A Review On The Characterisation of Natural Fibres and Their Composites After Alkali Treatment and Water Absorption

Plastics, Rubber and Composites
Macromolecular Engineering
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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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Download by: [University of Colorado at Boulder Libraries] Date: 15 March 2017, At: 00:37
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-

backs in using these natural fibres as reinforcement
Synthetic fibre-based polymer composites have found
in the composite materials. These include hydrophilic
extensive applications in sports equipment, furniture,
nature of the fibres and poor fibre/matrix adhesion
aerospace, automotive industries, etc. due to their
characteristics. The moisture resistance and fibre/
high strength to weight ratio and excellent mechanical
matrix adhesion characteristics could be enhanced by
properties. Specifically, high performance application
the modification of the fibre surface and removal of
like aircraft structures heavily relies upon the synthetic
the impurities like wax and oil, hemicellulose and
fibre-made composites. Commonly used synthetic
lignin.
reinforcements include carbon, glass and aramid.
However, fossil fuel depletion and the other environ-
mental impacts associated with the production of the Modification of the natural fibre surface
synthetic fibres have made the researchers to look for
environment-friendly alternatives via natural fibres. Fibre surface of a natural fibre can be modified by
So, natural fibre is gaining increased attention among means of physical methods and chemical treatment.
the various researchers in recent years due to their Physical methods involve stretching, calendaring,
low density, good mechanical properties, biodegrad- cold plasma treatment, electric discharge method, etc.
ability, sustainability, good thermal and acoustic prop- [3]. Commonly used chemical methods for modifi-
erties, low cost and abundance. Natural fibres are cation of the fibre surface include alkalisation, acety-
classified into different categories as per the chart lation, benzoylation, bleaching (baking soda) and
below (Figure 1) [1] and Figure 2 shows the picture silane treatment [6]. The topic of interest of this
of various natural fibres [2]. study is only the effect of alkalisation on the mechan-
Significant amount of research works can be ical, chemical and thermal properties of various natural
found on the material characterisation of natural fibres and its composites along with their water absorp-
fibres like hemp, flax, sisal, kenaf, coir and jute tion behaviour.
and their composites based on the polymer matrices.
In general, the molecular structure of these natural Alkalisation
fibres is made up of cellulose, hemicellulose, lignin,
pectin, wax and oils and the percentage of such sub- Alkalisation, also known as the mercerisation process,
stances present in various natural fibres is given in involves the immersion of natural fibres in concen-
Table 1 [3–5]. trated sodium hydroxide (NaOH) solution. NaOH
CONTACT M. Chandrasekar [email protected] 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
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
Figure 3. Typical structure of (i) untreated and (ii) alkali-treated traditionally studied by several researchers using scan-
cellulose fibres [3]. ning electron microscope (SEM) images (Figure 5).
The alkali-treated grass fibres were found to undergo
reacts with the hydroxyl group of the natural fibres, fibrillation (Figure 6) which is splitting of a single-fibre
removes the hemicellulose, lignin, wax and oils that bundle into smaller ones with the increase in alkali con-
surround the external surface of the fibre leading to centration due to the removal of cementing materials
increase in the surface roughness (Refer to Figure 8), and other impurities. Fibrillation and removal of
aspect ratio and reduction in the fibre diameter and cementing substances along with impurities increase
results in a mercerised cellulose structure (as shown the effective surface area for mechanical interlocking
in Equation (1)) which improves interfacial bonding between the matrix and fibre, thus improving the inter-
between the hydrophilic fibres and hydrophobic poly- facial bonding [13,15,16]. Similarly, increment of fibril-
mer matrices [7]. lation effects with the increase in alkali concentration
has been reported by Karthikeyan et al. on the coir fibres
Fibre-OH + NaOH fibre-O-Na+ + H2 O (1) [9]. Aydin et al. reported that fibrillation effect on the
A typical untreated natural fibre appears to be sur- flax fibres became more pronounced as the alkali con-
rounded by cementing materials like lignin, hemicellu- centration was increased to 30% [17]. Fibrillation effect
lose and other impurities like wax and oils (Figure 3) was also reported by Liu et al. on the hemp fibres treated
[1], whereas the alkali-treated natural fibres were with 13 g L−1 NaOH for 3 h [18]. Another highlight of
found to be clean and rough due to the partial removal subjecting the natural fibres to alkali treatment is the
of lignin, hemicellulose and other impurities [8]. increase in the degree of surface roughness as compared
Alkali treatment of natural fibres results in the to that of the untreated fibres due to the removal of lig-
increase of exposure of cellulose content in the fibre nin and hemicellulose as reported by Punyamurthy et al.
surface (Table 3 where the percentage in cellulose con- on abaca fibres [6]. This characteristic of surface rough-
tent increases after the alkali treatment) [9–11], while ness, due to the removal of lignin and hemicellulose with
the hemicellulose and lignin get removed along with the increase in NaOH concentration and immersion
the impurities like wax and oils [12]. Alkali treatment time, was also reported by Sinha and Rout for the jute
also affects the crystalline properties by converting cel- fibres [19]. However, according to Liu et al., the increase
lulose I into cellulose II [13]. 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
Material characterisation techniques
and immersion time, beyond which delignification of
Material characterisation is an important aspect in the fibre takes place resulting in damaged fibre and
understanding the behaviour of natural fibres and leading to decrease in the mechanical properties
its composites to various loads and conditions, [3,4]. Symington et al. also reported that over-treat-
water absorption, chemical treatment methods, etc. ment of sisal, flax, kenaf and abaca fibres with alkali
(Figure 4). Mechanical characterisation involves the can lead to fibre cracking and show detrimental effect
testing of tensile, flexural, compressive, fatigue and on the mechanical properties of the natural fibres.
impact properties as per the respective ASTM stan- They also emphasised that 10 min of NaOH treatment
dards. Thermal stability of the natural fibres and its of the natural fibres was sufficient to achieve the opti-
composites was studied by the use of thermo mal properties [20]. SEM micrographs of sisal fibres
Figure 4. Process undergone by the raw fibre and its composites.

