Plastics, Rubber and Composites

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A review on the characterisation of natural fibres

and their composites after alkali treatment and
water absorption

M. Chandrasekar, M. R. Ishak, S. M. Sapuan, Z. Leman & M. Jawaid

To cite this article: M. Chandrasekar, M. R. Ishak, S. M. Sapuan, Z. Leman & M. Jawaid

(2017) A review on the characterisation of natural fibres and their composites after alkali
treatment and water absorption, Plastics, Rubber and Composites, 46:3, 119-136, DOI:
10.1080/14658011.2017.1298550

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Published online: 13 Mar 2017.

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PLASTICS, RUBBER AND COMPOSITES, 2017
VOL. 46, NO. 3, 119–136
http://dx.doi.org/10.1080/14658011.2017.1298550

A review on the characterisation of natural fibres and their composites after

alkali treatment and water absorption
a a b b c
M. Chandrasekar , M. R. Ishak , S. M. Sapuan , Z. Leman and M. Jawaid
a
Department of Aerospace Engineering, Universiti Putra Malaysia, Selangor, Malaysia; bDepartment of Mechanical and Manufacturing
Engineering, Universiti Putra Malaysia, Selangor, Malaysia; cLaboratory of Biocomposite Technology, INTROP, Universiti Putra Malaysia,
Selangor, Malaysia

ABSTRACT ARTICLE HISTORY

Natural fibre-reinforced polymer matrix composites are gaining increased attention among the Received 10 September 2016
researchers due to their low density, biodegradability, abundance, good mechanical properties, Revised 15 February 2017
etc. Significant amount of research works can be found on the material characterisation of Accepted 20 February 2017
natural fibres like hemp, flax, sisal, kenaf, coir and jute and their composites based on the
KEYWORDS
polymer matrices. Natural fibres are hydrophilic in nature and exhibit poor interfacial Natural fibres and their
adhesion between fibre and matrix. Modification of the fibre surface by chemical methods, composites; alkali treatment;
such as alkalisation, benzoylation and acetylation, has been used by researchers to improve material characterisation;
the above-mentioned shortcomings. This review paper focuses on the effect of alkali water absorption
treatment on the material properties of various natural fibres and their composites along
with their water absorption behaviour.

Introduction Despite the advantages, there are some serious set-

Synthetic fibre-based polymer composites have found
extensive applications in sports equipment, furniture,
aerospace, automotive industries, etc. due to their
high strength to weight ratio and excellent mechanical
properties. Specifically, high performance application
like aircraft structures heavily relies upon the synthetic
fibre-made composites. Commonly used synthetic
reinforcements include carbon, glass and aramid.
However, fossil fuel depletion and the other environ-
mental impacts associated with the production of the
synthetic fibres have made the researchers to look for
environment-friendly alternatives via natural fibres.
So, natural fibre is gaining increased attention among
the various researchers in recent years due to their
low density, good mechanical properties, biodegrad-
ability, sustainability, good thermal and acoustic prop-
erties, low cost and abundance. Natural fibres are
classified into different categories as per the chart
below (Figure 1) [1] and Figure 2 shows the picture
of various natural fibres [2].
Significant amount of research works can be
found on the material characterisation of natural
fibres like hemp, flax, sisal, kenaf, coir and jute
and their composites based on the polymer matrices.
In general, the molecular structure of these natural
fibres is made up of cellulose, hemicellulose, lignin,
pectin, wax and oils and the percentage of such sub-
stances present in various natural fibres is given in
Table 1 [3–5].
backs in using these natural fibres as reinforcement
in the composite materials. These include hydrophilic
nature of the fibres and poor fibre/matrix adhesion
characteristics. The moisture resistance and fibre/
matrix adhesion characteristics could be enhanced by
the modification of the fibre surface and removal of
the impurities like wax and oil, hemicellulose and
lignin.
Modification of the natural fibre surface
Fibre surface of a natural fibre can be modified by
means of physical methods and chemical treatment.
Physical methods involve stretching, calendaring,
cold plasma treatment, electric discharge method, etc.
[3]. Commonly used chemical methods for modifi-
cation of the fibre surface include alkalisation, acety-
lation, benzoylation, bleaching (baking soda) and
silane treatment [6]. The topic of interest of this
study is only the effect of alkalisation on the mechan-
ical, chemical and thermal properties of various natural
fibres and its composites along with their water absorp-
tion behaviour.
Alkalisation
Alkalisation, also known as the mercerisation process,
involves the immersion of natural fibres in concen-
trated sodium hydroxide (NaOH) solution. NaOH

CONTACT M. Chandrasekar chandrasekar.25j@gmail.com Department of Aerospace Engineering, Universiti Putra Malaysia, 43400 UPM Serdang,
Selangor, Malaysia
© 2017 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
120 M. CHANDRASEKAR ET AL.

Figure 1. Classification of various natural fibres [1].

Figure 2. Photographic images of the different types of natural fibres [2].

Table 1. Chemical composition of various natural fibres as reported by researchers [4,5].

Fibre Cellulose (wt-%) Hemicellulose (wt-%) Lignin (wt-%) Pectin (wt-%) Wax (wt-%) Moisture (wt-%)
Abaca 56–63 20–25 7–9 – 3 –
Bamboo 26–43 30 21–31 – – –
Flax 71 18.6–20.6 2.2 2.3 1.7 10.0
Hemp 70.2–74.4 17.9–22.4 3.7–5.7 0.9 0.8 10.8
Jute 61–71.5 13.6–20.4 12–13 0.2 0.5 12.6
Kenaf 72 20.3 9 – – –
Sisal 65 12 9.9 – 2 11.0
Coir 32–43 0.15–0.25 40–45 1.8 – 10.0

