Hindawi Publishing Corporation

Journal of Composites
Volume 2014, Article ID 350737, 12 pages
http://dx.doi.org/10.1155/2014/350737

Research Article
Interfacial Adhesion Characteristics of Kenaf Fibres Subjected to
Different Polymer Matrices and Fibre Treatments

Umar Nirmal, Saijod T. W. Lau, and Jamil Hashim

Centre of Advanced Materials and Green Technologies, Faculty of Engineering and Technology, Multimedia University,
75450 Jalan Ayer Keroh Lama, Melaka, Malaysia

Correspondence should be addressed to Umar Nirmal; [email protected]

Received 15 July 2014; Revised 9 October 2014; Accepted 12 October 2014; Published 6 November 2014

Academic Editor: Sandro C. Amico

Copyright © 2014 Umar Nirmal et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

This study is aimed at determining the interfacial adhesion strength (IAS) of kenaf fibres using different chemical treatments in
hydrochloric (HCl) and sodium hydroxide (NaOH) with different concentrations. Single fibre pullout tests (SFPT) were carried out
for both untreated and treated fibres partially embedded into three different polymer matrices; polyester, epoxy, and polyurethane
(PU) as reinforcement blocks and tested under dry loading conditions. The study revealed that kenaf fibres treated with 6% NaOH
subjected to polyester, epoxy, and PU matrices exhibits excellent IAS while poor in acidic treatment. The effect of SFPT results was
mainly attributed to chemical composition of the fibres, types of fibre treatments, and variation in resin viscosities. By scanning
electron microscopy examination of the material failure morphology, the fibres experienced brittle and ductile fibre breakage
mechanisms after treatment with acidic and alkaline solutions.

1. Introduction extensively in many structural applications such as natural

fibre reinforced car roof and catamaran hull. Moreover,
Presently, critical driving forces such as cost, weight reduction due to overwhelming interest of using natural fibres in the
coupled with increased emphasis in research on renewable aforesaid, Quig and Dennison [4] and Nirmal et al. [7]
materials has resulted in extensive growing interests on have forecasted that there will be a dramatic increase of
natural fibres for composite applications. This is due to the more than USD $1634 million potential on the consumption
fact that natural fibres are less costly and have low specific of natural fibre composites in various applications, mainly
weight and higher strength and stiffness than glass fibre in aerospace industry, marine sector, automotive industry,
which was previously reported by Gill and Yousif [1]. Liu et al. sporting segments, and construction industries.
[2] reported that natural fibres are readily available from Greater potential on the use of natural fibre composites is
renewable sources, where their production requires little apparent with the enhanced performance of treated natural
energy by taking in CO2 and releasing O2 back to the environ- fibres. Many published works done by Aziz and Ansell [8],
ment. Furthermore, Joshi et al. [3] and Quig and Dennison Aziz et al. [9], John and Thomas [10], McNally and McCord
[4] revealed that natural fibres possess good thermal and [11], Ray [12], Mwaikambo and Bisanda [13], Yousif and Ku
acoustic insulating properties, low in density (i.e., low wear [14], Alsaeed et al. [15], Shalwan and Yousif [16], Brown [17],
of tooling and no skin irritation), and are producible with Brahmakumar et al. [18], and Kenins [19] have shown that
low investment. However, Fukuhara [5] stated that natural chemical treatments enhanced the mechanical performance
fibre composites exhibit low environmental impact resistance of treated natural fibres compared to the untreated ones.
and are subject to moist degradation that had limited their In the case of alkaline treatment, Nirmal et al. [20] and
usage on nonstructural applications. Recent research by Pothan et al. [21] indicated that greater improvements on
Dillon [6] showed that significant improvements of these natural fibre reinforced composites can be attained because
properties can be attained via appropriate fibre treatment. As of removal of impurities on fibre surface and its lignin
a result, treated natural fibre composites are now being used (which is hydrophilic), thus exposing more of the cellulosic
2 Journal of Composites

fibre region that allows it to be bonded cohesively with Table 1: Chemical composition of kenaf fibres [29].
the polymer matrix. Besides, Sgriccia et al. [22] highlighted
Composition wt.%
that silane treatment generally coats the fibre surface which
creates a chemical bridge between the natural fibre and the Cellulose 45–57
matrix, thereby increasing the bonding strength between Hemicellulose 20–22
the fibre and matrix. Leman et al. [23] and Harper [24] Lignin 8–13
revealed in their work that chemical treatment also reduces Pectin 3–5
the hydrophilic nature of a natural fibre and improves the
lifespan by reducing development of fungi. Further than that,
160
Pothan et al. [21] and Torres and Cubillas [25] investigated the
effects of chemical treatment using stearic acid on mechanical 140
bonding strength between flax fibre and polypropylene. They
concluded that acid treatment modified flax fibre surface but 120
not the fibre bulk.
Other than chemical treatments, attempts were made to 100