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 TGA

reveal that surface roughness of the natural fibres TGA is a thermal analysis technique in which a mass
increases with the increased NaOH concentration change (in %), thermal decomposition temperature
(Figure 7). and thermal stability of the natural fibre before and
Fiore et al. subjected the kenaf fibres to 6% NaOH after the NaOH treatment can be assessed [24].
for 48 and 144 h, and they indicated that 48 h treat- Findings from TGA results of Puglia et al. indicate
ment removed surface impurities and other cementing that thermal stability of the alkali-treated flax fibres
substances and lead to increase in the mechanical prop- (Phormium tenax) decreased slightly. Also, the alkali-
erties, whereas 144 h treatment produced a detrimental treated fibres have shown a reduced weight loss %
effect on the fibre surface (Figure 8) [22]. than the untreated flax fibres, indicating the removal
Alkali treatment causes formation of pores on the of cementing substances [25]. Similar results have
surface of the sugar palm fibre (Figure 9) and decreases been reported by Zhu et al. based on their experiments
their density and diameter due to the removal of on flax fibres [26]. TGA results from Guduri et al.
cementing substances and other impurities [23]. 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
Thermal properties alkali treatment. They also found that the thermal stab-
The thermal stability of the various alkali-treated natu- ility of the flax fibres relied upon the alkali concentration
ral fibres was analysed by researchers using TGA, DSC and immersion time [8]. Borchani et al. reported that
and DMA. temperature at maximum rate of decomposition
Figure 8. SEM images: (a) untreated kenaf fibres; (b) after 48 h in NaOH solution; and (c) after 144 h [22].
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 before and after the alkali treatment. It gives infor-
the Alfa fibres. According to them, the alkali-treated mation on thermal stability of the natural fibres
Alfa fibres showed low moisture than the untreated through the measurement of glass transition tempera-
fibres [27]. Liu et al. reported that the temperature at ture (Tg), cold crystallisation peak temperature (Tc)
the maximum rate of decomposition obtained through and melting temperature (Tm) as a function of temp-
weight % and derivative weight % for the Indian grass erature [24]. Also, % of crystallinity can be obtained
fibres increased with the increase in alkali concen- from the DSC thermogram [30].
tration, thereby resulting in the improvement of the The parameters like Tg, Tc and Tm that can be
thermal stability of the fibre after alkali treatment. obtained from a typical DSC thermogram are shown
This was due to the removal of hemicellulose and lignin in Figure 10. The DSC results of various natural fibres
content after NaOH treatment [13]. Three-phase and their composites reported by some of the research-
characteristics of weight (mass) loss % with the increas- ers are given in Table 2 (Figure 10).
ing temperature were obtained through the TGA results
by Zhu et al. on untreated/alkali-treated flax fibres [26]. DMA
Similar 3-phase characteristic of weight loss % with the DMA involves the measurement of change in stiffness
increasing temperature was also reported by Vasquez (loss modulus, storage modulus), damping (tanδ) and
et al. on the sweet sorghum fibres. First phase is credited glass transition temperature Tg of the composite with
to the removal of moisture and second phase was attrib- untreated and NaOH-treated natural fibres. The for-
uted to the removal of cementing substances [7]. How- mula for tanδ is given in Equation (2):
ever, Kaushik et al. reported 2-phase characteristics of
′′ loss modulus
weight loss % against the temperature range for sisal tan d = EE′ = (2)
storage modulus
fibres in which the first phase was attributed to the
breakdown of hemicellulose, glycosidic linkage and According to Fiore et al., alkali treatment of kenaf
loss of moisture, whereas the second phase of decompo- fibres led to a significant reduction and shifting of
sition was attributed to the cellulosic and lignin degra- the tanδ peaks of the composites reinforced with the
dation [21]. TGA results from Ray et al. on the jute alkali-treated fibres compared to the composite made
fibre-reinforced unsaturated polyester composite from the untreated fibres. They indicated that stacking
showed a decrease in thermal stability after alkali treat- sequence of the composite did not affect the loss
ment [28]. Experiments by Fook and Yatim on the alkali moduli and tanδ peaks [22]. Karsli and Aytac per-
treatment of kenaf fibres with pH ranging from 8 to 14 formed DMA on flax fibre/poly-lactic acid (PLA)/PC
showed that weight loss % increased (density decreases) composite with untreated and alkali-treated fibres,
as a result of increase in pH, this was due to the etching and they found that storage modulus increased with
away of lignin, hemicellulose, pectin, etc from the kenaf the increase in alkali concentration, whereas peak of
fibre due to the alkali treatment [29]. tanδ decreased with the increasing alkali concentration
[30]. Results obtained by Guduri et al., on the storage
DSC modulus and tanδ for the flax/bio-copolyester compo-
DSC thermogram was found to be highly helpful in site, were in contrast to those of Karsli and Aytac, in
studying the thermal stability of the natural fibres which the storage modulus decreased with the
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 cellulose, hemicellulose, lignin, pectin and water mol-
shifted with the increasing NaOH concentration [8]. ecules. The peak characteristics of the untreated flax
fibres, belonging to cellulose, pectin, lignin, etc., are
given in Table 4.
Chemical properties
In general, on comparing the absorbance character-
The chemical composition of the untreated and alkali- istics of untreated fibres with alkali-treated fibres over
treated natural fibres have been studied by various the wavenumbers, it can be observed that some of the
researchers using FTIR and XRD spectroscopy. characteristic peaks, which can be seen in the case of
The chemical composition of a natural fibre is made untreated fibres, disappear for the alkali-treated fibres.
of cellulose, hemicellulose, lignin, pectin, moisture, wax This was attributed to the removal of cementing sub-
and oils (Table 1). Owing to the alkali treatment, the stances like hemicellulose, lignin, pectin and moisture.
percentage of these substances gets decreased or The notable changes in the FTIR spectrum of alkali-
removed as could be seen in Table 3. treated flax fibres, as observed by various researchers,
were the disappearance of characteristic peaks at cer-
FTIR spectroscopy tain range of wavenumbers 1735 and 1525 cm−1 and
The analysis of alkali-treated and untreated natural indication of the removal of hemicellulose and lignin
fibres using FTIR involves the measurement of [8,14,25,26]. In the case of the untreated flax fibres,
absorbance against the wavenumber range of 400– peak for hydroxyl group (−OH group) was higher.
6000 cm−1. In the plot, each characteristic peak corre- This particular characteristic peak decreased after the
sponds to the composition of natural fibres like 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