Figure 3. Typical structure of (i) untreated and (ii) alkali-treated
cellulose fibres [3].
reacts with the hydroxyl group of the natural fibres,
removes the hemicellulose, lignin, wax and oils that
surround the external surface of the fibre leading to
increase in the surface roughness (Refer to Figure 8),
aspect ratio and reduction in the fibre diameter and
results in a mercerised cellulose structure (as shown
in Equation (1)) which improves interfacial bonding
between the hydrophilic fibres and hydrophobic poly-
mer matrices [7].
Fibre-OH + NaOH
fibre-O-Na+ + H2 O (1)
A typical untreated natural fibre appears to be sur-
rounded by cementing materials like lignin, hemicellu-
lose and other impurities like wax and oils (Figure 3)
[1], whereas the alkali-treated natural fibres were
found to be clean and rough due to the partial removal
of lignin, hemicellulose and other impurities [8].
Alkali treatment of natural fibres results in the
increase of exposure of cellulose content in the fibre
surface (Table 3 where the percentage in cellulose con-
tent increases after the alkali treatment) [9–11], while
the hemicellulose and lignin get removed along with
the impurities like wax and oils [12]. Alkali treatment
also affects the crystalline properties by converting cel-
lulose I into cellulose II [13].
Material characterisation techniques
Material characterisation is an important aspect in
understanding the behaviour of natural fibres and
its composites to various loads and conditions,
water absorption, chemical treatment methods, etc.
(Figure 4). Mechanical characterisation involves the
testing of tensile, flexural, compressive, fatigue and
impact properties as per the respective ASTM stan-
dards. Thermal stability of the natural fibres and its
composites was studied by the use of thermo
Figure 4. Process undergone by the raw fibre and its composites.
PLASTICS, RUBBER AND COMPOSITES 121
gravimetric analysis (TGA), dynamic mechanical
analysis (DMA) and differential scanning calorimetry
(DSC), while the chemical composition characteristics
were analysed using FTIR and XRD spectroscopy.
Characterisation of the alkali-treated natural
fibres
Surface morphology
The surface morphology or microstructural changes in
the natural fibres after the alkali treatment have been
traditionally studied by several researchers using scan-
ning electron microscope (SEM) images (Figure 5).
The alkali-treated grass fibres were found to undergo
fibrillation (Figure 6) which is splitting of a single-fibre
bundle into smaller ones with the increase in alkali con-
centration due to the removal of cementing materials
and other impurities. Fibrillation and removal of
cementing substances along with impurities increase
the effective surface area for mechanical interlocking
between the matrix and fibre, thus improving the inter-
facial bonding [13,15,16]. Similarly, increment of fibril-
lation effects with the increase in alkali concentration
has been reported by Karthikeyan et al. on the coir fibres
[9]. Aydin et al. reported that fibrillation effect on the
flax fibres became more pronounced as the alkali con-
centration was increased to 30% [17]. Fibrillation effect
was also reported by Liu et al. on the hemp fibres treated
with 13 g L−1 NaOH for 3 h [18]. Another highlight of
subjecting the natural fibres to alkali treatment is the
increase in the degree of surface roughness as compared
to that of the untreated fibres due to the removal of lig-
nin and hemicellulose as reported by Punyamurthy et al.
on abaca fibres [6]. This characteristic of surface rough-
ness, due to the removal of lignin and hemicellulose with
the increase in NaOH concentration and immersion
time, was also reported by Sinha and Rout for the jute
fibres [19]. However, according to Liu et al., the increase
in alkali concentration leads to softening of the hemp
fibres as can be observed from their SEM images [18].
There exists an optimum concentration of NaOH
and immersion time, beyond which delignification of
the fibre takes place resulting in damaged fibre and
leading to decrease in the mechanical properties
[3,4]. Symington et al. also reported that over-treat-
ment of sisal, flax, kenaf and abaca fibres with alkali
can lead to fibre cracking and show detrimental effect
on the mechanical properties of the natural fibres.
They also emphasised that 10 min of NaOH treatment
of the natural fibres was sufficient to achieve the opti-
mal properties [20]. SEM micrographs of sisal fibres
122 M. CHANDRASEKAR ET AL.

Figure 5. SEM micrographs of flax fibres (a) untreated fibres and fibres treated with (b) 2.5%, (c) 5% and (d) 7% NaOH solution [14].

Figure 6. Fibrillation effect – SEM images of (a) raw Indian grass fibre, (b) grass fibre treated with 5% NaOH for 2 h, (c) 10% NaOH
for 4 h, (d) 10% NaOH for 8 h, and (e) 10% NaOH for 16 h [13].

Figure 7. SEM micrographs of sisal fibres (a) untreated raw fibre, (b) alkali-treated 5% for 4 h. (c) alkali-treated 10% for 4 h. (d)
alkali-treated 15% for 4 h [21].
treated with the increasing NaOH concentration levels
reveal that surface roughness of the natural fibres
increases with the increased NaOH concentration
(Figure 7).
Fiore et al. subjected the kenaf fibres to 6% NaOH
for 48 and 144 h, and they indicated that 48 h treat-
ment removed surface impurities and other cementing
substances and lead to increase in the mechanical prop-
erties, whereas 144 h treatment produced a detrimental
effect on the fibre surface (Figure 8) [22].
Alkali treatment causes formation of pores on the
surface of the sugar palm fibre (Figure 9) and decreases
their density and diameter due to the removal of
cementing substances and other impurities [23].
Thermal properties
The thermal stability of the various alkali-treated natu-
ral fibres was analysed by researchers using TGA, DSC
and DMA.
Figure 8. SEM images: (a) untreated kenaf fibres; (b) after 48 h in NaOH solution; and (c) after 144 h [22].
PLASTICS, RUBBER AND COMPOSITES 123
TGA
TGA is a thermal analysis technique in which a mass
change (in %), thermal decomposition temperature
and thermal stability of the natural fibre before and
after the NaOH treatment can be assessed [24].
Findings from TGA results of Puglia et al. indicate
that thermal stability of the alkali-treated flax fibres
(Phormium tenax) decreased slightly. Also, the alkali-
treated fibres have shown a reduced weight loss %
than the untreated flax fibres, indicating the removal
of cementing substances [25]. Similar results have
been reported by Zhu et al. based on their experiments
on flax fibres [26]. TGA results from Guduri et al.
were in contrast to the results by Puglia et al. in which
the thermal stability (temperature at maximum rate of
decomposition) of the flax fibres increased after the
alkali treatment. They also found that the thermal stab-
ility of the flax fibres relied upon the alkali concentration
and immersion time [8]. Borchani et al. reported that
temperature at maximum rate of decomposition
124 M. CHANDRASEKAR ET AL.
Figure 9. SEM images: (a) untreated sugar palm fibres (b) alkali-treated sugar palm fibres with pores on the surface [23].
increased with the increase in alkali concentration on
the Alfa fibres. According to them, the alkali-treated
Alfa fibres showed low moisture than the untreated
fibres [27]. Liu et al. reported that the temperature at
the maximum rate of decomposition obtained through
weight % and derivative weight % for the Indian grass
fibres increased with the increase in alkali concen-
tration, thereby resulting in the improvement of the
thermal stability of the fibre after alkali treatment.
This was due to the removal of hemicellulose and lignin
content after NaOH treatment [13]. Three-phase
characteristics of weight (mass) loss % with the increas-
ing temperature were obtained through the TGA results
by Zhu et al. on untreated/alkali-treated flax fibres [26].
Similar 3-phase characteristic of weight loss % with the
increasing temperature was also reported by Vasquez
et al. on the sweet sorghum fibres. First phase is credited
to the removal of moisture and second phase was attrib-
uted to the removal of cementing substances [7]. How-
ever, Kaushik et al. reported 2-phase characteristics of
weight loss % against the temperature range for sisal
fibres in which the first phase was attributed to the
breakdown of hemicellulose, glycosidic linkage and
loss of moisture, whereas the second phase of decompo-
sition was attributed to the cellulosic and lignin degra-
dation [21]. TGA results from Ray et al. on the jute
fibre-reinforced unsaturated polyester composite
showed a decrease in thermal stability after alkali treat-
ment [28]. Experiments by Fook and Yatim on the alkali
treatment of kenaf fibres with pH ranging from 8 to 14
showed that weight loss % increased (density decreases)
as a result of increase in pH, this was due to the etching
away of lignin, hemicellulose, pectin, etc from the kenaf
fibre due to the alkali treatment [29].
DSC
DSC thermogram was found to be highly helpful in
studying the thermal stability of the natural fibres
before and after the alkali treatment. It gives infor-
mation on thermal stability of the natural fibres
through the measurement of glass transition tempera-
ture (Tg), cold crystallisation peak temperature (Tc)
and melting temperature (Tm) as a function of temp-
erature [24]. Also, % of crystallinity can be obtained
from the DSC thermogram [30].
The parameters like Tg, Tc and Tm that can be
obtained from a typical DSC thermogram are shown
in Figure 10. The DSC results of various natural fibres
and their composites reported by some of the research-
ers are given in Table 2 (Figure 10).
DMA
DMA involves the measurement of change in stiffness
(loss modulus, storage modulus), damping (tanδ) and
glass transition temperature Tg of the composite with
untreated and NaOH-treated natural fibres. The for-
mula for tanδ is given in Equation (2):
′′ loss modulus
tan d = EE′ = (2)
storage modulus
According to Fiore et al., alkali treatment of kenaf
fibres led to a significant reduction and shifting of
the tanδ peaks of the composites reinforced with the
alkali-treated fibres compared to the composite made
from the untreated fibres. They indicated that stacking
sequence of the composite did not affect the loss
moduli and tanδ peaks [22]. Karsli and Aytac per-
formed DMA on flax fibre/poly-lactic acid (PLA)/PC
composite with untreated and alkali-treated fibres,
and they found that storage modulus increased with
the increase in alkali concentration, whereas peak of
tanδ decreased with the increasing alkali concentration
[30]. Results obtained by Guduri et al., on the storage
modulus and tanδ for the flax/bio-copolyester compo-
site, were in contrast to those of Karsli and Aytac, in
which the storage modulus decreased with the
 PLASTICS, RUBBER AND COMPOSITES 125

