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Characterisation Studies and Impact of Chemical Treatment on Mechanical

Properties of Sisal Fiber

Article  in  Instrumentation Science & Technology · January 2011

DOI: 10.1163/156855411X610250

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 Composite Interfaces 18 (2011) 527–541
brill.nl/ci

Characterisation Studies and Impact of Chemical Treatment

on Mechanical Properties of Sisal Fiber

Mohd. Akram Khan ∗ , Sapana Guru, Prabha Padmakaran, Deepti Mishra,

Manish Mudgal and Savita Dhakad
CSIR — Advanced Materials and Processes Research Institute (Council of Scientific and Industrial
Research), Hoshangabad Road, Bhopal 462 064 (M.P), India
Received 12 May 2011; accepted 29 August 2011

Abstract
The availability of natural fibers with their high performance and low cost contributes to a healthy ecosystem
and fulfills the economic interests of the society. Sisal fiber, which is easily cultivated, is one of the most
widely used natural fibers. For the present studies, characterisation of locally available sisal fiber of M.P.
state in India was carried out with the investigation on the effect of alkali treatment with a wide range of
different concentrations on the mechanical properties of sisal fiber. The physical and chemical properties of
sisal fiber were analyzed with known methods and results were found to be similar to earlier reported values.
Alkali treatment was carried out with different concentrations and mechanical properties were evaluated
with Lloyd Fiber Testing Instrument. The results show that the chemical treatment enhances the mechanical
properties of fiber up to a limit and is found to decrease with further increase in concentration. Scanning
Electron Microscopy was used to investigate the morphology of untreated and alkali treated sisal fibers
which indicated that the different concentrations of alkali alter the fiber surfaces with variations. Sisal fibers
before and after alkali treatment were characterised further by thermogravimetry to establish their thermal
stability, and measurements showed that alkali treated fiber became more thermal resistant than the untreated
fiber and it was also noticed that thermal resistance decreases at higher concentration.
© Koninklijke Brill NV, Leiden, 2011

Keywords
Sisal fibre, interface, alkali treatment, mechanical properties, SEM, thermal analysis

1. Introduction
Natural fibers have proved to be effective reinforcement in thermoplastic matrix
composites [1], and they have extensive application in building and civil engi-
neering fields [2]. The ease of availability and biodegradability aspect of natural
fibers contribute to a healthy ecosystem while their low cost and high performance

* To whom correspondence should be addressed. E-mail: mohdakramkhan@rediffmail.com;

