant mass of fiber was observed [12].
2.5 Fabrication of composite specimens
To investigate the effect of chemical treatment on the tensile and flexural properties of sisal/HDPE composites, the specimen for
tensile and flexural tests were prepared by injection moulding process. The tensile and flexural samples were prepared for varying
content of NaOH + MA treated fibers i.e. 7.5% and 30% in HDPE matrix. To see the effect of chemical treatment of NaOH + MA
and NaOH + BP + MA on tensile and flexural behavior, the specimen were also prepared by reinforcing 7.5% and 30% treated

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(NaOH + BP + MA) sisal fibers in HDPE matrix. The composition of various specimens is given in Table 1 and 2. The density of
sisal fibers (f)= 1.45 g/cc [13] and density of HDPE (m)= 0.94 g/cc [14] and Vf and Vm are wt.% of sisal fiber and HDPE matrix
respectively.
Table 1. Composition of composite specimens (NaOH + MA treated sisal/HDPE composites).
Sisal fiber (Vf )

HDPE (Vm)

7.5

Fresh
46.25

Recycled
46.25

30

35

35

Sample density
=(f Vf+m Vm)/100
0.9783
1.0930

Table 2. Composition of composites specimens (NaOH + BP + MA treated sisal/HDPE composites).


Sisal fibers(Vf)

HDPE (Vm)

Sample density
= (f Vf+m Vm)/100

Fresh

Recycled

7.5

46.25

46.25

0.9783

30

35

35

1.0930

The dimension of the sample and die for tensile and flexural specimens are strictly according to ASTM D638 (2010) and ASTM
D790 (2002) standards respectively.
2.6 Tensile and flexural testing
The tensile tests of the fabricated samples were conducted according to ASTMD-638 standard and flexural tests were according to
the ASTMD-790 standard in Central institute of plastic engineering & technology (CIPET) Amritsar on a Universal Testing Machine
(UTM). Before performing the tests all the samples were conditioned by putting them in a controlled environment chamber (Make:
KASCO industries, Pune) at 25C and 50% RH. For tensile testing, dumbbell shaped samples were subjected to uniaxial tensile load
by gripping their ends in UTM (Model: SS UTM 1250, Capacity 250 KN, Make: P.S.I sales Pvt. Ltd.) by keeping a gauge length of
57 mm. The results were obtained at two different points, as mentioned in Table 3 and 4 by testing five similar specimens
corresponding to each composition which were averaged to estimate the tensile strength of composite specimens corresponding to
different compositions. In order to estimate flexural strength of composites specimens the short beam shear tests were conducted. It is
basically 3-Point bending test which leads to failure by inter-laminar shear strength. These tests were conducted on UTM over a spam
length of 107 mm.
2.7 Examination of fiber surface and fractography
The analysis of the fractured surface of the tensile samples and surface morphology of the treated sisal fibers were done with the
help of scanning electron microscopy (SEM). For SEM, JEOL scanning electron microscope (Model: JSM6510LV) has been used
having maximum magnification of 1 Lac. The samples for SEM observation were prepared with the JEOL fine coater (Model: JFC1600) by gold and platinum coating of 5 nm thickness.
3. Results and discussion
3.1 Effect of chemical treatments on sisal fibers
In order to investigate the effect of chemical treatments on the fiber, the morphology features of the sisal fibers were investigated
by SEM. The SEM images of the untreated and treated sisal fibers are shown in Fig. 1and Fig. 2. The surface of the untreated sisal
fibers appears very smooth due to the presence of oil and wax materials on the surface (Fig. 1a). The waxy matter provides plainness
and smoothness to fibers. When sisal fibers are treated with 10 wt. % NaOH the surface of the fibers becomes rough (Fig. 1b) due to
removal of waxy materials from the surface, thereby, enhancing the bonding between fiber and matrix during the fabrication of
composites. Further the NaOH treatment breaks bundled structure of the fibers as evident from Fig. 1b. The surface of the fiber gets
rougher when the NaOH treated fibers are treated with MA at 55C (Fig. 1b). The SEM image shown in Fig. 2b indicated that after
treating the fibers with NaOH followed by the BP treatment, wrinkles are formed on the surface and bundles are further converted
into fibrous form. Upon subjecting these fibers to MA treatment, micro fibril appearance is revealed on the surface and even tearing

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at some places occurs (Fig. 2a and 2c). The MA treatment seems to have detrimental effect on sisal fibers and may deteriorate the
mechanical properties of polymer composites.

(a)

(b)

Fig. 1 (a) Untreated sisal; (b) 10 wt.% NaOH treated sisal at room temperature

(a)

(b)

(c)

Fig. 2 (a) NaOH + MA treated fibers at 55C; (b) NaOH + BP treated at room temperature; (c) NaOH + BP + MA treated fibers at 55C.

3.3 Mechanical properties of composites


The tensile and flexural strength of the different composites specimens, obtained by averaging the five readings for five similar
specimens at each composition, are summarized in Tables 3 to 6.
Table 3. Tensile strength of HDPE compioste reinforced with NaOH + MA treated sisal fibers.
Sr. No.