Figure 10. Tg, Tc and Tm from the DSC thermogram [31].

Table 2. Tg, Tc and Tm of various natural fibres before and after NaOH treatment obtained from the DSC thermogram.
Oil palm empty fruit bunch/PLA
Flax/PLA [17] [32] Hemp/PLA [33] PALF/PLA [34]
NaOH treated NaOH treated NaOH treated NaOH
Parametersa Raw (10 and 30%) Raw (3–7%) Raw (10, 20 and 30%) Raw treated 5%
Tg (°C) 62.45 51.76 and 46.18 57.0 59.7 57.8 (pure PLA) 56.5, 57.8 and 56.9 58 57
Tc (°C) 127.29 118.02 and 109.45 119.7 105.0 122.7 116.7, 105.1 and 108.6 97 85
Tm (°C) 152.64 142.81 and 141.58 140.5 and 147 143.9 and 151.5 152.3 150.9, 155.6 and 154.1 169 166
% Xc – – 30.52 43.11 20.4 25.2, 39.4 and 38.3 30.5 29.1
a
The numerical data reported here are identical to the data published by the cited researchers.

increasing alkali concentration and the tanδ peaks
shifted with the increasing NaOH concentration [8].
Chemical properties
The chemical composition of the untreated and alkali-
treated natural fibres have been studied by various
researchers using FTIR and XRD spectroscopy.
The chemical composition of a natural fibre is made
of cellulose, hemicellulose, lignin, pectin, moisture, wax
and oils (Table 1). Owing to the alkali treatment, the
percentage of these substances gets decreased or
removed as could be seen in Table 3.
FTIR spectroscopy
The analysis of alkali-treated and untreated natural
fibres using FTIR involves the measurement of
absorbance against the wavenumber range of 400–
6000 cm−1. In the plot, each characteristic peak corre-
sponds to the composition of natural fibres like
cellulose, hemicellulose, lignin, pectin and water mol-
ecules. The peak characteristics of the untreated flax
fibres, belonging to cellulose, pectin, lignin, etc., are
given in Table 4.
In general, on comparing the absorbance character-
istics of untreated fibres with alkali-treated fibres over
the wavenumbers, it can be observed that some of the
characteristic peaks, which can be seen in the case of
untreated fibres, disappear for the alkali-treated fibres.
This was attributed to the removal of cementing sub-
stances like hemicellulose, lignin, pectin and moisture.
The notable changes in the FTIR spectrum of alkali-
treated flax fibres, as observed by various researchers,
were the disappearance of characteristic peaks at cer-
tain range of wavenumbers 1735 and 1525 cm−1 and
indication of the removal of hemicellulose and lignin
[8,14,25,26]. In the case of the untreated flax fibres,
peak for hydroxyl group (−OH group) was higher.
This particular characteristic peak decreased after the
alkali treatment, indicating the removal of moisture