Observations
enhance mechanical properties of natural fibre reinforced dfibre(avg.) = 51.8 𝜇m
80
plastic composites by modifying the resin properties. How-
ever, very limited work has been carried out in comparing the 60
difference in mechanical properties of natural fibre reinforced
with varying resin properties. Cordes and Daniel [26] used 40
four different types of polyester resin to reinforce kenaf fibre.
In the study, results showed that modified polyester enables 20
the kenaf fibre to bond firmly with the resin matrix thereby 0
enhancing its mechanical properties of the composite . In the 0 20 40 60 80 100 120
year 2011, Nirmal et al. [20] investigated single fibre pullout Kenaf diameter (𝜇m)
test using betelnut reinforced thermosetting composites,
namely, epoxy and polyester. Experimental results revealed Figure 1: Determination of effective average diameter of kenaf fibre.
that epoxy gave better performance compared to polyester
resin due to the fact that epoxy has lower viscosity compared
to polyester which increased fibre surface wettability and 2. Materials Preparation
improved fibre bonding with the matrix.
In recent years, more focus has been made in investigating 2.1. Preparation of Fibres. Kenaf fibre (Hibiscus cannabinus
mechanical properties and tribological characteristics using L.) used for the current work was obtained from Malaysian
kenaf fibre as the reinforcing agent for composites. Many Agricultural Research and Development Institute (MARDI).
researchers such as John and Thomas [10], Narish et al. [27], Raw fibres as received contained dust and husk; therefore it
Chin and Yousif [28], Bernard et al. [29], and Nishino et al. was subjected to a thorough cleaning process. Firstly, the raw
[30] evaluated the tribological performance and mechanical fibres were dusted in open air before being cleansed by using
properties of treated and untreated kenaf fibre reinforced domestic water to remove the dust and impurities present.
composites and concluded that the latter had shown excellent This is followed with oven drying for 24 hours at 40∘ C. Next,
alternative to glass fibre composites and metallic composites the fibres were gently combed unidirectionally and placed on
in specific applications. a clean paper sheet. The cleaned fibres were then separately
From the compilation of work done on kenaf fibre com- soaked in sodium hydroxide (NaOH) and hydrochloric acid
posites by Kim et al. [31], it can be said that the mechanical (HCl) of 4% and 6% concentrations, for 12 hours at room
strength of the composites relies on the content of fibre in temperature. After that, the fibres were taken out from their
the composites (up to 70% vol). Most of the treatments done respective treatments and rinsed using distilled water. The
by researchers such as Leman et al. [23], Harper [24], and fibres were then dried in oven at 40∘ C for 24 hours. Finally,
Agrawal et al. [32] (i.e., alkaline and silane treatment) were the untreated and treated fibres were cut to desired lengths
proven to enhance the mechanical properties of composites. (∼100 mm) for test specimen preparations. By means of a 10X
In general, mechanical failures of these composites are mostly NK Vision microscope, the kenaf diameter was determined
due to fibre pullout, fibre debonding, and fibre breakage. from a control sample size containing 160 sets of individual
Based on published works, limited literature is available kenaf fibres. Distribution of different kenaf fibre diameters
on the effects of fibre treatment (alkaline and acid) and with respect to the number of observations is presented in
concentration of chemical treatment on the mechanical Figure 1. Based on Figure 1, the average diameter of the kenaf
properties and interfacial adhesion strength of kenaf fibre. fibre cross section is 51.8 𝜇m. The chemical composition of
Therefore, this study is necessary in order to evaluate the kenaf fibres is presented in Table 1. It is to be noted here that
interfacial adhesion strength between untreated kenaf fibre the idea of using NaOH and HCl treatment is to explore the
and chemically treated kenaf fibre impregnated in thermoset possibility to promote high adhesion strength of the kenaf
(epoxy, polyester) and thermoplastic (polyurethane) matrices fibre by means of “chemically coupling” the treated fibres
at dry loading conditions. to the polymer resin. Although it is generally known that
Journal of Composites 3