akramkhan@ampri.res.in

© Koninklijke Brill NV, Leiden, 2011 DOI:10.1163/156855411X610250

528 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

are able to fulfill the economic interests of communities and industries. Natural
fibers such as sisal, jute, coir, banana and others are classified as lignocellulosic
fibers [3]. Agava sisalana for example is a monocotyledon plant and member of
family Agavaceae which comprises some twenty genera. The genus Agava con-
tains 300 species which are native to North or South America [4]. A few species of
A. sisalana are grown commercially and from these, the greater part of the world’s
hard fiber is obtained. A. sisalana is the most important species of the genus Agava.
Sisal fiber is one of the most widely used natural fibers and is very easily cultivated.
The fiber is obtained from the leaves, which arise from the bole of the plant in close
rosette which is triangular in cross-section but becomes thinner and more flattened
towards the tip which generally bears a terminal spine shape. Agava sisalana is a
xeropytic plant that will not grow well in poorly drained soil. It is in the wet season
that the plant produces new leaves, so it does need a certain rainfall if it is to be
cultivated profitably and in sufficiently large quantities [4].
Sisal fiber is a strong leaf fiber with short renewal time. Sisal stalk grows to
about one meter in height and the fiber is contained in the lance shaped leaves
that grow out from the stalk in a dense rosette. Sisal plant produces about 200–
250 commercially available leaves and each leaf contains 1000–1200 fiber bundles
which is composed of 4% fiber, 0.75% cuticle, 8% dry matter and 87.25% water
[5]. Tanzania and Brazil are the two main sisal fiber producing countries in the
world [5]. Wilson [6] indicated that sisal fiber contains 78% cellulose, 8% lignin,
10% hemi-cellulose, 2% wax and about 1% of ash by weight, but Rowell et al.
[7] found that sisal contains 43–56% cellulose, 7–9% lignin, 21–24% pentose and
0.6–1.1% ash. Chand and Hashmi [8] showed that the cellulose and lignin content of
sisal vary from 49.62 to 60.95% and 3.75 to 4.40%, respectively. The large variation
in chemical compositions arises from different sources, age, extraction methods,
etc.
At present sisal fibers are used as ropes for the marine and agriculture industry.
Other applications of sisal include twines, cords, upholstery, padding, mat making,
fishing nets, fancy articles such as purses, wall hangings, table mats, etc. Sisal fiber
is also used as reinforcement in polymer matrix composites and is attracting more
attention for manufacturing low cost composite building materials in developing
countries [9–12]. Natural fiber based composites are environmentally friendly to a
large extent. In the case of synthetic fiber based composites, despite their useful-
ness in service, they are difficult to recycle and re-process after service life [2]. The
hydrophilic character of natural fibers leads to composites with weak interfaces.
Sisal fibers are hydrophilic in nature because they are derived from lignocellu-
losics, which contain strongly polarized hydroxyl groups [13]. They also possess
surface impurities such as wax and natural oils and sometimes processing oils are
also deposited at the surface. The effects of surface modification, such as dewax-
ing, alkali treatment, etc. on the properties of fibers and biocomposites, have been
studied recently in order to overcome some inconvenience associated with the use
of lignocellulosic fibers.
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 529

Cellulose forms the main structural constituent of plant fibers and contributes
immensely to the mechanical properties of plant fibers. Components such as lignin
and hemi-cellulose play an important part in the characteristic properties of the
fibers. Toughness is the tendency of plant fibers to absorb energy in impact and is
decreased with a decreasing amount of lignin and hemi-cellulose while at the same
time the strength and stiffness of the fiber is increased up to a limit. These fibers,
therefore, are inherently incompatible with hydrophobic matrices [14]. The major
limitations of using these fibers as reinforcement in such matrices include poor
interfacial adhesion between polar hydrophilic fiber and a non-polar hydrophobic
matrix [13]. Pretreatment of the fiber can clean the fiber surface, chemically modify
the surface, stop the moisture absorption process and increase the surface roughness
which improves adhesion between fiber–matrix although loss of fiber strength may
occur simultaneously [14].
In the present study, the characterisation of sisal fiber found locally as well as me-
chanical properties of these sisal fibers before and after alkali treatment have been
evaluated. The effect of surface modification on tensile strength, Young’s modu-
lus and elongation at break of the sisal fiber after different concentration treatment
are also analyzed and discussed. Scanning electron microscopy has been used to
investigate the morphological changes on untreated and alkali treated sisal fibers.
Thermogravimetric analysis was done to study the thermal behaviour of sisal fiber
before and after alkali treatment.

2. Material and Methods

Sisal fibers, from the species A. sisalana were supplied by a local agency of Madhya
Pradesh, India. The sisal fibers used for the present study were four to six years of
age.

2.1. Physical Properties of Sisal Fiber

2.1.1. Density
The fiber density was measured using Citizen analytical density meter. It is based
on the comparison of sample mass in air (weight on top pan) to the same sample
mass in liquid (on bottom pan). The programme calculates the density of the sample
and displays it.

2.1.2. Diameter
The diameter was determined by using the Scanning Electron Microscope (Jeol,
Japan) and M/s Oxford, UK Model JSM5600/LINK ISIS300.