Table 3. Chemical composition of the jute and Alfa fibres Table 4. FTIR peak characteristics of untreated flax fibres [36].
before and after alkali treatment [27,35]. FTIR characteristics of the untreated flax fibres
Jute fibres Alfa fibres
Position/cm−1 Assignment Belonged chemicals
5% NaOH 1% NaOH
treated for treated for ∼3335 V (OH) free –
Component % Untreated 24 h Untreated 6h ∼2850 V (CH2) symmetrical Organic compounds
∼1735 V (C=O) ester Pectin
Cellulose 71.1 80.3 46.2 78.2 ∼1635 Adsorbed water All the chemicals
Hemicellulose 15.9 9.6 30.2 11.6 ∼1595 V (C=C) aromatic Lignin
Lignin 11.8 7.6 19.9 4.9 ∼1505 V (C=C) aromatic Lignin
Other components 1.2 2.5 – – ∼1155 V (C–C) ring breathing Largely from cellulose
(ash, water, pectin) ∼1105 V (C–O–C) glycosidic Cellulose
126 M. CHANDRASEKAR ET AL.
as well as hemicellulose and lignin which absorbs water
molecules [14]. FTIR results by El-shekeil on kenaf
fibre-based polyurethane composites indicated that
the characteristic peaks disappear at certain wavenum-
bers (1740 and 1250 cm−1), indicating the removal of
cementing substances like hemicellulose [24]. FTIR
spectroscopic results on the untreated and alkali-trea-
ted Alfa fibres showed that characteristic peak intensi-
ties (1731 cm−1 and broad absorption band at
3359.8 cm−1) diminish with the increasing alkali con-
centration. This was due to the removal of cementing
substances [37].
XRD analysis
XRD analysis involves studying the changes in crystal-
linity index (CI %) of the untreated and alkali-treated
fibres by measuring the minimum peak intensity or
height of the minimum intensity between major
peaks (corresponding to amorphous or non-crystalline
material) and maximum peak intensity or highest dif-
fraction peak (corresponding to crystalline material).
The formula for calculating crystallinity index is
given by Segal method as in Equation (3):
(I002 − Iam )
CI(%)=
I002
where I002 is the maximum intensity diffraction peak
measured at a diffraction angle of 2θ = 22.8° and Iam
is the minimum intensity diffraction peak measured
at a diffraction angle of 2θ = 18° [27,37,38]. Crystalli-
nity index of various natural fibres reported by the
different authors is given in Table 5.
The XRD results of Benyahia et al. on Alfa fibres
showed that both the crystallinity index (CI%) and
peak or maximum intensity increased due to the
NaOH treatment [37]. Hosur et al. studied the effect
of alkali treatment on the flax fibre structure using
XRD. According to them, the peak intensity tends to
increase with the increase in NaOH concentration
(2.5, 5 and 7%) [14]. However, the XRD results
obtained by Aydin et al. were in contrast to the results
obtained by Hosur et al. where the peak intensity
decreases with the increasing alkali concentration (10,
20 and 30%) for the flax fibres. The decreasing trend
Table 5. Crystallinity index of some of the natural fibres before
and after alkali treatment obtained through XRD – Segal
method.
Crystallinity index (CI %)a
Fibre Untreated Alkali treated Alkali concentration (%)
Alfa [27] 59.5 66.7
Flax [14] 72.6 78.9
Sisal [21] 71.7 74.3
Jute [39] 71.39 84.46
Hemp [39] 87.87 89.77 30
Kapok [39] 45.75 58.42
a
The numerical data reported here are identical to the data published by
the cited researchers.
was attributed to the conversion of crystalline I to crys-
talline II and increase in amorphous portion of the cel-
lulose [17]. However, according to the XRD results of
Borchani et al. for Alfa fibres, there was no transform-
ation of cellulose I into cellulose II [27].
Mechanical properties of the alkali-treated
natural fibres
Mechanical properties of some natural fibres along
with the synthetic fibres are given in Table 6 along
with the properties of synthetic fibres for comparison.
Hongling et al. studied the effect of various alkali
concentrations and immersion time of hemp fibres
through tensile and bending tests. According to their
results, the increase in alkali treatments increases the
tensile strength of the hemp fibres, whereas the bend-
ing modulus and flexural rigidity decreased as the
NaOH concentration was increased [18]. Alkali treat-
ment of coir fibres (3% for 5 h) tends to decrease the
tensile strength, tensile modulus and elongation %.
According to them, this was due to the etching away
of binding component between the micro-fibres [41].
Meheddene et al. showed that prolonged treatment
(1, 2, 4 and 10% for 2, 4 and 24 h) of the fan palm fibres
(3) with higher NaOH concentration could cause severe
deterioration in the tensile strength of the treated
fibres, whereas the tensile modulus and % of elongation
did not get affected by the alkali treatment process [42].
Kanchireddy and Muzenda coated the grass fibres with
polycarbonate and subjected them to alkali treatment.
They found that polycarbonate-/alkali-treated grass
fibre showed superior tensile strength than the
uncoated and raw fibre [43]. According to Wong
et al., the increase in alkali concentration leads to
reduction in strain at failure and ductility of the bam-
boo fibres [44]. Hashim et al. subjected kenaf fibres to
2% NaOH at 2 and 100°C for 30 and 480 min. From
their results, it was concluded that the immersion
time had a major impact on the tensile mean strength
value of the fibre, whereas the temperature had a small
impact [45]. Abdal-hay et al. found that ultimate tensile
strength and % elongation of the single fibre increased
significantly due to the alkali treatment (6% for 3 h)
[46]. According to Haameem et al., 10% NaOH-treated
Napier grass fibres showed better single-fibre tensile
properties compared to the untreated fibres [47].
Table 6. Mechanical properties of some of the natural fibres
and synthetic fibres [3,40].
Young’s
Density Tensile modulus Elongation at
1
Fibres (g cm−3) strength (MPa) (GPa) break (%)
2.5
5 Jute 1.3–1.45 393–773 13–26.5 1.16–1.5
6 Flax 1.50 345–2000 27.5–85 2.7–3.2
Hemp 1.14 690 30–60 1.6
8 E-glass 2.5 2000–3500 70 2.5
Carbon 1.7–1.9 4000 230–240 1.4–1.8
Aramid 1.4 2800–3600 80–190 2–4

