Sci Eng Compos Mater 2017; 24(5): 731–738

Varun Mittal* and Shishir Sinha

Study the effect of fiber loading and alkali

treatment on the mechanical and water absorption
properties of wheat straw fiber-reinforced epoxy
composites
DOI 10.1515/secm-2015-0441 increasing worldwide in recent years [1, 2]. Owing to the
Received October 26, 2015; accepted February 26, 2016; previously low cost, low density, and effective mechanical proper-
published online March 30, 2016 ties of various natural fibers such as jute, bagasse, wheat
straw, rice straw, coir, and banana, it is possible to use
Abstract: The aim of this research was to study the fea-
them as replacements for synthetic fibers in a composite
sibility of using wheat straw fiber with epoxy resin for
application [3]. Various industries like packaging, auto-
developing natural fiber-polymer composites. For this
motive, and building construction have been encouraged
purpose, the epoxy resin was reinforced with 5, 10, 15,
to use biofibers in their applications in lieu of non-renew-
20, and 25 wt.% of the wheat straw fiber with the help of
able reinforcing materials [4–6]. The chemical composi-
the hand lay-up technique. Further, in order to improve
tion of wheat straw is similar to that of wood and cellulose
the composite characteristic, wheat straw fibers were
structures, which are embedded in an amorphous matrix
treated with three different concentrations of alkali (1%,
of hemicellulose and lignin. They have good mechanical
3%, and 5%). The mechanical and water absorption
strength. Various investigations have been carried out
properties of the treated fiber composites were charac-
on several types of biofibers such as coir, wheat straw,
terized and compared with those of untreated fiber-filled
banana, hemp, bamboo, and wood to study the influence
epoxy composites. It was observed that the mechanical
of these fibers on the mechanical and thermal properties
properties and water resistance were reduced with the
of composite materials. Some investigations have been
increase in wheat straw fiber loading from 5 to 25 wt.%.
carried out on wheat straw fiber (WSF) to study the effect
Among the three levels of alkali treatment, the compos-
of fiber on the mechanical and physical properties of com-
ite made with 3% alkali-treated fiber exhibited superior
posite materials.
mechanical properties than the other untreated and
­
For instance, Avella et al. examined the thermal and
treated fiber composites, which pointed to an efficient
mechanical properties of wheat straw-reinforced polyester
fiber-matrix adhesion. The scanning electron micro-
composites. Initially, WSF is treated with high-­temperature
scope was used to observe the surface features of the
steam, which provides the fiber a more reactive property
wheat straw fiber.
and more cellulose content. The authors reported that the
Keywords: composites; epoxy resin; mechanical proper- treated fiber composite has a higher value of the Young
ties; water absorption; wheat straw. modulus than the neat polyester. From their thermal
study, they found that the presence of WSFs in the com-
posite increases the rate of polyester crystallization; this
1 Introduction is due to the nucleating effect, while the crystalline of
samples remains unchanged [7]. Xiaoqun et al. analyzed
The requirement for natural fiber composite products the various properties of medium-density wheat straw
such as ply board, door panels, dashboards, etc., has been particle board using different adhesives like methyl-
ene diphenyl diisocyanate, urea formaldehyde, soybean
protein isolate, and soybean flour as well as chemical
*Corresponding author: Varun Mittal, Department of Chemical treatment of the wheat straw. They reported that among
Engineering, Indian Institute of Technology Roorkee, Roorkee
all adhesives, the particle board made from methylene
247667, Uttrakhand, India, Tel.: +91-9897154061,
e-mail: vrn.mttl1@gmail.com
diphenyl diisocyanate showed the best mechanical per-
Shishir Sinha: Department of Chemical Engineering, Indian Institute formance and water resistance than the other adhesives.
of Technology Roorkee, Roorkee 247667, Uttrakhand, India The treated wheat straw particle board had improved
732 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites

mechanical performance over the untreated wheat straw is a desirable material to make these types of board. From
particle board [8]. Panthapulakkal and Sain studied the the X-ray photo-electron spectroscopy results, they found
effect of molding techniques, compatibilizer, and fungal that urethane groups (-NH-C = O) are joined with the wheat
treatment of wheat straw and corn stem on the mechanical straw surface, which gives a positive effect on the strength
properties of the wheat straw/corn stem composites. They and thermal stability of composites [13]. Montaño-Leyva
reported that higher shear compounding of WSF compos- et al. studied the influence of fiber size (fiber median
ites showed similar properties to that composite produced diameter d50 = 1.1 mm, 62 μm, and 8 μm) on the mechani-
by the milled wheat straw. This is because fiber breakage is cal properties of the composites that were fabricated by
occurring during high shear compounding, which effects successive grinding processes (cut milling, impact milling,
the similar aspect ratio to that of milled straw. Compatibi- and ball milling, respectively). They reported that tensile
lizer and fungal treatment also enhanced the tensile and modulus and stress at break improved while strain at
flexural properties of the wheat straw polypropylene com- break was reduced by increasing the fiber content up to
posites [9]. Halvarssona et al. studied the mechanical and 11.1 vol.%. They found that the hydrophobicity of fibers
water absorption properties of medium-density fiber board can be increased by successive grinding, and small fibers
composites that are produced by various varieties of wheat have a large specific area for bonding. Interfacial adhesion
straw and different resin contents (14–17%) like urea mela- is better in the d50 = (8 μm > 62 μm > 1.1 mm) order, whereas
mine formaldehyde, a mixture of urea melamine formal- the fiber elongation (which reflects the fiber aspect ratio)
dehyde-resin, and urea melamine phenol formaldehyde. decreases in the order d50 = (1.1 mm > 62 μm > 8 μm) [14].
They observed that the average density is the factor that Babaei et al. analyzed the effect of (three levels of both
affects properties like internal bond, modulus of rupture, azodicarbonamide and nanoclay) loading on the mechani-
and modulus of elasticity. The water absorption and mate- cal and foaming properties of wheat straw flour/high-
rial swelling properties of composites decrease or increase density polyethylene composites. They observed that the
the density of straw. They also reported that increasing average cell size and cell density improved with the addi-
the melamine content in composites results in improve- tion of azodicarbonamide, but the simultaneous addition
ment in the water resistance and tensile properties [10]. of both azodicarbonamide and nanoclay reduced the cell
Pan et al. examined the influence of WSF content, size, size and improved the cell density. Mechanical resistance
and coupling agent on the mechanical characteristics of also went down with a decrease in the content of the azodi-
WSF-reinforced polypropylene composites. They observed carbonamide, whereas increasing the content of nano-
that increasing the WSF content up to 40% gives a better clay up to 2% enhanced the mechanical resistance. The
value of tensile strength and modulus but a lower value water absorption and thickness swelling properties also
of elongation. They also found that composites made by increased with the addition of azodicarbonamide [15]. Con-
fine particle fibers ( > 35 mesh) have a little bit high value of sequently, in this experiment, the effect of fiber content on
tensile strength. They reported that composites attained a the mechanical and water absorption behavior of the WSF
maximum value of mechanical strength at 10 wt.% maleic epoxy composites was analyzed. The outcome of integrat-
anhydride grafted polypropylene (MAPP) concentration, ing the three levels of alkaline treatment of WSF-epoxy
but the magnitude of the flexural modulus remained the composite is also reported.
same [11]. Reddy et al. examined the influence of fiber
content and coupling agent (maleic anhydride grafted
polypropylene) on the water absorption and flexural prop-
erties of WSF-reinforced clay composites. They reported
2 Materials and methods
that flexural modulus and resistance to water absorption
improved by raising the concentration of WSF and that of 2.1 Materials used
the coupling agent. From the scanning electron micros-
copy (SEM) morphology, they observed that addition of 2.1.1 Wheat straw fiber
coupling agent increases the interfacial adhesion between
the fibers and polymer matrix, thus affecting the flexural (i) WSF has been procured from a local agricultural
properties of composites [12]. Zhang et al. analyzed the farm in Meerut, Uttar Pradesh (India). The moisture
mechanical, thermal, and water absorption behavior of the content of fiber was found to be 6–7%. The length of
wheat straw reinforced with urea-formaldehyde adhesives WSF varied from 8 to 15 mm, with an average length
composite. They observed that the particle board formed of 12 mm. WSFs were washed with distilled water to
with WSF shows efficient mechanical strength; hence, it remove undesirable adhered impurities, followed
 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites 733

by drying in an oven at 72°C for 48 h to remove 2.2.4 Testing of mechanical properties

moisture.
(ii) Owing to their high strength, toughness, and resil- The tensile and flexural properties of the WSF-epoxy
ience, the epoxy resin AW106 and the curing agent ­composites were evaluated with a 2716-002 Instron Model
HV953IN were selected. When mixed, they give excel- 5982 (Grove city, PA, USA). These properties were deter-
lent resistance to chemical and moisture attack, with mined in accordance with the ASTM D3039 [18] and ASTM
outstanding electrical insulating properties. The D790 [19] procedure, respectively, at a cross-head rate
mixture has a density of 1.1 g/cm3. These were pro- of 2 mm/min. The dimension for the specimen were as
cured from M/S Petro Araldite Pvt. Limited, Manali, follows: tensile, 250 mm long and 25 mm wide; flexural,
­Chennai, India. 100 mm long and 25 mm wide.
(iii) Sodium hydroxide (NaOH) was procured from M/S The impact strength was calculated using an impact
Himedia Laboratories Pvt. Limited, Mumbai, India. testing machine, TINIUS OLSEN Model Impact 104
(­Hoorsham, PA, USA), with a hammer weighing 4 kg. It
was determined using ASTM standard D256 [20]. The test
2.2 Method used specimen had a dimension of 63.5 mm × 12.7 mm. Three
specimens were tested in each composite, and the average
2.2.1 Untreated fiber value of specimens was recorded. In all experiments, due
care was taken to check the reproducibility of data.
The WSF was rinsed with distilled water and dried in an
oven. The dried fibers were assigned as untreated fibers.
2.2.5 SEM morphology