as well as hemicellulose and lignin which absorbs water was attributed to the conversion of crystalline I to crys-
molecules [14]. FTIR results by El-shekeil on kenaf talline II and increase in amorphous portion of the cel-
fibre-based polyurethane composites indicated that lulose [17]. However, according to the XRD results of
the characteristic peaks disappear at certain wavenum- Borchani et al. for Alfa fibres, there was no transform-
bers (1740 and 1250 cm−1), indicating the removal of ation of cellulose I into cellulose II [27].
cementing substances like hemicellulose [24]. FTIR
spectroscopic results on the untreated and alkali-trea-
Mechanical properties of the alkali-treated
ted Alfa fibres showed that characteristic peak intensi-
natural fibres
ties (1731 cm−1 and broad absorption band at
3359.8 cm−1) diminish with the increasing alkali con- Mechanical properties of some natural fibres along
centration. This was due to the removal of cementing with the synthetic fibres are given in Table 6 along
substances [37]. with the properties of synthetic fibres for comparison.
Hongling et al. studied the effect of various alkali
concentrations and immersion time of hemp fibres
XRD analysis through tensile and bending tests. According to their
XRD analysis involves studying the changes in crystal- results, the increase in alkali treatments increases the
linity index (CI %) of the untreated and alkali-treated tensile strength of the hemp fibres, whereas the bend-
fibres by measuring the minimum peak intensity or ing modulus and flexural rigidity decreased as the
height of the minimum intensity between major NaOH concentration was increased [18]. Alkali treat-
peaks (corresponding to amorphous or non-crystalline ment of coir fibres (3% for 5 h) tends to decrease the
material) and maximum peak intensity or highest dif- tensile strength, tensile modulus and elongation %.
fraction peak (corresponding to crystalline material). According to them, this was due to the etching away
The formula for calculating crystallinity index is of binding component between the micro-fibres [41].
given by Segal method as in Equation (3): Meheddene et al. showed that prolonged treatment
(I002 − Iam ) (1, 2, 4 and 10% for 2, 4 and 24 h) of the fan palm fibres
CI(%)= (3) with higher NaOH concentration could cause severe
I002
deterioration in the tensile strength of the treated
where I002 is the maximum intensity diffraction peak fibres, whereas the tensile modulus and % of elongation
measured at a diffraction angle of 2θ = 22.8° and Iam did not get affected by the alkali treatment process [42].
is the minimum intensity diffraction peak measured Kanchireddy and Muzenda coated the grass fibres with
at a diffraction angle of 2θ = 18° [27,37,38]. Crystalli- polycarbonate and subjected them to alkali treatment.
nity index of various natural fibres reported by the They found that polycarbonate-/alkali-treated grass
different authors is given in Table 5. fibre showed superior tensile strength than the
The XRD results of Benyahia et al. on Alfa fibres uncoated and raw fibre [43]. According to Wong
showed that both the crystallinity index (CI%) and et al., the increase in alkali concentration leads to
peak or maximum intensity increased due to the reduction in strain at failure and ductility of the bam-
NaOH treatment [37]. Hosur et al. studied the effect boo fibres [44]. Hashim et al. subjected kenaf fibres to
of alkali treatment on the flax fibre structure using 2% NaOH at 2 and 100°C for 30 and 480 min. From
XRD. According to them, the peak intensity tends to their results, it was concluded that the immersion
increase with the increase in NaOH concentration time had a major impact on the tensile mean strength
(2.5, 5 and 7%) [14]. However, the XRD results value of the fibre, whereas the temperature had a small
obtained by Aydin et al. were in contrast to the results impact [45]. Abdal-hay et al. found that ultimate tensile
obtained by Hosur et al. where the peak intensity strength and % elongation of the single fibre increased
decreases with the increasing alkali concentration (10, significantly due to the alkali treatment (6% for 3 h)
20 and 30%) for the flax fibres. The decreasing trend [46]. According to Haameem et al., 10% NaOH-treated
Napier grass fibres showed better single-fibre tensile
Table 5. Crystallinity index of some of the natural fibres before properties compared to the untreated fibres [47].
and after alkali treatment obtained through XRD – Segal
method. Table 6. Mechanical properties of some of the natural fibres
Crystallinity index (CI %)a and synthetic fibres [3,40].
Fibre Untreated Alkali treated Alkali concentration (%) Young’s
Density Tensile modulus Elongation at
Alfa [27] 59.5 66.7 1
Fibres (g cm−3) strength (MPa) (GPa) break (%)
Flax [14] 72.6 78.9 2.5
Sisal [21] 71.7 74.3 5 Jute 1.3–1.45 393–773 13–26.5 1.16–1.5
Jute [39] 71.39 84.46 6 Flax 1.50 345–2000 27.5–85 2.7–3.2
Hemp [39] 87.87 89.77 30 Hemp 1.14 690 30–60 1.6
Kapok [39] 45.75 58.42 8 E-glass 2.5 2000–3500 70 2.5
a
The numerical data reported here are identical to the data published by Carbon 1.7–1.9 4000 230–240 1.4–1.8
the cited researchers. Aramid 1.4 2800–3600 80–190 2–4
Mechanical properties of the composites (immersion time 24 h)/polyester composite led to sig-
reinforced with alkali-treated fibres nificant improvement in the flexural strength and
modulus [51].
Mechanical properties of the natural fibres and their
composites depend on the type of plant fibre used,
type of matrix involved and interfacial adhesion Bagasse fibre-reinforced composites
between the fibre and matrix [30]. The changes in
mechanical properties due to alkalisation have been Acharya et al. treated bagasse fibres with 5% NaOH for
studied by various researchers by subjecting the 2, 4 and 6 h. Best flexural properties of bagasse/epoxy
untreated and alkali-treated natural fibre and their composite were achieved when 5% NaOH-treated
composites to tensile, compressive, flexural and impact fibres with the immersion time of 4 h were used [11].
loads. Mechanical characterisation is done according to According to Vilay et al., alkali treatment and the
the ASTM standards depending on whether the increase in fibre loading of the bagasse fibre in unsatu-
material tested is fibre or composite and the type of rated polyester composites resulted in higher tensile
matrices involved. and flexural properties in comparison to the composite
This section describes the impact of alkali treatment with the untreated fibres [52].
on the mechanical properties of various natural fibre-
based composites. Table 7 shows the parameters used
Bamboo fibre-reinforced composites
by various researchers to study the effect of alkali treat-
ment on the natural fibres and its 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-
Abaca fibre-reinforced composites cated that density of the composites decreased with
Shibata et al. treated abaca fibres with 2% NaOH for the increase of NaOH concentration, leading to higher
2 h and studied its flexural properties through treated porosity, resulting effect due to the removal of cement-
and untreated fibre/biodegradable polyester composite, ing composites. Based on their results, inter facial shear
and they found that considerable increment in flexural strength (IFSS) was found to increase, while the per-