Mechanical properties of the composites
reinforced with alkali-treated fibres
Mechanical properties of the natural fibres and their
composites depend on the type of plant fibre used,
type of matrix involved and interfacial adhesion
between the fibre and matrix [30]. The changes in
mechanical properties due to alkalisation have been
studied by various researchers by subjecting the
untreated and alkali-treated natural fibre and their
composites to tensile, compressive, flexural and impact
loads. Mechanical characterisation is done according to
the ASTM standards depending on whether the
material tested is fibre or composite and the type of
matrices involved.
This section describes the impact of alkali treatment
on the mechanical properties of various natural fibre-
based composites. Table 7 shows the parameters used
by various researchers to study the effect of alkali treat-
ment on the natural fibres and its composites.
Abaca fibre-reinforced composites
Shibata et al. treated abaca fibres with 2% NaOH for
2 h and studied its flexural properties through treated
and untreated fibre/biodegradable polyester composite,
and they found that considerable increment in flexural
strength was obtained for the composite with treated
fibres in comparison to the untreated fibre-based com-
posite [49].
Alfa fibre-reinforced composites
Both tensile and flexural strength/modulus of the Alfa
fibre-based polyester composites were found to be
improved by various concentrations of alkali treatment
(1, 3, 5 and 7% for 24 h) by Benyahia et al. [37].
According to Arrakhiz et al., 1.6 mol L−1 NaOH treat-
ment of Alfa fibres for 48 h resulted in better tensile
strength and young’s modulus than the untreated
fibre-based composite [50]. Based on their studies,
Rokbi et al. concluded that 5% NaOH-treated alfa
Table 7. Alkali treatment conditions of some natural fibres as reported by the researchers.
Fibres Matrix NaOH Concentration
Abaca [6] – 15 times the weight of
fibres
Alfa [37] Polyester 1, 3, 5 and 7%
Bamboo [44] Polyester 1, 3 ad 5%
Coir [5] Epoxy 5%
Flax [14] Polyester and Polyester 2.5, 5 and 7%
biopolymer blend resin
Jute [28] Vinyl ester 5%
Kenaf [45] – 2 and 10%
Sisal [48] Unsaturated polyester 2, 6 and 10%
Sugar Palm Epoxy 2.5 and 5%
[15]
PLASTICS, RUBBER AND COMPOSITES 127
(immersion time 24 h)/polyester composite led to sig-
nificant improvement in the flexural strength and
modulus [51].
Bagasse fibre-reinforced composites
Acharya et al. treated bagasse fibres with 5% NaOH for
2, 4 and 6 h. Best flexural properties of bagasse/epoxy
composite were achieved when 5% NaOH-treated
fibres with the immersion time of 4 h were used [11].
According to Vilay et al., alkali treatment and the
increase in fibre loading of the bagasse fibre in unsatu-
rated polyester composites resulted in higher tensile
and flexural properties in comparison to the composite
with the untreated fibres [52].
Bamboo fibre-reinforced composites
KJ Wong et al. studied the effect of alkali treatment (1,
3 and 5%) on density and tensile properties of the bam-
boo fibre-based polyester composite, and they indi-
cated that density of the composites decreased with
the increase of NaOH concentration, leading to higher
porosity, resulting effect due to the removal of cement-
ing composites. Based on their results, inter facial shear
strength (IFSS) was found to increase, while the per-
centage improvement falls with the increasing alkali
concentration [44]. According to Lu et al., composite
with 2% NaOH-treated bamboo fibre/epoxy resin
showed improvement in tensile strength and %
elongation at break by 71 and 53%, respectively [53].
Banana fibre-reinforced composites
Venkateshwaran et al. treated banana fibres with 0.5–
20% NaOH concentration for 30 min and studied the
tensile, flexural and impact properties of the epoxy-
based composite reinforced with treated and untreated
fibres. Among the various concentration levels, 1%
NaOH treatment produced the best tensile, flexural
and impact properties which was attributed to the
Soaking
time Soaking temperature Drying
72 h 30°C Dried at room temperature for 48 h
24 h 25°C 80°C for 48 h
24 h Room temperature 24 h under sun
1/2 h 20°C lab temperature 24 h in open air and 50°C in the oven for 8 h
1h Room temperature 80°C for 24 h
2, 4, 6 and 30°C Room temperature for 48 h followed by oven
8 drying for 100°C for 6 h
½ and 8 h Room temperature 100–105°C for 1 h
and 100°C
2, 3 and 65°C under constant Open air for 4–5 days
5h stirring
1, 4 and Room temperature Dried at room temperature for 4 days
8h
128 M. CHANDRASEKAR ET AL.
improved interfacial adhesion. They also observed that
high concentration level of NaOH leads to deterio-
ration of the mechanical properties which was due to
the fibre damage caused by the alkali treatment [54].
Curua fibre-reinforced composites
Gomes et al. dipped curua fibres into 5, 10 and 15%
NaOH concentration for 1 and 2 h. They found that
the tensile strength and fracture strain of alkali-treated
fibre/biodegradable corn starch composite was higher
than the composite with the untreated curua fibre [55].
Coir fibre-reinforced composite
According to Yan et al., 5% NaOH concentration for
30 min resulted in higher tensile, flexural strength and
modulus of the coir fibre-based composites [5]. Exper-
imental investigation on alkali treated (2, 4, 6 and 8%
for 10 days) coir fibre-based epoxy composite by
Karthikeyan revealed that impact strength was better
for the composites with alkali-treated fibres than the
untreated fibre-based composites [9]. According to
Gu Huang, during NaOH treatment of coir fibres at
2, 4, 6 and 8% for 4 weeks, there was no significant
difference in the tensile strength of treated fibre/PP
composite even after immersing for 4 weeks. Their
hypothesis for negligible change in tensile strength
for various concentration levels of NaOH was due to
the improved fibre/matrix adhesion [56]. According
to Arrakhiz et al., tensile properties of 1.6 mol L−1
NaOH-treated coir fibre/HIPS composite with the
immersion time of 48 h showed only a 10% improve-
ment compared to the untreated fibre-based compo-
site [57].
Flax fibre-reinforced composites
Merlin et al. utilised higher concentration of NaOH
(10, 20 and 30%) on the short fibre/poly-lacic acid
composites and found that tensile modulus decreases
gradually with increasing NaOH concentration. The
decrease in tensile modulus was attributed to the
heavy damage on the fibres caused by the increased
alkali concentration [17]. Karsli and Aytac found
that 2% alkali-treated flax fibres with the PLA/PC
composites showed the highest tensile strength and
modulus compared to the composites with 5% and
10% NaOH concentration [30]. Van de weyenberg
et al. performed NaOH treatment of various concen-
tration levels on the unidirectional flax fibres and
they found that when the concentration of NaOH
was raised beyond 23%, both the longitudinal and
transverse tensile strength of the treated fibre/epoxy
composite declined significantly, indicating the
damage on the treated fibres at such high concen-
trations. According to them, even a 4% NaOH
treatment for 45 seconds was sufficient to achieve
30% increment in transverse tensile strength and
treatment of flax fibres at high concentration level
beyond 10% could lead to the deterioration in the
longitudinal and transverse tensile strength [58].
Grass fibre-reinforced composites
Impact strength of the Napier grass fibre-based epoxy
composites showed an increasing trend with the increase
in fibre weight % and alkali concentration. The highest
impact strength was obtained for composites with 2%
NaOH-treated fibres and 20% fibre loading [10].
Hemp fibre-reinforced composites
Based on the results of Islam et al., it can be concluded
that the alkali treatment of hemp fibre-reinforced
PLA composites with 30% fibre loading leads to sig-
nificant improvement in the interfacial bonding
between the fibre and matrix which, in turn, leads to
the higher mechanical properties [59]. Similar
improvements in the mechanical properties of
hemp/polylactide composites due to 5% NaOH treat-
ment for 30 min and with the increase of fibre loading
were reported by Moyeenuddin et al. They also high-
lighted that 30% weight of fibre loading with the
alkali-treated fibres in the composite gave the best
tensile, flexural and impact properties [60]. Suardana
et al. performed alkali treatment at various concen-
tration levels (2, 4 and 6% at 70°C for 1 h) on
hemp/PP composites and found that alkali treatment
improved the tensile and flexural strength, indicating
the enhanced wettability between fibre and matrix.
Among the various concentration levels utilised, 4%
NaOH treatment of fibres leads to the best mechanical
properties of the composite [61].
Jute fibre-reinforced composites
The mechanical properties of jute fibre-reinforced
vinyl ester composite showed a declining trend with
the increase in alkali concentration and immersion
time [35]. Owen subjected jute fabric to 20% NaOH
for 25 min at room temperature and found that the
epoxy composites reinforced with alkali-treated jute
fabric produced better tensile, flexural and impact
properties than the composite with untreated fibres
[62]. Leela et al. reported an increase in tensile strength
of jute fibre-reinforced polypropylene composite for
20% fibre loading and up to 10% NaOH concentration.
Also, tensile modulus increased with the increase in
fibre loading and NaOH concentration, whereas %
elongation at break for the composites showed a
steep declining trend with the increasing fibre loading
and NaOH concentration [63].

