27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

PREPARATION AND CHARACTERISATION OF

EPOXY/SILICA/KENAF COMPOSITE USING HAND LAY-UP
METHOD
C. N. Aiza Jaafar1,*, I. Zainol2 and M. A. Muhammad Rizal1
1
Faculty of Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
2
Chemistry Department, Faculty of Science and Mathematics, Universiti Pendidikan Sultan
Idris, 35900 Tanjung Malim, Perak, Malaysia

Abstract
Epoxy/silica/kenaf composites was fabricated using a simple technique of hand lay-up
method. The effect of silica content on mechanical properties of epoxy composites was
investigated by varying the silica content, ranging from 10 to 50 wt% whereas the effect of
kenaf addition on the epoxy/silica composites was studied by addition of 13 wt% of alkaline
treated kenaf fibre. The composites was fabricated in 180 mm x 180 mm metal mould and pre-
cured at 80 oC for 2 hours and post-cured at 110 oC for 2 hours. Non-woven kenaf fibre was
treated with 3 wt% NaOH to improved surface interaction between epoxy matrixes. The
mechanical properties of composites were examined by means of flexural and impact test. It is
found that 30 wt% silica content produced epoxy/silica composites with highest impact
strength i.e 6.5 kJ/m2. Addition of kenaf fibre however produce stronger composite with the
values of 54 MPa and 10.6 kJ/m2 of highest flexural and impact strength, respectively.
Scanning electron microscope (SEM) was used to observe the surface morphology of the
fractured surface of composites. SEM analysis revealed that epoxy composites with treated
kenaf fibre showed better surface interaction between kenaf fibre and epoxy resin thus exhibit
higher mechanical properties. The composite produced in this research has high potential to be
used in household and domestic product application.

Keywords: kenaf fibre, alkaline treatment, epoxy composites

1.0 INTRODUCTION

Green composite made of renewable agricultural and forestry feedstock is the best
alternatives to synthetic fibre reinforced composites. There are many advantages of using
natural fibres such as abundance, biodegradability, non-corrosive, minimal health hazard,
fracture resistance, acceptable specific properties and renewable [1]. In recent decade, the
usage of conventional fibre has found to be decreasing in demand as the natural fibre have
shown the same characteristics in term of strength and quality of the fibre. The recent
research has proven that the addition of additives such as fillers and catalyst as well as
application of chemical treatment have led to natural fibre based product can substitute the
conventional fibre. Sanjay and Yogesha, [2] reported that the natural fibre hybrid composite
is the best option to have a structure with lightweight application. The replacement of
conventional fibre with natural fibre in various industries such as manufacturing and
automotive can give benefits to the aspects of economic, environmental and social as this
type of fibre has better properties in electrical resistance and possesses good in mechanical,
thermal and insulating properties as well as high resistance to fracture [3].
It is well known that a major flaw of effectiveness of natural fibre composites are due to
contradictory between hydrophilic fibres and hydrophobic matrix. This will cause a poor in
adhesion of fibre/matrix as the presence of two conflicting elements which are pendant
hydroxyl and polar groups. As a results, it may reduce the quality of mechanical properties as
high moisture uptake occur in the composite materials [4]. To overcome this problem, the

*Corresponding author. Tel.: +603-89464379; fax: +603-86567122.

E-mail address: cnaiza@upm.edu.my
 27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

improvement of fibre matrix attraction can be done either by matrix modification engaging
additive or improving fibre surface [5].
Hand lay- up is the one technique of open moulding process that apply for
manufacturing various composites product from small to large size. The steps of this process
are: firstly, the mould is prepared with required size and shape, followed by removing the
residue and dust on it. Secondly, a first layer of releasing agent is applied to all along mould
surface in order to have a good quality surface after curing. Thirdly, a roll stock of fibre
reinforcement is placed on the mould and subsequently laminating resin is put on it by
pouring, blushing, spraying or using paint roller. This technique is known as simple and cost
effective process as it does not need require specific machine help the process. This process
is also known as a key part of composite industry because of its adaptability and quantity [6].
The objective of this research to examine the flexural and impact properties of
epoxy/kenaf composite toughened with silica filler composites. Kenaf fibre was alkaline
treated with 3 wt% of NaOH to improve interfacial interaction between matrix and fibre.