(a) Untreated kenaf fibre

(b) 4%-HCL (c) 6%-HCL

(d) 4%-NaOH (e) 6%-NaOH

Figure 2: SEM images showing the difference of kenaf fibre texture because of various chemical treatments compared to untreated fibre.

acidic treatment could destroy the natural fibre by means of 2.2. Types of Polymer Resins Used and Their Basic Properties.
acidic deterioration, some review works claimed the opposite In the current study, influence of different polymer resin on
[33, 34]. interfacial adhesion strength was considered. Thermoplas-
Micrographs of untreated and treated kenaf fibres are tic polyutherene (Mirathane 5117A/B), thermoset polyester
presented in Figures 2(a)–2(e). In Figure 2(a), impurities can (Butanox M-60), and thermoset epoxy (DER 331) resins have
be clearly seen on the surface of the untreated fibre although been adopted as polymer matrices for the present study.
the fibre has been thoroughly cleaned using domestic water. Besides being locally manufactured and easily available, these
On the other hand, chemically treated fibres in 4% HCl resins as specified by Nirmal et al. [20], Narish et al. [27], and
and NaOH (Figures 2(b) and 2(d)) revealed lesser amount Nirmal et al. [43] were selected due to their cost effectiveness
of impurities along the surface. Describing possibilities of and wide applications. Table 2 highlights some of the different
impurities dissolved in the solution, Figure 2(c) shows the types of polymers and their main applications.
fibre treated in 6% HCl solution with evidence of clean but For thermosetting resin, Butanox M-60 unsaturated
rough surface. Similar results were observed for 6% NaOH polyester resin was mixed with 1.5 wt% of methyl ethyl
treated fibres (Figure 2(e)) with clean and smooth outer sur- ketone peroxide (MEKP). On the other hand, thermoset
face. With 6% NaOH treatment, traces of impurities were not epoxy used is a liquid reaction product of Epichlorohydrin
observed indicating higher surface area of bonding between and Bisphenol-A. The curing agent used was polyamide. The
fibre and matrix. epoxy resin and hardener were mixed uniformly at a weight
4 Journal of Composites

Resin poured inside the Adhesive

“U” shaped cavity tape
Elastomer Le Adhesive tape
zinc mould Resin Drilled hole

Kenaf fibre
50 mm 50 mm
(a) Fabrication method of the pullout test specimens (b) Prepared pullout test specimen

Figure 3: (a) Schematic illustration of the mould and (b) corresponding test specimen.

Table 2: Types of polymers and their applications. into the zinc mould as illustrated in Figure 3(a). It is to
be noted here that the kenaf fibre diameters vary largely
Thermoset polymers as it is derived naturally. Hence, to control (i.e., minimize
Types Applications the fibre diameter variation) the fibre’s diameter, the fibres
Polyester [35–37] Composite material/bearing application were selected from the control sample size containing 160
Epoxides [38–40] Boat hulls/composite material individual kenaf fibres. Finally, resin was poured into the
Thermoplastic polymers mould cavity and allowed to cure at 26 ± 2∘ C for 24 hours
Types Applications before further curing in an oven for 12 hours at 40∘ C. Lastly,
Polyutherene [41, 42] Name tags/canopies/lenses for car lights a hole of 6 mm in diameter is drilled through the block at
determined distance from the edge (𝐿 𝑒 = 20 mm). This was
done to cut off the fibre length embedded in the resin where
Table 3: Basic properties of the different types of resin used at 25∘ C. the effective fibre length for the pullout test was set at 20 mm.
Polyester Butanox M-60 Figure 3(b) gives a schematic illustration of prepared pullout
Physical state Liquid
test specimens.
Density 1170 kg/m3
Viscosity 25 mPa⋅s 3. Experimental Procedure
Epoxy DER 331
Single fibre pullout tests (SFPT) were performed using
Physical state Liquid the universal test system (1000Q Standalone) shown in
Density 1100 kg/m3 Figure 4(a), with a loading speed of 1 mm/min. Yousif et al.
Viscosity 15000 mPa⋅s [37] indicated that the accuracy of the machine is 70.5% of
Polyurethane Mirathane 5117-A/B reading from full scale to 0.2% load cell capacity per ASTM
Physical state Liquid E4 and 0.1% of setting (0.05% at 10 in/min).
Density 1400 kg/m3 SFPT was carried out to determine the interfacial adhe-
Viscosity 5200 mPa⋅s sion characteristics between untreated and treated kenaf fibre
embedded in different polymer matrix. Figure 4(b) gives an
illustration of the direction of loading force, with test speci-
ratio of 2 : 1. Concerning thermoplastic resin, Mirathane mens firmly clamped together using the jaw clamps. Experi-
5117-A was adopted. The resin was mixed uniformly with ments were conducted under room temperature conditions
hardener (Mirathane 5117-B) at a mixing ratio of 100 : 35 by and each test was repeated five times before the average
weight percentage. Information of the three polymer resins results were tabulated. Interfacial adhesion strength (𝜏𝑖 ) for
used is listed in Table 3. current study was determined using