An SEM study was conducted using LEO 435 VP with

2.2.2 Alkali treatment of the WSF the following specifications: acceleration voltage up to
30 kV, magnification range (10 × –300,000 × ), detection
WSF was soaked with a concentration of 1%, 3%, and 5% mode (secondary and backscattered electron), and use of
NaOH solution at ambient temperature for 2 h [16], then printer and camera to record images. The test sample was
washed with distilled water to remove the NaOH solution mounted on the apparatus after fusing with silver gel and
binding to the WSF, and dried in an air oven for 48 h at the coating with gold to avoid electrical charging during the
temperature of 72°C before making the composites. examination period.

2.2.6 Water absorption test

2.2.3 Preparation of composites
The effect of water absorption on the WSF-epoxy com-
For the preparation of the composites, the epoxy resin posites was calculated using ASTM D570 [21]. The test
(AW106) and curing agent (HV953IN) were mixed (as per specimen had dimensions of 76.2 mm length and 25.4 mm
the recommendation of the manufacturer) followed by width. The percentage of water absorption in the com-
adding (5, 10, 15, 20 and 25 wt.%) the untreated and 1%, posite material was determined by the weight difference
3%, and 5% alkali-treated WSFs, and stirred in a mixer between the sample immersed in distilled water and dry
for 10–15 min at a rotational speed of 223.6 g to obtain a sample, using the following equation
homogenous mixture. The mixture was poured into the
MF-MI
mold having a size of 300 × 300 × 10 mm3 and was cured %M = × 100. (1)
MI 
for 24 h at ambient temperature. All composite materials
made for this research were manufactured using the hand
lay-up technique [17]. In order to avoid the problem of
sticking of composite material, the mold was coated with
3 Results and discussion
Teflon sheet, which may lead to the problem of bubble
formation. To overcome such a problem, a roll-over sheet 3.1 Mechanical properties
with a heavy roller was incorporated. Every composite
cast was cured under a load of 25 kg for 24 h before it was Figures 1–5 show the effect of the WSF loading (5, 10, 15,
removed from the mold. 20, and 25 wt.%) and three levels of concentration (1%,
734 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites

Figure 1: Effect of fiber content and alkali treatment on the tensile

strength of WSF-epoxy composites. Figure 3: Effect of fiber content and alkali treatment on the flexural
strength of WSF-epoxy composites.

Figure 2: Effect of fiber content and alkali treatment on the tensile

modulus of WSF-epoxy composites.
Figure 4: Effect of fiber content and alkali treatment on the flexural
modulus of WSF-epoxy composites.

3%, and 5%) of alkali treatment of fibers on the tensile

strength, tensile modulus, flexural strength, flexural There was an improvement of approximately 11% in tensile
modulus, and impact strength of the WSF-epoxy com- strength and 4% in tensile modulus of the composite made
posites. A reduction in the mechanical properties of WSF- with 1% NaOH-treated fibers. Further, with the NaOH
epoxy composites was observed with the addition of the concentration increased to 3%, the tensile strength was
WSF in neat epoxy resin. This is due to the low strength changed from 12.8 to 15.8 MPa, and the tensile modulus
of the WSF and poor adhesion between the fiber and was also increased from 945 to 1315 MPa. Finally, when the
polymer matrix caused by a cluster of the fiber, resulting NaOH concentration was increased to 5%, we observed that
in the absence of polymer between the fibers. both tensile strength and tensile modulus decreased.
As seen from Figures 1 and 2, the tensile strength and Similarly, from Figures 3 and 4, the flexural strength
tensile modulus of the 1% alkali-treated fiber composites at and flexural modulus of the 1% alkali-treated fiber com-
5% fiber loading were 12.8 MPa and 945 MPa, respectively, posites at 5% fiber content were 26.5 MPa and 1663 MPa,
against the tensile strength and tensile modulus of untreated respectively, against the flexural strength and flexural
fiber composites (11.5 MPa and 906 MPa, respectively). modulus of untreated fiber composites of 23.8 MPa and
 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites 735

1496 MPa, respectively. An improvement of approxi-

mately 11% was observed in both flexural strength and
flexural modulus. Further, when the NaOH concentra-
tion increased to 3%, the flexural strength increased from
26.5 to 35.5 MPa and the flexural modulus also increased
from 1663 to 2200 MPa. Lastly, when the NaOH concentra-
tion was increased to 5%, we observed that both flexural
strength and flexural modulus decreased.
From Figure 5, WSF-epoxy composites showed low
impact strength compared to pure epoxy. The impact
strength of neat epoxy was 28.8 J/m; after the addition
of 5% untreated WSF in the polymer, the impact strength
of the composites was reduced to 25.2 J/m. The impact
strength of the 1% alkali-treated fiber composites remark-
ably increased from 25.2 to 28.7 J/m. Further, when the
Figure 5: Effect of fiber content and alkali treatment on the impact
NaOH concentration was increased to 3%, the impact
strength of WSF-epoxy composites.