Kenaf fibre-reinforced composites
Fiore et al. performed experiments on kenaf/epoxy
composites with the fibres treated with 6% alkaline
for long immersion time 48 and 144 h. They found
that the tensile strength improved for composite with
48 h NaOH-treated kenaf fibres which was due to the
improvement of fibre–matrix compatibility due to the
alkali treatment [22]. According to El-Sheikeil, the ten-
sile, flexural and impact properties of kenaf/poly-
urethane composites showed a decreasing trend with
the increasing alkali concentration [24]. According to
Yousif et al., the 6% NaOH-treated kenaf/epoxy com-
posite showed an improvement in flexural strength
by 36% compared to the untreated fibre-based compo-
site. This was due to the improved interfacial adhesion
and pores on the NaOH-treated fibres which increased
the interlocking sites between the fibre and matrix [64].
Oftypha Angustifolia fibre-reinforced
composites
Dedeepya et al. investigated the tensile properties of
composites made from the oftypha Angustifolia fibres
and found that the tensile strength increases with alkali
treatment and with the increase of fibre content [65].
Palm fibre-reinforced composites
Findings of the Anike et al. implied that alkali treat-
ment of raffa palm fibre-based unsaturated polyester
composites leads to significant enhancement on the
tensile properties in comparison to the untreated com-
posites. Also, tensile properties showed an increasing
trend as a result of increase in fibre loading [66]. Simi-
lar results have been achieved by Obasi on alkali treat-
ment of the oil palm press fibre-reinforced epoxy
composites. They also reported that optimal mechan-
ical properties were achieved for 20% fibre content in
their work [67]. Abdal-hay et al. studied the effect of
alkali-treated date palm fibres on the tensile properties
of the epoxy-based composite and they found that
composites with 6% NaOH-treated date palm fibres
produced enhanced tensile strength and elastic mod-
ulus which was due to the improved adhesion between
the fibre and matrix due to the alkali treatment [46].
Pineapple leaf fibre (PALF)-reinforced
composites
According to Huda et al., 5% NaOH treatment of PALF
fibres for 2 h at room temperature leads to the
enhanced flexural and impact strength of the compo-
site made with PLA compared to the composite with
untreated PALF fibres [34]. In their study, Siregar
et al. reported that higher alkali concentration and
immersion time lead to detrimental effect on the tensile
properties of the pineapple leaf fibres (PALF)/HIPS
PLASTICS, RUBBER AND COMPOSITES 129
composite and increasing the immersion temperature
has no significant effect on fibre strength mean value
[68]. In another study, Siregar et al. found that HIPS-
based composite with 4% alkali-treated PALF fibres
for 1 h produced highest tensile, flexural and impact
properties [69]. Lopattananon et al. utilised 1, 3, 5
and 7% NaOH concentration on PALF fibres for 18 h
at room temperature, and they found that 5%
NaOH-treated fibre with natural rubber composite
gave the best tensile strength [70]. In another study,
Lopattananon et al. immersed PALF fibres with 5%
NaOH for 1 h at room temperature and studied the
flexural and impact properties of the epoxy composite
reinforced with treated and untreated PALF fibres.
They found that alkali-treated fibre-based composite
produced higher flexural and impact strength than
the untreated fibre-based composite [71].
Sisal fibres-reinforced composites
Based on the experimental results from Bisanda, it was
concluded that there was some slight increase in com-
pressive strength of the sisal/epoxy composites after
mercerisation. He also reported improved resin uptake
by the sisal fibres due to alkalisation, thus leading to
more rigid and denser composite with improved wett-
ability [16]. Mustafa and Dauda found that alkali treat-
ment of sisal fibres embedded in unsaturated polyester
resin leads to the enhanced tensile, flexural and impact
properties in comparison to the untreated sisal fibre-
based composite depending on the concentration levels
and immersion time of NaOH [48]. Similar results on
the improvement of tensile and flexural properties for
sisal/epoxy composite with the alkali-treated fibres
have been reported by Somashekar and Santhakumar,
while the impact strength decreased with the alkali
treatment [72]. Likewise, according to Sreekumar
et al., the impact strength of the sisal/polyester compo-
site with the alkali-treated fibres decreased, while the
tensile and flexural strength showed a rising trend
[73]. Kim and Netravali found that 2 M NaOH-treated
sisal fibre/soy protein concentrate resin composite
showed higher fracture stress and young’s modulus
than the composite with untreated fibres. According
to them, this improvement in the tensile properties
was due to the enhanced interfacial adhesion between
the fibre and the matrix [74].
Sugar palm fibre-reinforced composites
Sapuan et al. investigated the effect of alkali treatment
and immersion time on the sugar palm fibre-based
composites; they found that flexural strength and mod-
ulus were higher for 1 and 4 h but inferior for 8 h
immersion time [15]. Bachtiar et al. achieved 12.85%
increase in impact properties due to alkali treatment
(0.5 M NaOH for 8 h immersion time) of sugar palm
fibre-reinforced epoxy composite [75]. Chalid and
130 M. CHANDRASEKAR ET AL.
Imam subjected the ijuk fibre (part of the sugar palm
tree)/polylactic acid composite to alkali (0.25 M
NaOH solution for 30 min); they found that alkalis-
ation improves the wettability between the ijuk fibre
and PLA matrix, thereby leading to enhancement in
tensile strength and modulus, respectively [23].
Other natural fibre-based composites
Abral et al. subjected screw pine fibres to 2–15% NaOH
for 1 h and fabricated the treated fibres into composite
with the unsaturated polyester resin. 5 and 7% NaOH-
treated fibre-based composite produced better tensile
and flexural strength by considerable margin than the
composite with untreated fibres [76]. According to
Mylsamy et al., epoxy-based composite with 5%
NaOH-treated agave fibre for 30 min resulted in
improved tensile, flexural, compressive and impact
strength than the untreated fibre-based composite.
They also utilised 3, 7 and 10 mm fibre lengths in the
composite and found that 3 mm fibre length gave the
best mechanical properties which was due to the
enhanced fibre/matrix interfacial adhesion [77].
Water absorption behaviour
Since the natural fibres are hydrophilic in nature, they
absorb moisture from the atmosphere. Owing to this
moisture absorption by fibres, the hydrogen bond
breaks and hydroxyl groups form a new hydrogen
bond with water molecules. This causes swelling of
the natural fibres within the hydrophobic matrix lead-
ing to dimensional instability, matrix cracking and
poor mechanical properties [3].
Water absorption of the natural fibre and their com-
posites has been studied by various researchers. %
water absorption of alkali-treated and untreated
fibres/composite was calculated based on the formula
in Equation (4) [29]:
(Final weight − Initial weight)
%water absorption =
Initial weight
× 100
(4)
where final weight is the weight of the sample
measured after water treatment and initial weight is
the weight of the dry sample [12,19,43].
In general, alkali-treated natural fibres and their com-
posites showed good moisture resistance by absorbing
less moisture than the untreated fibres [6,12,14,43].
Results obtained by Lam and Jamaludin were in contrast
to the results obtained by most of the researchers, in
which water absorption ability of the alkali-treated fibres
was higher than that of the untreated fibres [29]. Reza
and Krishna studied the water absorption behaviour of
jute/epoxy composite and found that water uptake and
swelling increase with the addition of jute fibres to
epoxy matrix [78]. Similar characteristics on swelling
and increase of moisture uptake of the composite with
the increase in fibre loading have been reported by
Munoz and Garcia for the flax fibres [79].
Effect of immersion time
Zhu et al. studied the water absorption behaviour of
flax/tannin composites and found that tensile proper-
ties decreased as the composite was immersed in a
water bath for 3 days regardless of the different pre-
treatment methods [80]. Naveen et al. treated sisal/cot-
ton woven fibre mat to distilled water for 24 h and
found that tensile strength decreased up to 25% com-
pared to that of the dry specimen [81]. Haameem
et al. observed that tensile and flexural strength of the
Napier fibre/polyester composite tend to decrease
with the increased immersion time when the Napier
grass fibres were subjected to distilled water at 25°C
for 24, 48, 98, 196 and up to 552 h [82].
Effect of fibre loading
Umit Huner investigated the effect of various percen-
tages of fibre loading (1, 5 and 10%) on the water
absorption behaviour of flax fibre-reinforced epoxy
composite; he found that water absorption character-
istic increased with the increase in fibre loading %
[83]. Dhakal also reported similar characteristic of
increasing moisture uptake with the increase in fibre
volume fraction which is mainly due to high cellulose
content of the hemp fibres [84]. Munoz and Garcia
studied the influence of water absorption on the mech-
anical properties of flax fibre-reinforced composites
and found that water uptake increased with the fibre
loading (40 and 55 wt-%). They also reported an
increase in mechanical properties of the composite
after the water treatment [79]. Similar results on the
increased moisture uptake with the increase in fibre
loading of sisal/coconut fibres/epoxy composite have
been reported by Girisha and Gunti [85]. According
to Romanzini et al., as the volume fraction of the
ramie fibre in the hybrid ramie/glass fibre polyester
composites was increased, a light weight structure
was obtained but with the penalty of the higher water
absorption into the hybrid composite [86].
Effect of temperature
In his work, Umit Huner subjected flax fibre-
reinforced epoxy composite to the water at elevated
temperature (90°C) and found that moisture-induced
degradation of the composite was significant at elev-
ated temperature [83]. Similar results were obtained
by Dhakal et al. for the hemp fibre-reinforced unsatu-
rated polyester composites. They also reported that