𝐹debonding (max)
2.3. Preparation of Composite. Interfacial adhesion com- 𝜏𝑖 = , (1)
posites were fabricated according to established research 𝑑fibre × 𝜋 × 𝐿 𝑒
methods for fibre pullout test done by Quek and Yue [44],
Wong et al. [35], and Valadez-Gonzalez et al. [36]. Firstly, a where 𝜏𝑖 = interfacial adhesion strength, 𝐹debonding (max) =
“U” shaped zinc channel with cross section dimensions of maximum force just before debonding occurs (refer Figure 5),
25.4 mm × 25.4 mm was used as a mould. Using elastomers 𝑑fibre = corresponding fibre’s diameter measured in 𝜇m, 𝐿 𝑒 =
cut to size with the width of zinc mould, a small hole insertion 20 ± 0.05 mm.
was made through the centre of each of the elastomers. Next,
the mould inner walls were sprayed with a layer of a release 4. Results and Discussions
agent. Then, kenaf fibres from the control sample size (cf.
Figure 1) were carefully inserted into the holes made through The corresponding results on the average maximum debond-
the elastomer using tweezers and the whole set-up was placed ing force of the kenaf fibre subjected to different types of
Journal of Composites 5

Applied
load

Adhesive
tape

50 mm
Kenaf fibre

20 ± 0.05 mm
m
Resin

Clamping
jaws
(a) (b)

Figure 4: (a) Universal test machine; (b) schematic illustration of test specimen and direction of loading force for an IAS test.

4.0 4.0

3.5 3.5

3.0 3.0
Fdebonding(max) (N)

Fdebonding(max) (N)

2.5 2.5

2.0 2.0

1.5 1.5

1.0 1.0

0.5 0.5

0.0 0.0
Ut H4 H6 N4 N6 Ut H4 H6 N4 N6
Types of treatment (%) Types of treatment (%)
(a) Polyester (b) Epoxy
4.0

3.5

3.0
Fdebonding(max) (N)

2.5

2.0

1.5

1.0

0.5

0.0
Ut H4 H6 N4 N6
Types of treatment (%)
(c) Polyurethane

Figure 5: Average maximum debonding force (𝐹d ) for untreated (Ut) and treated kenaf fibre subjected to different polymer resins. Remark:
H: hydrochloric acid, N: sodium hydroxide.
6 Journal of Composites

Debonding

Fibre breakage Torn fibre

“Brittle-like” fracture of fibre
Smooth surface
Chipped off Single fibre
polyester Fibre rupture
Fibre breakage
mechanism

Fibre breakage Fibre split

Impurities mechanism

Loose fibre

(a) Polyester-Ut (b) Polyester-H4

Fibre breakage
mechanism

“Brittle-like” fracture of fibre

Debonding
Micro crack on
fibre surface Torn fibre
Smooth surface
Broken fibre

Fibre contraction

(c) Polyester-H6 (d) Polyester-N4

Fibre breakage
Single fibre

Fibre strands
“Ductile-like” fibre breakage

(e) Polyester-N6

Figure 6: Corresponding SEM images after the pullout test for untreated and treated kenaf fibre using polyester as the resin.