2.1.3. Fiber Length

The length of the fiber was measured by physical means taking the length of 10
fibers at a time. The average of length of 10 fibers was considered as fiber length.
530 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

2.2. Chemical Properties of Sisal Fiber

2.2.1. Holocellulose
The carbohydrate portion of the vast majority of plants is composed of cellulose
and hemi-cellulose polymers with minor amounts of other carbohydrate polymers
such as starch and pectins. The combination of cellulose and the hemi-celluloses is
called holocellulose and usually accounts for 65–70% of the plant dry weight. These
polymers are made up of simple sugars, mainly D-glucose, D-mannose, D-galactose,
D -xylose, L -arabinose, D -glucuronic acid, and lesser amounts of other sugars such
as L-rhamnose and D-fucose. These polymers are rich in hydroxyl groups which are
responsible for moisture sorption through hydrogen bonding [15].
2.2.2. Procedure to Estimate Holocellulose
2.5 g of sample was weighted in conical flask. 80 ml of hot distilled water, 0.5 ml
acetic acid, and 1 g of sodium chlorite was added and filled to make the solution up
to 250 ml. The mixture was heated on a water bath at 70◦ C. After 60 min, 0.5 ml of
acetic acid and 1 g of sodium chlorite was added. After each succeeding hour, fresh
portions of 0.5 ml acetic acid and 1 g sodium chlorite were added with shaking. Ad-
dition of 0.5 ml acetic acid and 1 g of sodium chlorite was repeated until the fibers
were completely separated from lignin. It usually requires 6 h of chloriting, and the
sample can be left without further addition of acetic acid and sodium chlorite in the
water bath overnight. At the end of 24 h of reaction, the sample was cooled and
the holocellulose filtered off onto filter paper until the yellow color (the color of
holocellulose is white) and the odor of chlorine dioxide was removed. The holocel-
lulose was filtered, washed with acetone, oven dried at 105◦ C for 24 h, placed in a
desiccator for an hour and weighed [15].
2.2.3. Cellulose
Cellulose is the most abundant organic chemical on the face of the earth. It is a nat-
ural polymer consisting of D-anhydro-glucose (C6 H11 O5 ) repeating units joined by
β-(1–4)-glucosidic linkages at C1and C5 position. The degree of polymerization is
around 10 000 and each repeating unit contains three hydroxyl groups. These hy-
droxyl groups and their ability to hydrogen bond play a major role in directing the
crystalline packing and also govern the physical properties of cellulose. Solid cel-
lulose forms a microcrystalline structure with regions of high order, i.e., crystalline
regions, and regions of lower order, i.e., amorphous regions. Cellulose is resistant
to strong alkali but easily hydrolyzed by acid to water soluble sugars [13].
2.2.4. Determination of Cellulose Content
1 g of the sample was weighed and placed inside a beaker where 25 ml of 80% acetic
acid, 1 ml of concentrated nitric acid and 4 glass beads were added and the mixture
was refluxed for 20 min on cellulose refluxing apparatus. The fibre was washed into
a 50 ml centrifuge tube with hot 95% ethanol. The liquid was decanted, 95% ethanol
was added, and the whole stirred and centrifuged for another 5 min. The liquid was
decanted, the sample washed with hot 95% ethanol and filtered by suction. The
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 531