Test standard

Sisal (Wt.%)

HDPE (50% fresh+50% recycled)

Tensile strength (MPa)

T1

ASTMD-638

7.5

92.5

19.27

T2

ASTMD-638

30

70

11.99

Table 4. Tensile strength of HDPE composites reinforced with NaOH + BP + MA treated sisal fibers.
Sr. No.

Test standard

Sisal (wt.%)

HDPE(50% fresh+50%recycled)

Tensile strength (MPa)

BT1

ASTMD-638

7.5

92.5

19.12

BT2

ASTMD-638

30

70

15.75

Table 5. Flexural strength of HDPE composites reinforced with NaOH + MA treated sisal fibers.
Sr. No.

Test standred

Sisal (wt.%)

HDPE(50% fresh+50%recycled)

Flexural strength (MPa)

F1

ASTMD-790

7.5

92.5

17.86

F2

ASTMD-790

30

70

13.93

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Table 6. Flexural strength of HDPE composites reinforced with NaOH + BP + MA treated sisal fibers.
Sr No.

Test standred

Sisal (wt.%)

HDPE(50% fresh+50%recycled)

Flexural strength (MPa)

BF1

ASTMD-790

7.5

92.5

16.37

BF2

ASTMD-790

30

70

17.80

(a)
(b)
Fig. 3 (a) Comparison of (a) tensile strength; (b) flexural strength of NaOH + MA and NaOH + BP + MA treated fiber composites.

The comparison of tensile strength of NaOH + MA and NaOH + BP + MA treated sisal fibers/HDPE composites specimens,
having 7.5% (specimens T1 and BT1) and 30% (specimens T2 and BT2) fibers reveals that the composites with lower content of
7.5% (both treated fiber composites) have almost equal tensile strength (Fig. 3a) However at higher content of 30% the BT2
composite specimen have significantly higher tensile strength than T2 specimen. It could attributed to more fibrous structure of sisal
fibers in T2 (Fig. 4b) than BT2 (Fig. 4d) specimen as result of which more voids are present in T2 specimen which causes a
significant decreases in tensile strength at higher fiber content.

(a)

(b)

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(c)

(d)

Fig. 4 SEM images of fractured tensile specimens: (a) 7.5% NaOH + MA treated sisal fibers; (b) 30% NaOH + MA treated sisal fibers; (c) 7.5 % NaOH +
BP + MA; (d) 30% NaOH + BP+MA treated composites.

Unlike NaOH + MA treated specimen, the flexural strength of NaOH + BP + MA treated sisal fiber composite specimen increase
with increase in fiber content from 7.5% to 30% (Fig. 3b). It appears that due to presence of more fiber in bundled form in NaOH +
BP + MA treated fiber composites, especially at higher fiber content of 30 %, these specimens are able to take more transvers load
and offer more stiffness than composites specimen BF1 with fiber content of 7.5%. The higher flexural strength of BF2 specimen
than the specimen F2 could also be attributed to the presence of sisal fiber in more bundled form in NaOH + BP + MA treated fibers
specimen. The bundling effect is not able to dominate at lower sisal fiber content of 7.5% as evident from comparison of specimen
BF2 and F2.Similar results are observed by Mishra et al. [15] in which the tensile strength of MA treated sisal fiber composites
decreased with increase of reinforcement in HDPE matrix.
4. Conclusion
x
x
x

x
x
x

The treatment of the sisal fibers with NaOH or NaOH + BP leads to remove the waxy material from the fiber surface and
enhances roughness of the fiber surface. The subsequent treatment with the coupling agent (viz. MA) breaks down the
bundled structure of the fibers. The effect being less pronounced in NaOH + BP treated fibers than the NaOH treated fibers.
The addition of recycled HDPE into fresh HDPE enhances the tensile strength by 12.9% and flexural strength by 47.5%.
The reinforcement of the chemically treated (viz. NaOH + MA and NaOH + BP + MA) fibers into HDPE matrix (50%
fresh+ 50% recycled) leads to reduce the tensile and flexural strength. The reduction observed in tensile and flexural strength
increase with increase with fiber content, except for the flexural strength of NaOH + BP + MA treated fiber composites
which increase with increase with fiber content from 7.5% to 30%.
The NaOH + BP + MA treated sisal fibers composites shows much higher tensile strength than the NaOH + MA treated
composites at higher fiber content (30 wt.%) of fiber whereas at low fiber content of 7.5% both the compositions have
almost equal tensile strength.
The flexural strength of NaOH + BP + MA treated fiber composites is significantly higher at 30 wt.% fiber content but
relatively lower at 7.5 wt.% fiber content when compared to composites containing the same amount of NaOH + MA treated
sisal fibers.
The lower tensile and the flexural strength of the composites than the pure HDPE samples are attributed the poor interfacial
bonding between fiber and matrix, owing to the presence of the voids at the periphery of the sisal fibers. The number of
voids, acting as stress raisers, increase with the increase fiber content thereby causing further decrease in tensile and flexural
strength.

Acknowledgements
The experimental and analytic facilities offered by CIPET, Amritsar and SIC, Punjabi university, Patiala are duly acknowledged.
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