chemical treatments and matrices are presented in Figures polyurethane matrices, respectively, compared to untreated
5(a)–5(c). fibre. On the contrary, 6% HCl has worsened average max-
imum debonding force. The debonding force was decreased
4.1. Effect of Fibre Treatments. In general, Figure 5 indicates by 43%, 42.5%, and 11.9% subjected to polyester, epoxy, and
that the 6% NaOH treated kenaf fibre recorded the highest polyurethane matrices, respectively, compared to untreated
debonding force before fibre breakage/debonding for all fibre. The treatment with 6% NaOH resulted in the highest
the different types of matrices (i.e., polyester, epoxy, and value of IAS because of a complete removal of impurities
polyurethane). This is followed by the 4% NaOH treated on the kenaf fibre outer surfaces, hence increasing fibre
kenaf fibre, which yields the second highest average load. surface roughness, which is crucial during fabricating of
Remarkably, the maximum debonding force was low for all SFPT specimens (i.e., enhanced surface wettability of the
different matrices when the fibres were treated with HCl. fibre/matrix). From a reported work by Khan et al. [38],
There was a significant drop on the maximum debonding the residue on the fibre is the major reason in reducing the
force with higher HCl concentration (6% HCl). In summary, bonding strength between fibre and resin. Furthermore, Aziz
6% NaOH fibre treatment served to boost the average and Ansell [8] and Aziz et al. [9] confirmed in their work that
maximum debonding force by 51.6%, 86.6%, and 86.1%, the effect of alkaline treatment on kenaf fibres served to boost
with the kenaf fibre embedded in polyester, epoxy, and the mechanical properties of the composites as compared to
Journal of Composites 7

Fibre breakage
Single fibre Detached fibre stripes from single fibre

Torn fibre

Smooth surface

“Brittle-like” fracture of fibre Micro crack

Impurities

Hollow spots

(a) Epoxy-Ut (b) Epoxy-H4

Debonding

Debonding
Loose fibre

Macro crack
Deteriorated fibre

Fibre breakage

“Ductile-like” fibre breakage

(c) Epoxy-H6 (d) Epoxy-N4

“Ductile-like” fibre breakage

Fibre breakage

Debonding
Sign of fibre contraction

(e) Epoxy-N6

Figure 7: Corresponding SEM images after the pullout test for untreated and treated kenaf fibre using epoxy as the resin.

the untreated fibres. Moreover, Aziz and Ansell [8], Aziz et al. of the high delamination rate on the outer surfaces of the
[9], Huda et al. [39], Yousif and El-Tayeb [40], and Rokbi [41] kenaf fibre (cf. Figures 2(b) and 2(c)). More explanations on
revealed that alkaline treatment can remove impurities and the IAS will be discussed in Section 4.2 with the assistance of
lignocellulosic wax present on the fibre surface. It was also the SEM images.
reported by Aziz and Ansell [8], Aziz et al. [9], Quek and
Yue [44], and Oláh and Vancso [42] that alkaline treatment 4.2. Observation of SEM Morphology. The corresponding
had the potential to improve interfacial adhesion strength SEM images after the pullout test for the untreated and
between natural fibres and resin matrix, reduce composite treated kenaf fibre at different fibre treatments subjected to
porosity, and enhance wear performance of the composite. polyester, epoxy, and PU resins are shown in Figures 6–
However, acidic treatment (4% and 6% HCl) on kenaf fibres 8, respectively. Before taking the micrographs, the pullout
did not improve IAS of the fibre/matrix. This could be because samples were coated with a thin layer of gold by using an
8 Journal of Composites

Detached fibre strand

Fibre breakage
mechanism
Fibre detached from matrix “Brittle-like” fracture of fibre

Crack at Tiny hollow

resinous spots
Fibre breakage
region

Impurities
Sign of fibre contraction

(a) PU-Ut (b) PU-H4

Massive debonding

Debonding
Fibre breakage
Fibre split Detached fibre
Fibre split

Sign of brittle fracture

(c) PU-H6 (d) PU-N4

Fibre still in good shape Fibre breakage

Fibre axis

Rough fibre surface

(e) PU-N6

Figure 8: Corresponding SEM images after the pullout test for untreated and treated kenaf fibre using polyurethane (PU) as the resin.