strength was obtained for the composite with treated centage improvement falls with the increasing alkali
fibres in comparison to the untreated fibre-based com- concentration [44]. According to Lu et al., composite
posite [49]. with 2% NaOH-treated bamboo fibre/epoxy resin
showed improvement in tensile strength and %
elongation at break by 71 and 53%, respectively [53].
Alfa fibre-reinforced composites
Both tensile and flexural strength/modulus of the Alfa
Banana fibre-reinforced composites
fibre-based polyester composites were found to be
improved by various concentrations of alkali treatment Venkateshwaran et al. treated banana fibres with 0.5–
(1, 3, 5 and 7% for 24 h) by Benyahia et al. [37]. 20% NaOH concentration for 30 min and studied the
According to Arrakhiz et al., 1.6 mol L−1 NaOH treat- tensile, flexural and impact properties of the epoxy-
ment of Alfa fibres for 48 h resulted in better tensile based composite reinforced with treated and untreated
strength and young’s modulus than the untreated fibres. Among the various concentration levels, 1%
fibre-based composite [50]. Based on their studies, NaOH treatment produced the best tensile, flexural
Rokbi et al. concluded that 5% NaOH-treated alfa and impact properties which was attributed to the
Table 7. Alkali treatment conditions of some natural fibres as reported by the researchers.
Soaking
Fibres Matrix NaOH Concentration time Soaking temperature Drying
Abaca [6] – 15 times the weight of 72 h 30°C Dried at room temperature for 48 h
fibres
Alfa [37] Polyester 1, 3, 5 and 7% 24 h 25°C 80°C for 48 h
Bamboo [44] Polyester 1, 3 ad 5% 24 h Room temperature 24 h under sun
Coir [5] Epoxy 5% 1/2 h 20°C lab temperature 24 h in open air and 50°C in the oven for 8 h
Flax [14] Polyester and Polyester 2.5, 5 and 7% 1h Room temperature 80°C for 24 h
biopolymer blend resin
Jute [28] Vinyl ester 5% 2, 4, 6 and 30°C Room temperature for 48 h followed by oven
8 drying for 100°C for 6 h
Kenaf [45] – 2 and 10% ½ and 8 h Room temperature 100–105°C for 1 h
and 100°C
Sisal [48] Unsaturated polyester 2, 6 and 10% 2, 3 and 65°C under constant Open air for 4–5 days
5h stirring
Sugar Palm Epoxy 2.5 and 5% 1, 4 and Room temperature Dried at room temperature for 4 days
[15] 8h
improved interfacial adhesion. They also observed that treatment for 45 seconds was sufficient to achieve
high concentration level of NaOH leads to deterio- 30% increment in transverse tensile strength and
ration of the mechanical properties which was due to treatment of flax fibres at high concentration level
the fibre damage caused by the alkali treatment [54]. beyond 10% could lead to the deterioration in the
longitudinal and transverse tensile strength [58].
Curua fibre-reinforced composites
Gomes et al. dipped curua fibres into 5, 10 and 15% Grass fibre-reinforced composites
NaOH concentration for 1 and 2 h. They found that Impact strength of the Napier grass fibre-based epoxy
the tensile strength and fracture strain of alkali-treated composites showed an increasing trend with the increase
fibre/biodegradable corn starch composite was higher in fibre weight % and alkali concentration. The highest
than the composite with the untreated curua fibre [55]. impact strength was obtained for composites with 2%
NaOH-treated fibres and 20% fibre loading [10].
Coir fibre-reinforced composite
According to Yan et al., 5% NaOH concentration for Hemp fibre-reinforced composites
30 min resulted in higher tensile, flexural strength and
modulus of the coir fibre-based composites [5]. Exper- Based on the results of Islam et al., it can be concluded
imental investigation on alkali treated (2, 4, 6 and 8% that the alkali treatment of hemp fibre-reinforced
for 10 days) coir fibre-based epoxy composite by PLA composites with 30% fibre loading leads to sig-
Karthikeyan revealed that impact strength was better nificant improvement in the interfacial bonding
for the composites with alkali-treated fibres than the between the fibre and matrix which, in turn, leads to
untreated fibre-based composites [9]. According to the higher mechanical properties [59]. Similar
Gu Huang, during NaOH treatment of coir fibres at improvements in the mechanical properties of
2, 4, 6 and 8% for 4 weeks, there was no significant hemp/polylactide composites due to 5% NaOH treat-
difference in the tensile strength of treated fibre/PP ment for 30 min and with the increase of fibre loading
composite even after immersing for 4 weeks. Their were reported by Moyeenuddin et al. They also high-
hypothesis for negligible change in tensile strength lighted that 30% weight of fibre loading with the
for various concentration levels of NaOH was due to alkali-treated fibres in the composite gave the best
the improved fibre/matrix adhesion [56]. According tensile, flexural and impact properties [60]. Suardana
to Arrakhiz et al., tensile properties of 1.6 mol L−1 et al. performed alkali treatment at various concen-
NaOH-treated coir fibre/HIPS composite with the tration levels (2, 4 and 6% at 70°C for 1 h) on
immersion time of 48 h showed only a 10% improve- hemp/PP composites and found that alkali treatment
ment compared to the untreated fibre-based compo- improved the tensile and flexural strength, indicating
site [57]. the enhanced wettability between fibre and matrix.
Among the various concentration levels utilised, 4%
NaOH treatment of fibres leads to the best mechanical
Flax fibre-reinforced composites properties of the composite [61].
Merlin et al. utilised higher concentration of NaOH
(10, 20 and 30%) on the short fibre/poly-lacic acid
Jute fibre-reinforced composites
composites and found that tensile modulus decreases
gradually with increasing NaOH concentration. The The mechanical properties of jute fibre-reinforced
decrease in tensile modulus was attributed to the vinyl ester composite showed a declining trend with
heavy damage on the fibres caused by the increased the increase in alkali concentration and immersion
alkali concentration [17]. Karsli and Aytac found time [35]. Owen subjected jute fabric to 20% NaOH
that 2% alkali-treated flax fibres with the PLA/PC for 25 min at room temperature and found that the
composites showed the highest tensile strength and epoxy composites reinforced with alkali-treated jute
modulus compared to the composites with 5% and fabric produced better tensile, flexural and impact
10% NaOH concentration [30]. Van de weyenberg properties than the composite with untreated fibres
et al. performed NaOH treatment of various concen- [62]. Leela et al. reported an increase in tensile strength
tration levels on the unidirectional flax fibres and of jute fibre-reinforced polypropylene composite for
they found that when the concentration of NaOH 20% fibre loading and up to 10% NaOH concentration.
was raised beyond 23%, both the longitudinal and Also, tensile modulus increased with the increase in
transverse tensile strength of the treated fibre/epoxy fibre loading and NaOH concentration, whereas %
composite declined significantly, indicating the elongation at break for the composites showed a
damage on the treated fibres at such high concen- steep declining trend with the increasing fibre loading
trations. According to them, even a 4% NaOH and NaOH concentration [63].
Kenaf fibre-reinforced composites composite and increasing the immersion temperature