Figure 6: SEM morphology of wheat straw: (A) untreated, (B) treated with 1% NaOH, (C) treated with 3% NaOH, and (D) treated with 5% NaOH.
736 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites

Figure 7: SEM morphology of tensile fractured surface of all composites: (A) untreated, (B) treated with 1% NaOH, (C) treated with 3% NaOH,
and (D) treated with 5% NaOH.

strength also increased from 28.7 to 29.6 J/m. Finally, up of crystalline cellulose that is surrounded by hemicel-
when the NaOH concentration was increased to 5%, the lulose and lignin. These cells have a long end and are
impact strength increased to 31.2 J/m. overlapping with each other, and form the cellular struc-
Similar results had been found in the case of coir-pol- ture. The NaOH reacts with hydroxyl groups, which are
yester composites [22]. As described above, the fibrillation available in the hemicellulose part of the fiber, which con-
provides a good interfacial adhesion between the fiber tributes to the death of the cellular part of the fiber and
polymer matrix. However, for the 5% NaOH-treated fiber thereby the fibers are broken into various filament parts.
composites, the mechanical properties decreased with the
greater fibrillation because the larger fiber at break led to
stress losses at the interface of the polymer and fiber. The 3.2 SEM analysis
maximum improvement in tensile and flexural properties
was observed in the 3% NaOH-treated fiber composites; The morphology of the fiber surfaces that were treated
however, the impact strength had a high value in the 5% with alkali at different levels is shown in Figure 6A–D.
NaOH-treated fiber composites. It was observed that the filaments in the untreated fiber
However, the effect of various levels of alkali treat- were joined together, but separated after the applica-
ment on WSF was observed to increase the above proper- tion of the alkali treatment. This process is termed as
ties of the composites at all the WSF contents investigated. branching, which means breaking the untreated fiber
Wheat straw is a natural lignocellulose fiber. WSF is made into smaller scales by the dissipation of the hemicellulose
 V. Mittal and S. Sinha: Effect of fiber loading and alkali treatment on WSF-epoxy composites 737

flexural, and impact strength of the all WSF-epoxy com-

posites decreased with the addition of fiber content in the
polymer matrix. All alkali-treated WSF-epoxy composites
exhibited better mechanical properties than the untreated
WSF-epoxy composites having the same fiber loading. This
is because their respective treatment constructed rougher
surfaces, which provided a strong bonding between the
fiber and polymer matrix. An efficient improvement in
tensile strength and flexural strength was observed in
composites prepared with the 3% NaOH-treated fiber, and
in the impact strength of composites prepared with the
5% NaOH-treated fiber. These results were supported by
SEM micrographs of the variously treated fiber surface,
showing that the fibrils in the untreated fiber were coupled
together but got split after the alkali treatment, offering
more surface available for the adhesion between the fiber
and polymer, increasing the strength of the composites.
Figure 8: Water absorption curve for the WSF composites.

present in the fiber. The branching increases the adhe- Nomenclature

sion surface area present between the fiber and polymer,
leading to a strong bonding between them [23]. Hence, M water absorption
alkali t­reatment helps improve the interfacial adhesion. MF weight after immersion in water
MI dry initial weight
Figure 7A–D represents the morphology of the tensile frac-
NaOH sodium hydroxide
tured surface of untreated, 1%, 3%, 5% alkali treated fiber SEM scanning electron microscopy
composites respectively [24]. WSF wheat straw fiber

3.3 Water absorption Acknowledgments: Varun Mittal is extremely grateful to

the Ministry of Human Resources and Development, New
Figure 8 shows the percentage intake of water absorbed in Delhi, for providing fellowship for this research work. The
untreated and various levels of alkali-treated WSF-epoxy authors are also thankful to the Department of Chemical
composites. It was observed that the natural fiber compos- Engineering, Indian Institute of Technology Roorkee, for
ites had higher water absorption than pure epoxy resin; providing us with the necessary equipment and technical
with increases in the fiber content in epoxy, water absorp- knowledge for the success of this research work.
tion also increases because the lignocellulose materials
absorb more water.
On the other hand, it was observed that the alkali References
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