water absorption behaviour tends to follow Fickian
behaviour at room temperature, while at elevated
temperature, the behaviour was non-Fickian [84].
Non-Fickian behaviour and moisture-induced degra-
dation were also reported at elevated temperature by
Girisha and Gunti on sisal/coir hybrid composite
[85]. Scida et al. studied the influence of temperature
on the tensile strength and young’s modulus of flax/
epoxy composite by subjecting the composite to hygro-
thermal aging (90% humidity at 20 and 40°C), accord-
ing to them both the properties decreased due to the
treatment [87].
Effect of sea water, distilled water and salt
water treatment
Parween et al. studied the fracture toughness of sugar
palm fibre-based epoxy composites subjected to sea
water, pond water and contaminated water for 30
days. They found that fracture toughness and energy
release rate were higher for the sea water-treated com-
posites compared to the pond water and contaminated
water [88]. Deugou et al. investigated the tensile prop-
erties of flax/PLA composites to long immersion of sea
water up to 2 years and observed a linear relationship
between water uptake and % loss in tensile properties
[89]. Njoku and Obikwelu subjected okam fibre/polye-
ster resin to sea water for 16 weeks and found that the
tensile properties decreased significantly due to the
weakening of interfacial bonding between okam fibre
and polyester resin matrix [90]. Similar results on the
drastic decrease of tensile properties and high level of
water absorption were reported by Norlin et al. on
kenaf fibres [91]. Leman et al. observed improvement
in surface properties as well as the adhesion between
fibre and matrix for the sugar palm-reinforced epoxy
composite subjected to freshwater and sea water,
thereby resulting in the increase of tensile properties.
According to them, 30 days treatment in freshwater
and sea water gave best results for the tensile strength
of sugar palm/epoxy composite [92]. Ishak et al.
studied the effect of sea water on impact and flexural
strength of the sugar palm fibre epoxy composite.
They observed that the sea water-treated composites
showed higher impact and flexural properties for 20
and 30% fibre loading than the composites with the
untreated fibres. This improvement was attributed to
the removal of cementing substances and better
adhesion characteristics [93]. Akil et al. subjected the
jute fibre/unsaturated polyester composite to distilled
water and sea water treatment at room temperature
for 3 weeks and found that both the flexural and com-
pressive properties decreased with the increase in
moisture uptake. According to them, this decrease in
the mechanical properties was due to the plasticisation
of the fibre–matrix interface and swelling of the jute
fibres [94]. Seki et al. investigated the performance of
PLASTICS, RUBBER AND COMPOSITES 131
jute/polyester composite to distilled water and
saltwater for 2736 h at 34°C. They found that inter-
laminar shear strength (ILSS) was reduced by more
than 53% due to the water aging [95].
Effect of hybridisation
Sanjay and Yogesha utilised E-glass fibres along with
jute and kenaf fibres epoxy composites in different
combinations and subjected the hybrid composite to
salt water, distilled and normal water. They found
that hybridisation decreases the water uptake regard-
less of the type of water used [96]. Sule et al. used
glass fibres and okra fibres at different ratios and
found that 50:50 hybrid composite exhibited high
moisture resistance as well as superior tensile proper-
ties. They also highlighted that 20 mm fibre length
composites had the highest tensile strength, modulus
and least water absorption characteristics, whereas
the 40 mm fibre length composites had the highest %
of elongation at break [97]. Khalil et al. studied the
swelling characteristics and water absorption behav-
iour of oil palm empty fruit bunches/jute fibre compo-
site; they found that both swelling and water
absorption characteristics decreased due to the hybrid-
isation and the fibre and matrix bonding improved sig-
nificantly [98]. Yahaya et al. subjected the jute/Kevlar
and kenaf/Kevlar epoxy-based composite to 4 months
of water aging; they found that tensile properties get
reduced, whereas impact properties were not affected
and moisture uptake of the hybrid composite increased
due to the increase of the fibre loading [99]. Similarly,
Sezgin and Berkalp studied the hybridisation effect of
jute with carbon and E-glass fabric; they utilised nine
different stacking sequences of the composite and
found that the high impact resistance and high tensile
strength can be obtained by changing the stacking
sequence of the synthetic fibre composite in the
arrangement [100]. Panthapulakkal and Sain per-
formed flexural and impact tests on hemp-/glass
fibre-based polypropylene-based composites and
found that hybridisation enhances the mechanical
properties in comparison to the hemp/PP composites
[101]. Mishra et al. subjected the sisal and PALF to
5% alkali treatment for 1 h and then fabricated a hybrid
composite with sisal/pineapple leaf-/glass fibre-based
polyester and found that water uptake was consider-
ably lower than that of the individual fibre-based
composite. Alkali-treated sisal fibres in the hybrid
composite lead to better tensile and impact strength
[102].
Based on their experiments from the sisal/bamboo
unsaturated polyester resin-based hybrid composite,
Venkatesh et al. concluded that water absorption was
least as well as the tensile, flexural and impact proper-
ties were considerably higher than those of the individ-
ual fibre-based composite. It is to be noted that the
132 M. CHANDRASEKAR ET AL.
mechanical properties of the natural fibre-based hybrid
composite were inferior compared to those of the natu-
ral/synthetic fibre-reinforced hybrid composite [103].
Similar attempt on natural fibre-based hybrid compo-
site, through kenaf/PALF high density poly ethylene
composite by IS Aji et al., showed that water uptake
and impact strength can be improved by the addition
of kenaf fibre to the hybrid composite, while pineapple
fibre helped in increasing the tensile properties [104].
Venkateshwaran et al. studied the water absorption
and mechanical properties of the banana/sisal/epoxy
composite. They found that mechanical properties of
the hybrid composite could be increased by the use
of up to 50% fibre loading along with the reduction
in water absorption [105].
Changes in failure modes before and after
alkali treatment
The morphological changes in the natural fibres and its
composites, such as increase in surface roughness and
fibrillation effect with the increase in NaOH concen-
tration, have been reported by several authors through
SEM micrographs. Only a few researchers studied the
changes in failure modes before and after the merceri-
sation process of the natural fibres and its composites.
Guduri et al. studied the fracture behaviour of
untreated and alkali-treated woven flax fibre-based
bio-copolyester composite. Poor interfacial bonding
was observed as a large gap between the fibre and
matrix for the untreated composite, whereas the
alkali-treated surface remained intact, showing
improved interfacial bonding [8]. SEM micrographs
of the coir fibre-reinforced epoxy composites before
alkali treatment showed more fibre pull-out, gaps at
fibre/matrix interface and brittle fracture of the epoxy
matrix. After alkali treatment, larger load was required
to pull-out the treated fibres from the matrix, showing
improved interfacial bonding [5]. According to Ray
et al., two different failure modes were observed
based on the NaOH immersion time. For immersion
time between 0 and 4 h, fibre pull-out was the predo-
minant failure mode, whereas for immersion time
between 6 and 8 h, failure mode was transverse fracture
with minimum fibre pull-out [28]. According to Yousif
et al., the NaOH-treated kenaf/epoxy composite
showed breakage only at the end of the fibres, whereas
untreated kenaf/epoxy composite showed de-bonding,
tearing, detachments and pull-out of fibres due to the
low interfacial adhesion of fibres with the matrix
[64]. According to Rout et al., the untreated coir
fibre/polyester composite showed fibre pull outs and
was left with many holes, indicating the weak fibre/
matrix interfacial adhesion due to the incompatibility
between the untreated fibre/polyester, whereas compo-
site with 5% NaOH-treated fibres showed matrix
cracks with the fibre break at the ends, implying strong
adhesion between the fibre and matrix after alkali treat-
ment [106].
Conclusion
Natural fibres and its composites have gained increased
attention among the researchers in recent times due to
their biodegradability, low density, good mechanical
properties, abundance, etc. Despite of these benefits,
hydrophilic nature i.e. low moisture resistance and
poor fibre/matrix adhesion characteristics of natural
fibres have been the serious setbacks to their appli-
cation in various industries. Modification of the
fibre surface, using physical and chemical methods to
overcome the above-mentioned setbacks, has been
attempted by various researchers. Most commonly
used chemical methods include alkalisation, acety-
lation, benzoylation and silane treatment. Among the
various chemical treatments, alkali treatment seems
to be the most economical and effective method for
improving the moisture resistance and wetting
characteristics.
. Alkalisation, also known as mercerisation, is said to
remove the cementing substances such as hemicellu-
lose, lignin, pectin, waxes and oils.
. Alkalisation of natural fibres leads to the fibrillation
effect, which is splitting of a single-fibre bundle into
smaller ones, increasing the effective area for mech-
anical interlocking between fibres and matrix, thus
leading to improved interfacial bonding.
. Various thermoset, thermoplastic resins and biode-
gradable/biopolymer resins have been used by
researchers with the untreated and alkali-treated
natural fibres for composite fabrication. The biopo-
lymer and thermoplastic resins offers the recycling
ability and eco-friendly option. However, the
major setback with them is their less mechanical
strength.
. Improvement, as well as deterioration of the mech-
anical, physical properties and thermal stability of
the alkali-treated natural fibres and its composite,
depends heavily on the NaOH concentration level,
fibre loading % and immersion time. So, there exists
an optimum NaOH concentration level, fibre load-
ing % and immersion time for each and every natu-
ral fibre and its composite beyond which those
properties face a detrimental effect as reported by
several researchers.
. For some mercerised composites, storage modulus
showed an increasing trend with the increase in
NaOH concentration, whereas tanδ peak curve
showed a decreasing trend with the increasing alkali
concentration, while it was vice versa for other natu-
ral fibres.
. The notable changes in the FTIR spectrum of alkali-
treated natural fibres were the disappearance of