has no significant effect on fibre strength mean value
Fiore et al. performed experiments on kenaf/epoxy
[68]. In another study, Siregar et al. found that HIPS-
composites with the fibres treated with 6% alkaline
based composite with 4% alkali-treated PALF fibres
for long immersion time 48 and 144 h. They found
for 1 h produced highest tensile, flexural and impact
that the tensile strength improved for composite with
properties [69]. Lopattananon et al. utilised 1, 3, 5
48 h NaOH-treated kenaf fibres which was due to the
and 7% NaOH concentration on PALF fibres for 18 h
improvement of fibre–matrix compatibility due to the
at room temperature, and they found that 5%
alkali treatment [22]. According to El-Sheikeil, the ten-
NaOH-treated fibre with natural rubber composite
sile, flexural and impact properties of kenaf/poly-
gave the best tensile strength [70]. In another study,
urethane composites showed a decreasing trend with
Lopattananon et al. immersed PALF fibres with 5%
the increasing alkali concentration [24]. According to
NaOH for 1 h at room temperature and studied the
Yousif et al., the 6% NaOH-treated kenaf/epoxy com-
flexural and impact properties of the epoxy composite
posite showed an improvement in flexural strength
reinforced with treated and untreated PALF fibres.
by 36% compared to the untreated fibre-based compo-
They found that alkali-treated fibre-based composite
site. This was due to the improved interfacial adhesion
produced higher flexural and impact strength than
and pores on the NaOH-treated fibres which increased
the untreated fibre-based composite [71].
the interlocking sites between the fibre and matrix [64].
Sisal fibres-reinforced composites
Oftypha Angustifolia fibre-reinforced Based on the experimental results from Bisanda, it was
composites concluded that there was some slight increase in com-
Dedeepya et al. investigated the tensile properties of pressive strength of the sisal/epoxy composites after
composites made from the oftypha Angustifolia fibres mercerisation. He also reported improved resin uptake
and found that the tensile strength increases with alkali by the sisal fibres due to alkalisation, thus leading to
treatment and with the increase of fibre content [65]. more rigid and denser composite with improved wett-
ability [16]. Mustafa and Dauda found that alkali treat-
Palm fibre-reinforced composites ment of sisal fibres embedded in unsaturated polyester
resin leads to the enhanced tensile, flexural and impact
Findings of the Anike et al. implied that alkali treat- properties in comparison to the untreated sisal fibre-
ment of raffa palm fibre-based unsaturated polyester based composite depending on the concentration levels
composites leads to significant enhancement on the and immersion time of NaOH [48]. Similar results on
tensile properties in comparison to the untreated com- the improvement of tensile and flexural properties for
posites. Also, tensile properties showed an increasing sisal/epoxy composite with the alkali-treated fibres
trend as a result of increase in fibre loading [66]. Simi- have been reported by Somashekar and Santhakumar,
lar results have been achieved by Obasi on alkali treat- while the impact strength decreased with the alkali
ment of the oil palm press fibre-reinforced epoxy treatment [72]. Likewise, according to Sreekumar
composites. They also reported that optimal mechan- et al., the impact strength of the sisal/polyester compo-
ical properties were achieved for 20% fibre content in site with the alkali-treated fibres decreased, while the
their work [67]. Abdal-hay et al. studied the effect of tensile and flexural strength showed a rising trend
alkali-treated date palm fibres on the tensile properties [73]. Kim and Netravali found that 2 M NaOH-treated
of the epoxy-based composite and they found that sisal fibre/soy protein concentrate resin composite
composites with 6% NaOH-treated date palm fibres showed higher fracture stress and young’s modulus
produced enhanced tensile strength and elastic mod- than the composite with untreated fibres. According
ulus which was due to the improved adhesion between to them, this improvement in the tensile properties
the fibre and matrix due to the alkali treatment [46]. was due to the enhanced interfacial adhesion between
the fibre and the matrix [74].
Pineapple leaf fibre (PALF)-reinforced
composites Sugar palm fibre-reinforced composites
According to Huda et al., 5% NaOH treatment of PALF Sapuan et al. investigated the effect of alkali treatment
fibres for 2 h at room temperature leads to the and immersion time on the sugar palm fibre-based
enhanced flexural and impact strength of the compo- composites; they found that flexural strength and mod-
site made with PLA compared to the composite with ulus were higher for 1 and 4 h but inferior for 8 h
untreated PALF fibres [34]. In their study, Siregar immersion time [15]. Bachtiar et al. achieved 12.85%
et al. reported that higher alkali concentration and increase in impact properties due to alkali treatment
immersion time lead to detrimental effect on the tensile (0.5 M NaOH for 8 h immersion time) of sugar palm
properties of the pineapple leaf fibres (PALF)/HIPS fibre-reinforced epoxy composite [75]. Chalid and
Imam subjected the ijuk fibre (part of the sugar palm swelling increase with the addition of jute fibres to
tree)/polylactic acid composite to alkali (0.25 M epoxy matrix [78]. Similar characteristics on swelling
NaOH solution for 30 min); they found that alkalis- and increase of moisture uptake of the composite with
ation improves the wettability between the ijuk fibre the increase in fibre loading have been reported by
and PLA matrix, thereby leading to enhancement in Munoz and Garcia for the flax fibres [79].
tensile strength and modulus, respectively [23].
Effect of immersion time
Other natural fibre-based composites Zhu et al. studied the water absorption behaviour of
Abral et al. subjected screw pine fibres to 2–15% NaOH flax/tannin composites and found that tensile proper-
for 1 h and fabricated the treated fibres into composite ties decreased as the composite was immersed in a