ion sputtering model: JEOL, JFC-1600. The samples were debonding of the fibre against the matrix is evidenced. Similar
analyzed by SEM machine model: EVO 50 ZEISS-7636. All sign of defects can be seen when the fibres were subjected to
observing conditions were performed at room temperature epoxy resin for the untreated and treated samples; compare
of 28 ± 5∘ C and at humidity level of 80 ± 10%. Tables 4, 5, and Figure 7. Figure 8 illustrates the SEM images of the untreated
6 summarize the comparison of SFPT in polyester, epoxy, and and treated samples after the pullout tests subjected to PU
PU resin, respectively. resin. Generally, it is observed that the untreated samples
Figure 6 illustrates the micrograph images of single kenaf exhibited fibre breakage after the pullout test associated with
fibre subjected to polyester resin at different treatments. From slight fibre pullout. This fibre pullout could be due to the
the figure, effect of acidic and alkaline treatment has changed impurities on the fibre surfaces which lowered the surface
the properties of the fibre’s surface. Brittle-like fracture was wettability of the fibre against the resin matrix, that is, low
observed after the pullout test when the fibre was treated with IAS. When the fibres were treated with HCl, a brittle-like
HCl treatment. For alkaline treatment, the pullout samples fracture was evidenced at the end of the fibre after the pullout.
exhibited a ductile-like fracture. For the untreated samples, There was evidence of tiny hollow spots and deformed fibre
Journal of Composites 9

Table 4: Main fibre pullout mechanisms and their brief remarks for the different types of fibre treatments used subjected to polyester matrix
at dry loading conditions.

Polyester
Corresponding SEM Fibre
Brief remark/explanation Main fibre pullout mechanism
figure treatment
Debonding of fibre observed associated with slight
Fibre breakage associated with slight torn
Figure 6(a) Untreated chipping of polyester because of impurities on fibre
fibre from the core of the fibre
surfaces
(i) Sign of fibre rupture from the core of the fibre after
the pullout
(ii) Tendency of fibre to split from the main single fibre
Brittle-like fracture at end of fibre was
Figure 6(b) 4% HCl was high which contributed to many loose fibres
observed because of the acidic treatment
(iii) Fibre surfaces were smooth which ruined the
interfacial adhesion strength of the fibre against the
matrix
(i) Sign of fibre contraction during the SFPT
(ii) Fibre surfaces were smooth which lowered the IAS
Brittle-like fracture at end of fibre was
Figure 6(c) 6% HCl of the fibre and matrix
observed because of the acidic treatment
(iii) Sign of micro cracks on fibre surfaces which cause
the fibre to break during the pullout test
(i) Slight debonding of fibre with matrix
(ii) Fibre was torn apart from the main core fibre after
Figure 6(d) 4% NaOH Pure fibre breakage
the test indicating high interlocking capabilities of the
fibre and matrix
Evidence of many fibre strands from the core of the
Ductile-like breakage was observed at the
Figure 6(e) 6% NaOH fibre indicating that the fibre resisted the pullout force
end of the fibre
during the test

Table 5: Main fibre pullout mechanisms and their brief remarks for the different types of fibre treatments used subjected to epoxy matrix at
dry loading conditions.

Epoxy
Corresponding SEM Fibre
Brief remark/explanation Main fibre pullout mechanism
figure treatment
High amount of impurities observed on the fibre
Fibre breakage associated with mild torn
Figure 7(a) Untreated surfaces which significantly lowered the IAS of the fibre
fibre
and matrix
(i) Fibre stripes were easily detached from the core
main fibre because of the hollow spots on fibre surfaces
which contributed to stress concentrations during SFPT
Brittle-like fracture at end of fibre was
Figure 7(b) 4% HCl causing severe micro cracks on fibre surface
observed because of the acidic treatment
(ii) Relatively smooth fibre surfaces after the treatment
which did not contribute to any improvement in IAS of
the fibre against the matrix
(i) Massive debonding of fibre associated with macro
crack at the resinous region indicating that fibre could
not even withstand the low pullout force (less than Deteriorated fibre at the end of fibre
Figure 7(c) 6% HCl
0.8 N) breakage
(ii) Fibre easily ruptured because of high acidic
treatment
(i) Slight debonding of fibre was observed associated
with some loose fibre detached from the main core fibre
Ductile-like breakage was observed at the
Figure 7(d) 4% NaOH indicating that the fibre could withstand the high
end of the fibre
pullout force
(ii) Rough fibre surfaces
Slight debonding of fibre associated with severe signs of
fibre contractions which denotes that the fibre could Ductile-like breakage was observed at the
Figure 7(e) 6% NaOH
withstand the increment in pullout force (more than end of the fibre
2 N) during SFPT
10 Journal of Composites

Table 6: Main fibre pullout mechanisms and their brief remarks for the different types of fibre treatments used subjected to polyurethane
matrix at dry loading conditions.