characteristic peaks at certain range of wavenum-
bers, indicating the removal of cementing sub-
stances such as hemicellulose, lignin and pectin
regardless of the fibre employed.
. For XRD, peak intensity tends to increase with the
increase in NaOH concentration (below 10%) and
tends to decrease beyond 10% NaOH concentration.
Crystallinity index also tends to increase with the
increase in alkali concentration for the natural
fibres.
. In general, TGA results of weight loss % with
increasing temperature showed 2- and 3-phase
characteristics depending on the natural fibre, alkali
treatment conditions and immersion time. First
phase involves the evaporation of moisture and
second phase involves the removal of cementing
substances.
. DSC results from researchers indicate that only
slight changes in Tg, Tc and Tm were observed for
natural fibres treated with different concentration
levels of NaOH, whereas the degree of
crystallinity was found to be affected significantly,
indicating the transformation of cellulose I into cel-
lulose II.
. Improvement in mechanical properties of the var-
ious composites reinforced with the alkali-treated
fibres was due to the enhanced interfacial adhesion
between the fibre and matrix as reported by several
researchers with their results from the SEM images.
. Composites reinforced with alkali-treated natural
fibres showed matrix cracking, less fibre pull-out
and fibre breakage at the ends compared to the
untreated fibre-based composite which showed de-
bonding, tearing, large amount of fibre pull-out.
This was due to the weak interfacial adhesion
between the fibre and matrix for untreated fibre-
based composite which improved after the alkali
treatment of the fibres, leading to enhanced mech-
anical properties.
. Alkali -treated natural fibres and their composites
show good moisture resistance with the reduced
moisture uptake compared to the untreated fibres
and their composites.
. Moisture uptake of the natural fibres and their com-
posites increases with the increase in fibre loading.
. Moisture -induced degradation of the natural fibres
and its composites were significantly high at elev-
ated temperatures. The water diffusion behaviour
at room temperature tends to follow Fickian behav-
iour, whereas at the elevated temperature, the diffu-
sion behaviour was found to be non-Fickian.
. Moisture uptake of the natural fibre-based compo-
sites increases with the increase in fibre loading.
.
Hybridisation of the natural fibre-based composite
with the synthetic fibres like glass fabric significantly
reduces the water uptake. Similar results were
obtained by combining two different natural fibre-
PLASTICS, RUBBER AND COMPOSITES 133
based composite, but the mechanical properties
were inferior compared to those of the natural/syn-
thetic fibre-reinforced hybrid composite.
. Sea water treatment of the composites tends to
improve the interfacial adhesion between fibre and
matrix and leads to better mechanical properties
depending on the type of natural fibre subjected to
the sea water treatment.
. Long immersion of the natural fibres and its compo-
sites to water decreases their mechanical properties
like tensile strength and ILSS.
. Mechanical properties of the pure natural fibre-
based hybrid composite were found to be inferior
compared to that of the natural/synthetic fibre-
reinforced hybrid composite.
Disclosure statement
No potential conflict of interest was reported by the authors.
Funding
This work is supported by the research fund from Funda-
mental Research Grant Scheme, Malaysia (FRGS) [grant
number 5524741].
ORCID
M. Chandrasekar http://orcid.org/0000-0002-3637-7630
M. R. Ishak http://orcid.org/0000-0001-6923-2481
S. M. Sapuan http://orcid.org/0000-0003-0627-7951
Z. Leman http://orcid.org/0000-0002-3273-6675
M. Jawaid http://orcid.org/0000-0001-5348-5740
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