with the unsaturated polyester resin. 5 and 7% NaOH- water bath for 3 days regardless of the different pre-
treated fibre-based composite produced better tensile treatment methods [80]. Naveen et al. treated sisal/cot-
and flexural strength by considerable margin than the ton woven fibre mat to distilled water for 24 h and
composite with untreated fibres [76]. According to found that tensile strength decreased up to 25% com-
Mylsamy et al., epoxy-based composite with 5% pared to that of the dry specimen [81]. Haameem
NaOH-treated agave fibre for 30 min resulted in et al. observed that tensile and flexural strength of the
improved tensile, flexural, compressive and impact Napier fibre/polyester composite tend to decrease
strength than the untreated fibre-based composite. with the increased immersion time when the Napier
They also utilised 3, 7 and 10 mm fibre lengths in the grass fibres were subjected to distilled water at 25°C
composite and found that 3 mm fibre length gave the for 24, 48, 98, 196 and up to 552 h [82].
best mechanical properties which was due to the
enhanced fibre/matrix interfacial adhesion [77]. Effect of fibre loading
Umit Huner investigated the effect of various percen-
Water absorption behaviour tages of fibre loading (1, 5 and 10%) on the water
absorption behaviour of flax fibre-reinforced epoxy
Since the natural fibres are hydrophilic in nature, they
composite; he found that water absorption character-
absorb moisture from the atmosphere. Owing to this
istic increased with the increase in fibre loading %
moisture absorption by fibres, the hydrogen bond
[83]. Dhakal also reported similar characteristic of
breaks and hydroxyl groups form a new hydrogen
increasing moisture uptake with the increase in fibre
bond with water molecules. This causes swelling of
volume fraction which is mainly due to high cellulose
the natural fibres within the hydrophobic matrix lead-
content of the hemp fibres [84]. Munoz and Garcia
ing to dimensional instability, matrix cracking and
studied the influence of water absorption on the mech-
poor mechanical properties [3].
anical properties of flax fibre-reinforced composites
Water absorption of the natural fibre and their com-
and found that water uptake increased with the fibre
posites has been studied by various researchers. %
loading (40 and 55 wt-%). They also reported an
water absorption of alkali-treated and untreated
increase in mechanical properties of the composite
fibres/composite was calculated based on the formula
after the water treatment [79]. Similar results on the
in Equation (4) [29]:
increased moisture uptake with the increase in fibre
(Final weight − Initial weight) loading of sisal/coconut fibres/epoxy composite have
%water absorption =
Initial weight been reported by Girisha and Gunti [85]. According
× 100 to Romanzini et al., as the volume fraction of the
ramie fibre in the hybrid ramie/glass fibre polyester
(4)
composites was increased, a light weight structure
where final weight is the weight of the sample was obtained but with the penalty of the higher water
measured after water treatment and initial weight is absorption into the hybrid composite [86].
the weight of the dry sample [12,19,43].
In general, alkali-treated natural fibres and their com-
Effect of temperature
posites showed good moisture resistance by absorbing
less moisture than the untreated fibres [6,12,14,43]. In his work, Umit Huner subjected flax fibre-
Results obtained by Lam and Jamaludin were in contrast reinforced epoxy composite to the water at elevated
to the results obtained by most of the researchers, in temperature (90°C) and found that moisture-induced
which water absorption ability of the alkali-treated fibres degradation of the composite was significant at elev-
was higher than that of the untreated fibres [29]. Reza ated temperature [83]. Similar results were obtained
and Krishna studied the water absorption behaviour of by Dhakal et al. for the hemp fibre-reinforced unsatu-
jute/epoxy composite and found that water uptake and rated polyester composites. They also reported that
water absorption behaviour tends to follow Fickian jute/polyester composite to distilled water and
behaviour at room temperature, while at elevated saltwater for 2736 h at 34°C. They found that inter-
temperature, the behaviour was non-Fickian [84]. laminar shear strength (ILSS) was reduced by more
Non-Fickian behaviour and moisture-induced degra- than 53% due to the water aging [95].
dation were also reported at elevated temperature by
Girisha and Gunti on sisal/coir hybrid composite
Effect of hybridisation
[85]. Scida et al. studied the influence of temperature
on the tensile strength and young’s modulus of flax/ Sanjay and Yogesha utilised E-glass fibres along with
epoxy composite by subjecting the composite to hygro- jute and kenaf fibres epoxy composites in different
thermal aging (90% humidity at 20 and 40°C), accord- combinations and subjected the hybrid composite to
ing to them both the properties decreased due to the salt water, distilled and normal water. They found
treatment [87]. 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
Effect of sea water, distilled water and salt
found that 50:50 hybrid composite exhibited high
water treatment
moisture resistance as well as superior tensile proper-
Parween et al. studied the fracture toughness of sugar ties. They also highlighted that 20 mm fibre length
palm fibre-based epoxy composites subjected to sea composites had the highest tensile strength, modulus
water, pond water and contaminated water for 30 and least water absorption characteristics, whereas
days. They found that fracture toughness and energy the 40 mm fibre length composites had the highest %
release rate were higher for the sea water-treated com- of elongation at break [97]. Khalil et al. studied the
posites compared to the pond water and contaminated swelling characteristics and water absorption behav-
water [88]. Deugou et al. investigated the tensile prop- iour of oil palm empty fruit bunches/jute fibre compo-
erties of flax/PLA composites to long immersion of sea site; they found that both swelling and water
water up to 2 years and observed a linear relationship absorption characteristics decreased due to the hybrid-