2.0 MATERIALS AND METHODS

2.1 Materials
Epoxy resin, DER 331 was supplied by Dow Chemical Pacific Singapore and
cycloaliphatic amine was used as curing agent manufactured by Epochemie. Non-woven
kenaf fibre and silica powder (44 micron) were purchased from local suppliers.

2.2 Composite preparation.

Non-wowen kenaf fibre mat was cut into 180 mm x 180 mm to fit the metal mould. The
kenaf fibre mat was treated with 3 wt% NaOH for 24 hours at room temperature and washed
with distilled water before dry in oven at 60 oC. Silica powder was dried in oven at 80 oC for
overnight. For epoxy/silica composite preparation, epoxy resin was mixed with 10, 20, 30 and
50 phr silica powder using mechanical stirrer until completely homogenised. The curing agent
was mixed to the mixture with the proportion 1:10 of resin. The mixtures were stirred and
pour into the mould uniformly and undergone curing process. For epoxy/silica/kenaf
composites preparation, the kenaf fibre mat was place on top of the thin layer epoxy/silica
resin in the mould and the second epoxy was applied on top of the fibre mat. The process was
repeated until four layers were obtained. The metal sheet was placed on top of the composite
and clamp securely before undergone curing process. The curing process was pre-cured at
80 °C for 2 hours and post- cured at 110 °C in conventional oven. After curing process and
cool at room temperature the composites were detached from the mould and label. Table 1
represents the preparation of epoxy composites with its composition.

Table 1. Epoxy composites formulation

Sample Volume Ratio

Composite Epoxy Resin Kenaf (vol%) Silica (phr)
System (vol%)
EP 100 - 0
S10 100 - 10
S20 75.5 24.5 20
S30 75.5 24.5 30
S50 75.5 24.5 50
UTK 75.5 24.5 30
TK 75.5 24.5 30
 27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

2.3 Mechanical properties

Charpy impact test were conducted according to ASTM D6110 using GUNT WP400
impact tester. The dimension of specimens were 63.5 mm x 12.7 mm. The energy required
to break the sample was recorded. The results were taken from average of 5 measurements
for each composite. Flexural test were conducted according to ASTM D790 using INSTRON
Series 8500. The dimensions of specimens were 125 mm x 12.7 mm. The support was set the
span-to-depth ratio of 16:1. The cross head speed was set at 2.0 mm/min. Flexural test was
conducted to identify the ability of sample which is the composite material that can withstand
bending forces. For each loading, the results are taken from average 4 specimens tested.

2.4 Morphology analysis of fractured surface

Field emission scanning electron microscopy (FESEM), model Hitachi SU8020 was
used to observe the morphology of the fractured surface of samples and kenaf fibre. The
sample was coated with Pt for 150second prior to analysis.

3.0 RESULTS

3.1 Alkaline treatment of kenaf fibre.

Surface morphology of the alkaline treated and untreated kenaf was analysed using SEM is
shown in Figure 1. The untreated kenaf shows rough surface with many powdery impurities
as indicated in red circle (Figure 1(a)). The impurities might come from cellulose,
hemicellulose and lignins. The powder compound attached to the surface may be from the
broken fibres. Kalia et al. [7] have reported that highly concentrated hydroxyl groups on the
surface of kenaf may develop rough topography on the surface of the fibre. The alkaline
treated kenaf however showed clean and rough surface as shown in Figure 1(b). This
treatment removed the hemicellolose, lignin, and wax from the outer surface of kenaf fibers.
Similar observation was also reported by Kasiviswanathan et al. [8] in which they reported
that the alkaline treatment washed away the impurities that stayed on kenaf surface which
improved the surface interaction between kenaf fibre and polymer matrix.

(a) (b)

Figure 1: SEM micrograph of (a) untreated (b) 3 wt% NaOH treated kenaf fibre

3.2 Impact Test

The results of impact strength of epoxy and its composites are summaries in Figure 2. It
can be seen that addition of 10 phr silica filler in composite S10 have improved the impact
strength significantly (52 %) as compared to pure epoxy (EP). The maximum impact strength
was obtained when 30 phr silica was used as a filler in epoxy/silica composites. Silica powder
act as particulate fillers that reinforced epoxy matrix by providing stress transfer between
fillers and matrix. Moreover, the fillers also exhibited a good interfacial adhesion in the
polymer matrix that also helped in higher stress transfer between fillers and matrix [6]. The
 27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

presence of kenaf fibre in composites has improved slightly the impact strength as indicated
by composites UTK. Composites TK were fabricated using alkaline treated kenaf whereas
composites UTK was fabricated using untreated kenaf fibre. The results showed in improving
the impact strength of epoxy composite (TK) as compared to untreated kenaf (UTK)
epoxy/silica composites. Overall analysis inferred that the composite UTK exhibited the
highest impact strength of 10.6 kJ/m2 which improved in 187.73 % in comparison with pure
epoxy. It is because of the continuous fibre of kenaf mat gives additional energy absorption
during impact [9].