sample was washed three times with hot benzene, two times with 95% ethanol and
once with ether. The sample was placed inside a weighed crucible that was later
placed in the oven maintained at 105◦ C for 1 h. The crucible was later cooled in
desiccators and weighed. The percentage cellulose was calculated as follows [1],
α-cellulose (%) = (W2 /W1 ) × 100, (1)
where W2 is the weight of the oven-dry α-cellulose residue and W1 is the weight of
the original oven-dry holocellulose sample.
2.2.5. Hemi-cellulose
The hemi-cellulose fraction of plants consists of a collection of polysaccharides
composed of a combination of 5- and 6-carbon ring sugars. Hemi-cellulose dif-
fers from cellulose in three aspects. First, it contains several different sugar units
whereas cellulose contains only 1-4-β-D-glucopyranose units. Secondly, it exhibits
a considerable degree of chain branching containing pendant side groups that give
rise to its non-crystalline nature, whereas cellulose is a linear polymer. Thirdly, the
DP of hemi-cellulose is lower at around 50–300, whereas that in cellulose is 10–
100 times higher than that of hemi-cellulose. Hemi-cellulose is very hydrophilic,
soluble in alkali and easily hydrolyzed in acids [13].
2.2.6. Determination of Hemi-cellulose
2 g of oven dried holocellulose was weighted and placed into a beaker. 24% KOH
was added to the flask and samples were allowed to stand for 2 h. The mixtures
were filtered with and washed with additional KOH solution and the filtrate was
transferred into a beaker. The hemi-celluloses are then quantitatively precipitated
by the addition of alcohol (ethanol). The precipitated hemi-celluloses were isolated
by centrifuging for 10 min. The isolated hemi-cellulose was washed with alcohol
(ethanol) and ether and finally transferred into a crucible. The samples were dried
in an oven for 2 h at 105◦ C. After this, they were transferred into desiccators and
allowed to cool for 30 min after which their weights were taken. Hence, the per-
centage hemi-celluloses compositions of the samples were calculated as follows
[1].
Hemi-cellulose (%) = (W2 /W1 ) × 100, (2)
where W2 is the weight of the oven-dry hemi-cellulose residue and W1 is the weight
of the original oven-dry holocellulose sample.
2.2.7. Lignin
Lignins are amorphous, highly complex, mainly aromatic, polymers of phenyl-
propane units. They are totally insoluble in most solvents and cannot be broken
down to monomeric units. Lignin is totally amorphous and hydrophobic in nature.
It is the compound that gives rigidity to the plants. It is a complex three-dimensional
copolymer of aliphatic and aromatic constituents with very high molecular weight.
Hydroxyl, methoxy and carbonyl groups have been identified in lignin. Lignin has
been found to contain five hydroxyl and five methoxyl groups per building unit. It
532 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

is believed that the structural units of lignin molecule are derivatives of 4-hydroxy-
3-methoxy phenyl-propane. It is not hydrolyzed by acids, but it is soluble in hot
alkali, readily oxidized, and easily condensable with phenol [13].
2.2.8. Procedure to Estimate the Lignin Content
Approximately 200 mg of dried sample was weighed into a 100 ml centrifuge tube
(a sample was prepared by the same procedure as for holocellulose). To the sample
1 ml of 72% (w/w) H2 SO4 was added for each 100 mg of sample. The mixture
was stirred and dispersed thoroughly with a glass rod twice, then the tubes were
incubated in a water bath at 30◦ C for 60 min. The sample was removed and residue
was filtered. The residue was washed thoroughly with hot water and dried at 105◦ C
overnight. Lignin content was calculated from weights [15].
2.2.9. Wax
The extraction of wax was carried out by a Soxhlet apparatus using hexane treat-
ment for 8 h. The recovered extract was concentrated by rotary evaporator. After
the treatment, the sisal fibers were dried at 100◦ C overnight and the weight loss
was measured [16].
2.2.10. Moisture
The moisture content was determined by the percentage difference between the
initial weight of the sample and weight after 4 h oven drying at 105◦ C [16, 17].
2.3. Alkylation
Sisal fibers were washed with distilled water and finally dried in an oven. The dried
fibers designated as untreated fibers were subjected to alkali surface modification.
In the alkaline treatment, fibers were immersed in different concentrations of alkali
(NaOH) solution (1, 2, 5, 10, 15, 20, 25 and 30%) at 27◦ C for 4 h and then the fiber
was washed with distilled water repeatedly and finally with water containing acetic
acid to neutralize the excess sodium hydroxide and then the sample thoroughly
rinsed with distilled water. The fibers were then dried in an oven at 105◦ C for 24 h
[18, 19].
2.3.1. Mechanism of Alkylation
Alkali treatment of natural fibers, also called mercerization, is a common method
of chemical treatment. Alkali treatment leads to the increase in the amount of
amorphous cellulose at the expense of crystalline cellulose [20, 21]. The impor-
tant modification occurring here is the removal of hydrogen bonding in the network
structure. The reactions of NaOH with –OH groups of natural fibers and cellulose
are shown in Figs 1 and 2, respectively. Addition of aqueous sodium hydroxide to
natural fiber promotes the ionization of the hydroxyl group to the alkoxide [22]:
Fiber–OH + NaOH −→ Fiber–ONa+ + H2 O. (3)
This treatment removes a certain amount of lignin, wax and oils covering the exter-
nal surface of the fiber cell wall, depolymerizes the cellulose and exposes the short
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 533

Figure 1. Reaction of NaOH with –OH groups of natural fibers.