between water uptake and % loss in tensile properties isation and the fibre and matrix bonding improved sig-
[89]. Njoku and Obikwelu subjected okam fibre/polye- nificantly [98]. Yahaya et al. subjected the jute/Kevlar
ster resin to sea water for 16 weeks and found that the and kenaf/Kevlar epoxy-based composite to 4 months
tensile properties decreased significantly due to the of water aging; they found that tensile properties get
weakening of interfacial bonding between okam fibre reduced, whereas impact properties were not affected
and polyester resin matrix [90]. Similar results on the and moisture uptake of the hybrid composite increased
drastic decrease of tensile properties and high level of due to the increase of the fibre loading [99]. Similarly,
water absorption were reported by Norlin et al. on Sezgin and Berkalp studied the hybridisation effect of
kenaf fibres [91]. Leman et al. observed improvement jute with carbon and E-glass fabric; they utilised nine
in surface properties as well as the adhesion between different stacking sequences of the composite and
fibre and matrix for the sugar palm-reinforced epoxy found that the high impact resistance and high tensile
composite subjected to freshwater and sea water, strength can be obtained by changing the stacking
thereby resulting in the increase of tensile properties. sequence of the synthetic fibre composite in the
According to them, 30 days treatment in freshwater arrangement [100]. Panthapulakkal and Sain per-
and sea water gave best results for the tensile strength formed flexural and impact tests on hemp-/glass
of sugar palm/epoxy composite [92]. Ishak et al. fibre-based polypropylene-based composites and
studied the effect of sea water on impact and flexural found that hybridisation enhances the mechanical
strength of the sugar palm fibre epoxy composite. properties in comparison to the hemp/PP composites
They observed that the sea water-treated composites [101]. Mishra et al. subjected the sisal and PALF to
showed higher impact and flexural properties for 20 5% alkali treatment for 1 h and then fabricated a hybrid
and 30% fibre loading than the composites with the composite with sisal/pineapple leaf-/glass fibre-based
untreated fibres. This improvement was attributed to polyester and found that water uptake was consider-
the removal of cementing substances and better ably lower than that of the individual fibre-based
adhesion characteristics [93]. Akil et al. subjected the composite. Alkali-treated sisal fibres in the hybrid
jute fibre/unsaturated polyester composite to distilled composite lead to better tensile and impact strength
water and sea water treatment at room temperature [102].
for 3 weeks and found that both the flexural and com- Based on their experiments from the sisal/bamboo
pressive properties decreased with the increase in unsaturated polyester resin-based hybrid composite,
moisture uptake. According to them, this decrease in Venkatesh et al. concluded that water absorption was
the mechanical properties was due to the plasticisation least as well as the tensile, flexural and impact proper-
of the fibre–matrix interface and swelling of the jute ties were considerably higher than those of the individ-
fibres [94]. Seki et al. investigated the performance of ual fibre-based composite. It is to be noted that the
mechanical properties of the natural fibre-based hybrid adhesion between the fibre and matrix after alkali treat-
composite were inferior compared to those of the natu- ment [106].
ral/synthetic fibre-reinforced hybrid composite [103].
Similar attempt on natural fibre-based hybrid compo-
Conclusion
site, through kenaf/PALF high density poly ethylene
composite by IS Aji et al., showed that water uptake Natural fibres and its composites have gained increased
and impact strength can be improved by the addition attention among the researchers in recent times due to
of kenaf fibre to the hybrid composite, while pineapple their biodegradability, low density, good mechanical
fibre helped in increasing the tensile properties [104]. properties, abundance, etc. Despite of these benefits,
Venkateshwaran et al. studied the water absorption hydrophilic nature i.e. low moisture resistance and
and mechanical properties of the banana/sisal/epoxy poor fibre/matrix adhesion characteristics of natural
composite. They found that mechanical properties of fibres have been the serious setbacks to their appli-
the hybrid composite could be increased by the use cation in various industries. Modification of the
of up to 50% fibre loading along with the reduction fibre surface, using physical and chemical methods to
in water absorption [105]. overcome the above-mentioned setbacks, has been
attempted by various researchers. Most commonly
used chemical methods include alkalisation, acety-
Changes in failure modes before and after
lation, benzoylation and silane treatment. Among the
alkali treatment
various chemical treatments, alkali treatment seems
The morphological changes in the natural fibres and its to be the most economical and effective method for
composites, such as increase in surface roughness and improving the moisture resistance and wetting
fibrillation effect with the increase in NaOH concen- characteristics.
tration, have been reported by several authors through
SEM micrographs. Only a few researchers studied the . Alkalisation, also known as mercerisation, is said to
changes in failure modes before and after the merceri- remove the cementing substances such as hemicellu-
sation process of the natural fibres and its composites. lose, lignin, pectin, waxes and oils.
Guduri et al. studied the fracture behaviour of . Alkalisation of natural fibres leads to the fibrillation
untreated and alkali-treated woven flax fibre-based effect, which is splitting of a single-fibre bundle into
bio-copolyester composite. Poor interfacial bonding smaller ones, increasing the effective area for mech-
was observed as a large gap between the fibre and anical interlocking between fibres and matrix, thus
matrix for the untreated composite, whereas the leading to improved interfacial bonding.