14
Impact Strength (kJ/m2)

12
10
8
6
4
2
0
EP S10 S20 S30 S50 UTK TK
Sample

Figure 2: Impact strength of silica modified epoxy composites

3.3 Flexural Test

Figure 3 shows the flexural strength of S30, UTK, TK composites. It was observed that the
flexural strengths of epoxy/silica composites and epoxy/silica/untreated kenaf were similar
with the value about 40 MPa whereas epoxy/silica/treated kenaf showed the highest flexural
strength i.e 54 MPa. These results have proven that the alkaline treatment kenaf fibre mat in
epoxy composites enhanced the flexural strength. This is probably due to the clean kenaf
surface improved interfacial interaction between fibre and matrix, thus increased the ability of
stress transfer between fibre and matrix. The result is in agreement with the findings by Yousif
et al. [10], which studied on the pre-treatment by using sodium hydroxide (NaOH) solution for
kenaf fibres. Moreover, the application of silica powder did allow plastic void growth around
the debonded particles, which increased the difficulty of crack propagation during fracture
[11]. This will cause a relatively high loading of silica particle which is up to 30 phr that was
required to achieve a reasonable toughening effect in epoxy composite, and it could also
increase the viscosity of the resin mixtures [12].

3.4 Morphology analysis of fractured surface

Figure 4 shows the morphology of fractured surface of S30, UTK and TK composites.
The clean fracture surface of epoxy/silica composites (S30) indicated a brittle failure. This is
probably due to the silica was homogeneously distributed in entire matrix during preparation.
This observation is supported by Xue et al. [13]. SEM micrograph of epoxy/silica/untreated
kenaf (UTK) composites exhibited a rough fractured surface with fibre pull out. The pull out
fibre (red circles) indicated weak surface interaction between fibre and matrix of composite.
The pull out of silica particle can be seen as cloudy spherical shape in matrix. The dark circles
(red circles) in matrix indicated the void created by fibre pull-out. The arrows in Figure 4(b)
show the unbroken fibre that pulled out from the opposite sample’s surface. The clear pull out
of the fibres shows the interfacial adhesion of the kenaf fibres with low epoxy matrix. Based
 27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

on the findings by Yousif et al. [10], the existence of dark circles shows the failure of
composite that was contributed by the poor interfacial adhesion between fibre and matrix,
instead of the strength of the fibre itself. Composites TK (Figure 4(c)) is indicated less dark
circles but more broken fibre (red circles) distributed in the matrix. The broken fibre showed
good surface interaction between fibre and matrix, thus exhibited a higher impact and flexural
strength of the composite.

60
Flexural Strength (MPa)

50
40
30
20
10
0
S30 UTK TK
Sample

Figure 3: Flexural moduli of silica modified epoxy composites

(a) (b)

Fibre pulls out

Voids

(c)

Broken fibre

Figure 4: SEM micrograph of fractured surfaces of (a) Composite S30, (b) composite UTK
and (c) composite TK

4.0 CONCLUSION (c)

Hand lay-up method successfully produce reasonably good mechanical properties of
epoxy composites. Epoxy composite modified silica and alkaline treated kenaf exhibit the
highest impact and flexural strength which 10.6 kJ/m2, 54.1 MPa respectively. SEM analysis
 27th Scientific Conference of the Microscopy Society Malaysia (27th SCMSM 2018)

proved the alkalinisation treatment of kenaf with 3 wt% of NaOH did remove impurities from
kenaf surface and improved interfacial interaction between fibre and matrix.

5.0 ACKNOWLEDGEMENT
I would like to thank Department of Mechanical and Manufacturing Engineering,
Faculty of Engineering, Universiti Putra Malaysia for providing us funds to complete this
research.

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