Figure 2. Reaction of NaOH with –OH groups of cellulose.

length crystallite [23]. Mercerization increases the number of possible reactive sites
and allows better fiber wetting.
2.4. Determination of Mechanical Properties of Sisal Fiber
Tensile testing of untreated as well as alkali treated fibers of different ranges was
conducted on Lloyd Fiber Testing Instrument. Fibers of known diameter were
mounted on a cardboard window of 50 cm and then the window was mounted in
between he jaws of the instrument. Tests were conducted at a cross-head speed of
2 mm/min. 10 samples of each fiber were tested to ascertain the tensile strength.
2.5. Scanning Electron Microscopy
The SEM micrographs of sisal fiber surfaces of untreated and alkali treated fibers
were taken using a Scanning Electron Microscope Make JEOL, Japan and M/s Ox-
ford, UK Model JSM5600/LinkISIS300 Resolution 3.5 nm/138 eV. The SEM has a
magnification limit of 1 Lakh times.
2.6. Thermal Analysis
Thermogravimetric analysis was carried out using a Mettler Toledo (Model-
TGA/DSC-1 Star) instrument. Samples were heated from 50 to 600◦ C with the
heating rate 10◦ C min−1 in nitrogen air atmosphere.

3. Results and Discussion

The physico-chemical properties of untreated sisal fiber are reported in Table 1.
The variation in mechanical properties of untreated and alkali treated sisal fiber are
534 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

Table 1.
Untreated sisal fiber properties

Properties
Density Diameter Fiber Holo- Cellulose Hemi- Lignin Wax Moisture
(g/cc) (µm) length cellulose content cellulose content content content
(m) (%) (%) (%) (%) (%) (%)

Results 1.25–1.35 150–190 0.9–1.10 77–85 65–73 9–11 5–6 0.9–1.2 9–11

Table 2.
Variation in mechanical properties of sisal fiber untreated and after treatment

S. no. Concentration Tensile Young’s Elongation

of treatment strength (MPa) modulus (GPa) at break (%)

1. Untreated 342 12.5 2.5

2. 1 360.2 14.3 3.3
3. 2 375.9 15.6 4.2
4. 5 320.7 14.8 3.8
5. 10 290.5 13.7 2.3
6. 15 267.5 12.4 2.7
7. 20 242.2 11.7 2.5
8. 25 219.5 10.4 2.6
9. 30 145.4 9.4 2.2

as in Table 2. The graphical representation of variation in tensile strength, Young’s

modulus and elongation at break for untreated and alkali treated sisal fiber is given
in Figs 3–5, respectively.
3.1. Mechanical Properties
Sisal fibers have been characterised by different authors from time to time through-
out the world. As is widely known many factors such as climatic conditions, age,
type of soil, extraction methods may severely affect the structure of fibers, their
chemical composition and physical properties.
The physical and chemical properties of untreated sisal fiber are shown in Ta-
ble 1. The untreated sisal fiber has density in range 1.25–1.35 g cm−3 , diameter
150–190 µm, fiber length 0.9–1.10 m and chemical composition values of holo-
cellulose 77–85%, cellulose 65–73%, hemi-cellulose 9–11%, lignin 5–6%, wax
0.9–1.2% and the moisture content in the fiber is found to be 9–11%. These values
are in agreement with other data for this type of lignocellulosic fibers as reported in
the literature.
Table 2 presents the mean of different mechanical properties of fiber before and
after each variation of alkali treatment. The highest and lowest values of tensile
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 535

Figure 3. Variation in tensile strength of sisal fiber.

Figure 4. Variation in Young’s modulus of sisal fiber.

strength for treated sample varied from 145.4 to 375.9 MPa with the highest value
for fiber treated with 2% alkali solution (Fig. 3). With increasing concentration of
treatment of alkali NaOH, decrease in tensile properties is observed. Chemically
536 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

Figure 5. Variation in elongation at break of sisal fiber. (a) Untreated sisal fiber, (b) 2% alkali treated
sisal fiber, (c) 5% alkali treated sisal fiber, (d) 20% alkali treated sisal fiber, (e) 30% alkali treated sisal
fiber.