alkali-treated surface remained intact, showing . Various thermoset, thermoplastic resins and biode-
improved interfacial bonding [8]. SEM micrographs gradable/biopolymer resins have been used by
of the coir fibre-reinforced epoxy composites before researchers with the untreated and alkali-treated
alkali treatment showed more fibre pull-out, gaps at natural fibres for composite fabrication. The biopo-
fibre/matrix interface and brittle fracture of the epoxy lymer and thermoplastic resins offers the recycling
matrix. After alkali treatment, larger load was required ability and eco-friendly option. However, the
to pull-out the treated fibres from the matrix, showing major setback with them is their less mechanical
improved interfacial bonding [5]. According to Ray strength.
et al., two different failure modes were observed . Improvement, as well as deterioration of the mech-
based on the NaOH immersion time. For immersion anical, physical properties and thermal stability of
time between 0 and 4 h, fibre pull-out was the predo- the alkali-treated natural fibres and its composite,
minant failure mode, whereas for immersion time depends heavily on the NaOH concentration level,
between 6 and 8 h, failure mode was transverse fracture fibre loading % and immersion time. So, there exists
with minimum fibre pull-out [28]. According to Yousif an optimum NaOH concentration level, fibre load-
et al., the NaOH-treated kenaf/epoxy composite ing % and immersion time for each and every natu-
showed breakage only at the end of the fibres, whereas ral fibre and its composite beyond which those
untreated kenaf/epoxy composite showed de-bonding, properties face a detrimental effect as reported by
tearing, detachments and pull-out of fibres due to the several researchers.
low interfacial adhesion of fibres with the matrix . For some mercerised composites, storage modulus
[64]. According to Rout et al., the untreated coir showed an increasing trend with the increase in
fibre/polyester composite showed fibre pull outs and NaOH concentration, whereas tanδ peak curve
was left with many holes, indicating the weak fibre/ showed a decreasing trend with the increasing alkali
matrix interfacial adhesion due to the incompatibility concentration, while it was vice versa for other natu-
between the untreated fibre/polyester, whereas compo- ral fibres.
site with 5% NaOH-treated fibres showed matrix . The notable changes in the FTIR spectrum of alkali-
cracks with the fibre break at the ends, implying strong treated natural fibres were the disappearance of
characteristic peaks at certain range of wavenum- based composite, but the mechanical properties
bers, indicating the removal of cementing sub- were inferior compared to those of the natural/syn-
stances such as hemicellulose, lignin and pectin thetic fibre-reinforced hybrid composite.
regardless of the fibre employed. . Sea water treatment of the composites tends to
. For XRD, peak intensity tends to increase with the improve the interfacial adhesion between fibre and
increase in NaOH concentration (below 10%) and matrix and leads to better mechanical properties
tends to decrease beyond 10% NaOH concentration. depending on the type of natural fibre subjected to
Crystallinity index also tends to increase with the the sea water treatment.
increase in alkali concentration for the natural . Long immersion of the natural fibres and its compo-
fibres. sites to water decreases their mechanical properties
. In general, TGA results of weight loss % with like tensile strength and ILSS.
increasing temperature showed 2- and 3-phase . Mechanical properties of the pure natural fibre-
characteristics depending on the natural fibre, alkali based hybrid composite were found to be inferior
treatment conditions and immersion time. First compared to that of the natural/synthetic fibre-
phase involves the evaporation of moisture and reinforced hybrid composite.
second phase involves the removal of cementing
substances.
. DSC results from researchers indicate that only Disclosure statement
slight changes in Tg, Tc and Tm were observed for
No potential conflict of interest was reported by the authors.
natural fibres treated with different concentration
levels of NaOH, whereas the degree of
crystallinity was found to be affected significantly, Funding
indicating the transformation of cellulose I into cel-
This work is supported by the research fund from Funda-
lulose II.
mental Research Grant Scheme, Malaysia (FRGS) [grant
. Improvement in mechanical properties of the var- number 5524741].
ious composites reinforced with the alkali-treated
fibres was due to the enhanced interfacial adhesion
between the fibre and matrix as reported by several ORCID
researchers with their results from the SEM images. M. Chandrasekar http://orcid.org/0000-0002-3637-7630
. Composites reinforced with alkali-treated natural M. R. Ishak http://orcid.org/0000-0001-6923-2481
fibres showed matrix cracking, less fibre pull-out S. M. Sapuan http://orcid.org/0000-0003-0627-7951
and fibre breakage at the ends compared to the Z. Leman http://orcid.org/0000-0002-3273-6675
untreated fibre-based composite which showed de- M. Jawaid http://orcid.org/0000-0001-5348-5740
bonding, tearing, large amount of fibre pull-out.
This was due to the weak interfacial adhesion References
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ISSN: 1465-8011 (Print) 1743-2898 (Online) Journal homepage: http://www.tandfonline.com/loi/yprc20

A review on the characterisation of natural fibres

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

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

ABSTRACT ARTICLE HISTORY

Introduction Despite the advantages, there are some serious set-

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].

gravimetric analysis (TGA), dynamic mechanical

Characterisation of the alkali-treated natural

Figure 4. Process undergone by the raw fibre and its composites.

treated with the increasing NaOH concentration levels TGA

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

Kenaf fibre-reinforced composites composite and increasing the immersion temperature

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