Polyurethane
Corresponding SEM Fibre
Brief remark/explanation Main fibre pullout mechanism
figure treatment
(i) Fibre was detached from matrix which caused
several fibre strands still embedded in the matrix
(ii) Sign of impurities on fibre surfaces which could
Figure 8(a) Untreated Fibre breakage with slight pullout
have caused severe crack at the resinous region during
the pullout (i.e., the impurities on the fibre surfaces
were forced out from the matrix)
(i) Sign of low fibre contraction and deformed fibre
surfaces due to the treatment
Brittle-like fracture at end of fibre was
Figure 8(b) 4% HCl (ii) Many tiny hollow spots on fibre surfaces which
observed because of the acidic treatment
caused several weak points (i.e., stress concentrations)
during the pullout
(i) Massive debonding associated with high amount of
fibre split from the main core fibre
(ii) Fibre could easily get detached as it was brittle after
Figure 8(c) 6% HCl the treatment Torn fibre and slight fibre pullout
(iii) However, the signs of fibre splits also showed that
the fibre resisted the pullout force when it was
embedded in PU as the matrix
Figure 8(d) 4% NaOH Slight debonding of fibre was seen at the resinous region Pure fibre breakage
(i) A rough fibre surface was observed after the
treatment which resisted the fibre from pulling out
from the matrix
Figure 8(e) 6% NaOH (ii) End of fibre breakage was still in good shape Pure fibre breakage
indicating that the fibre could withstand the high
pullout force (more than 3 N), thus increasing the IAS
of the fibre and matrix

surfaces which could be the reason why acidic treatment has Table 7: Improvement in IAS for the different treated kenaf fibre
degraded the IAS properties of fibre. For the case of alkaline when compared to the untreated kenaf fibres subjected to the
treatment, pure fibre breakage was evidence after the pullout different matrices.
test. The evidence from the SEM images suggests that the end H4 H6 N4 N6
of fibre breakage region was still in good shape indicating that
Polyester −15% −43% +37% +52%
the fibre could withstand the high pullout force. More details (3%) (4%) (3%) (4%)
on the fibre pullout mechanisms and their explanation are
Epoxy −25% −43% +71% +87%
provided in Tables 4–6 respectively. (4%) (4%) (4%) (3%)
In summary, comparison of IAS with different kenaf fibre
−16% −12% +45% +86%
treatment as compared to the untreated ones subjected to Polyurethane
(3%) (3%) (3%) (4%)
different types of matrices is presented in Table 7. From the
Note. All values in brackets represent the corresponding standard deviations
table, positive (+) sign denotes improvement in IAS while
as a result of repeating the measurements for five times.
negative (−) sign showed degradation of IAS of the fibre at
their respective treated conditions compared to the untreated
fibre. It can be seen that the improvement of IAS followed the
order of N6 > N4 > H4 >>> H6 for polyester and epoxy It is interesting to compare the current work with similar
matrices; 6% of NaOH fibre treatment demonstrated excel- work done by Nirmal et al. [20] using betelnut fibres. In
lent improvement in IAS of the fibre/matrix while 6% HCl that work, IAS of betelnut fibres treated with N6 increased
fibre treatment gave the worst IAS properties. However, when by about 141% and 115% when the fibres were embedded
the fibre was embedded in PU, the IAS followed the order of in polyester and epoxy resins, respectively, compared to the
N6 > N4 >>> H6 > H4. The slight difference in the order of untreated ones. Meanwhile, IAS decreased by about 4% and
IAS could have been owing to the type of resin used during 33% when the fibres were treated with H6 and embedded in
the SFPT. Therefore, more investigations on the chemical polyester and epoxy resins compared to the untreated ones.
analysis of the fibre and different types of treatments and resin When mapping these findings to the current work, it is noted
used are proposed in future works. that a much higher IAS is attainable using betelnut fibres as
Journal of Composites 11

compared to kenaf fibres; that is, IAS of betelnut fibres treated [6] J. H. Dillon, “Current problems and future trends in synthetic
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