Table 3.
Effect of different treatment methods on tensile properties of sisal fibre [24]

Treatments Tensile strength Tensile modulus Elongation

methods (g/tex) (×103 g/tex) at break (%)

Untreated 30.7 1.18 2.5

Benzol/alcohol 38.8 0.99 3.7
Acetic acid + alkali 9.3 0.39 2.6
Alkali 31.7 0.53 7.5
Acetylated 33.2 0.35 8.3
Thermal 42.0 1.22 3.5
Alkali thermal 27.6 0.70 4.7
Thermal alkali 25.7 0.71 4.4

treated sisal fibers showed a considerable decrease in tensile properties and this
decrease was attributed to the substantial delignification and degradation of cel-
lulose chains during chemical treatment. Chemical treatments have been found to
decrease the fiber strength due to breakage of the bond structure and disintegration
of the non-cellulosic materials [2].
The effect of treatment methods on tensile properties of sisal fiber is shown in
Table 3. It is observed that the fiber strength tends to increase up to 2% alkali treat-
ment and thereafter it tends to decrease. A similar pattern is also observed and
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 537

Table 4.
Variation in fiber tensile strength (MPa)
with different concentration [25]

Treatments Mean

None 324.2
0.25% NaOH 350.0
0.50% NaOH 372.8
1.0% NaOH 366.2
2.0% NaOH 375.4
5.0% NaOH 328.0
10.0% NaOH 296.9

reported in Table 4 where there is increase in strength of fiber up to 2% and be-

yond it shows a reducing trend. Similarly the values for Young’s modulus tested
were in the range of 4.4–15.6 GPa. The highest value reported was for 2% alkali
treated sample (Fig. 4). The elongation at break measurements were carried out for
the different treated fibers and they were in the range between 2.2 and 4.2% with
highest value again at 2% alkali treated sisal fiber (Fig. 5). There is a regular drop
in the properties after 2% of NaOH treatment up to 10% for treated fiber. The rest
of the values for elongation studies show (Fig. 5) no regular drop in values and
nearly the same values were found with only slight variation. Untreated sisal fibers
were found to have better mechanical properties than alkali treated sisal fiber at
higher concentrations.
3.2. Scanning Electron Microscopy
SEM micrographs of untreated and alkali treated (2, 5, 20 and 30% NaOH) sisal
fibers are shown in Fig. 6. As shown, Fig. 6(a) displays the micrograph of untreated
sisal fiber. It can be observed that untreated sisal fiber presents a network structure.
It can be observed as joined fiber bundles and presence of some cells on the sisal
surface derived from residues of parenchyma cells to which the fibers were bound
in the sisal plant [3]. When it is compared to alkali treated fiber, it is clear that there
are different morphological changes on the surface of the sisal fiber with different
concentrations. Figure 6(b) shows the sisal fiber after 2% alkali treatment and it
makes the sisal fiber slightly smoother. It can be observed from the micrograph
that 2% NaOH treatment does not cause major morphological changes on the fiber
surface. Figure 6(c) shows the 5% alkali treated sisal fiber and it can be observed
that treatment makes the sisal fiber surface even smoother.
Figure 6(d) and (e) shows 20 and 30% alkali treated sisal fiber, respectively. It
is evident from 20% alkali treated micrograph that a higher concentration of alkali
makes the fiber surface rougher and, from the SEM of 30% alkali treated sisal fiber,
it can be seen that at the higher concentration the alkali treatment leads to good
fiber bundle disaggregation [3]. As suggested by SEM micrographs, the chemical
538 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

(a) (b) (c)

(d) (e)

Figure 6. SEM images of (a) untreated and (b)–(e) alkali treated sisal fiber. (a) Untreated sisal fiber;
(b) 2% alkali treated sisal fiber; (c) 5% alkali treated sisal fiber; (d) 20% alkali treated sisal fiber;
(e) 30% alkali treated sisal fiber.

treatment tends to remove substances from the surface of sisal fiber and hence may
produce an improvement in the wettability property [25].
3.3. Thermogravimetric Analysis
Figure 7 gives the mass loss pattern of untreated sisal fiber and alkali treated sisal
fiber with different concentrations of alkali (NaOH) using measurements obtained
from TGA. The TGA graph was plotted with temperature (◦ C) along the x-axis and
weight retained (%) along the y-axis for untreated and alkali treated sisal fibers. The
weight loss of all samples up to 100◦ C was related to water loss associated with fiber
humidity. Despite fiber oven-drying before analysis, the total elimination of water is
made difficult by the hydrophilic character of the fibers, which present structurally
bound water molecules. It stands out that alkali treated sisal fibers present smaller
water loss. It was also observed that weight loss of sisal fiber decreases with in-
creasing concentration of alkali. This indicated lower hygroscopicity in relation to
that of untreated sisal fibers. The alkali treatment results in the partial extraction of
hemi-celluloses, which are highly hydrophilic and can be considered as the greatest
factor responsible for water absorption in lignocellulosic fibers, as they are more
accessible than cellulose chains of the crystalline regions [3].
It was observed that up to 200◦ C, untreated and alkali treated sisal fibers present
thermal stability, as the mass loss of all the samples was small. Thus, 200◦ C can
be considered the maximum application temperature of these fibers, since over this
temperature mass loss is large. From 300◦ C upwards, all samples present consid-
 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541 539

Figure 7. TGA graphs of untreated and alkali treated sisal fiber.

erable mass loss due to cellulose and hemi-cellulose decomposition. Over 400◦ C,
degradation occurs as a result of the break-up of the protolignin bonds [26, 27]. This
is also evident from Fig. 7 that as concentration of sodium hydroxide increased,
weight loss of fibers was found to decrease up to a limit. It is well established that
alkali treatment of natural fibres reduces the cementing material followed by the
removal of moisture, which makes the treated fiber more stable than the untreated
fiber. Thermogravimetric studies revealed that treated sisal fiber shows thermal re-
sistance between 2, 5, 10% (of 84.4, 89 and 88.9%, respectively) with respect to
untreated sisal fiber where 94% weight loss was observed at 600◦ C, it is also par-
tially due to the fact that some of the components of the fibre, such as lignocellulose,
that degrade at a lower temperature may be extracted during alkali treatment. It was
also found that weight loss was approximately similar at concentrations of 5 and
10% alkali. Alkali treated sisal fibers show decrease in thermal resistance when
subjected to higher concentrations of 20 and 30% where weight loss was 92 and
93% found at 600◦ C. It is an indication of the increase in amorphous cellulose at
higher concentration, which is known to have poor thermal resistance [28].

4. Conclusions
It can be concluded from the studies that there was an increase in mechanical prop-
erties, namely, tensile strength, Young’s modulus and elongation till 2% of alkali
treatment. It was observed that when sisal fiber was treated with more than 2% al-
540 M. A. Khan et al. / Composite Interfaces 18 (2011) 527–541

kali concentration, a regular fall in values for mechanical properties was observed,
which is due to excess delignification of the fiber.
It was observed from the micrograph study of sisal fiber that removal of impuri-
ties takes place after the alkali treatment. It may be an advantage for fiber–matrix
adhesion as it may facilitate both interlocking and the bonding reaction due to ex-
posure of hydroxyl groups to the matrices. Treated sisal fibres would have more
surface area compared to untreated fibres which may increase the adhesion between
the hydrophilic fibers and hydrophobic matrices. It was confirmed from the micro-
graph studies that higher concentration of alkali leads to fiber bundle disaggregation
which makes the fiber mechanically less resistant.
It was further confirmed from TGA studies that alkali treated sisal fibers are
thermally more stable than untreated fiber but at higher concentration of alkali,
amorphous cellulose increased which has poor thermal resistance, thus, making the
treated fibers less thermal resistant.

Acknowledgements
The authors are grateful to the Director, CSIR-AMPRI, Bhopal (M.P.), India for en-
couragement of the present research work and for permission to publish this paper.

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