Effect of NaOH soaking time on kenaf/glass fiber hybrid epoxy composites

Haslan Fadli Ahmad Marzuki, Engku Ahmadhilmi Engku Ubaidillah, Ain Farhana Wahid, Nur Ashila Shabirah
Jaffar, Nur Fatihah Mohd Saufi, and Sharifah Shahnaz Syed Bakar

Citation: AIP Conference Proceedings 1901, 030023 (2017); doi: 10.1063/1.5010488

View online: https://doi.org/10.1063/1.5010488
View Table of Contents: http://aip.scitation.org/toc/apc/1901/1
Published by the American Institute of Physics

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 Effect Of NaOH Soaking Time On Kenaf/Glass Fiber
Hybrid Epoxy Composites
Haslan Fadli Ahmad Marzuki1,a), Engku Ahmadhilmi Engku Ubaidillah1,b),
Ain Farhana Wahid2,c), Nur Ashila Shabirah Jaffar2,d), Nur Fatihah Mohd Saufi2,e),
and Sharifah Shahnaz Syed Bakar2,f)
1
Industrial Centre of Innovation (IC-I) in Industrial Design, SIRIM Berhad, Malaysia.
2
School of Materials Engineering, Universiti Malaysia Perlis, Malaysia

a)
Corresponding email: haslan@sirim.my
b)
hilmi@sirim.my
c)
aienzell@gmail.com
d)
ashilajaffar@gmail.com
e)
nurfatihahsaufi@gmail.com
f)
shahnaz@unimap.edu.my

Abstract. The study of NaOH soaking time on kenaf/glass fiber hybrid epoxy compositesis described in this work. Kenaf
fiber and glass fiber were used as filler while the matrix used was epoxy. The kenaf fiber was treated with 3% of NaOH
solution at different soaking time which were 3, 6 and 9 hours. The composite samples were produced using filament
winding process. The samples were subjected to tensile testing (ASTM 3036) to determine the mechanical properties of
kenaf filled epoxy composites and kenaf/glass fiber hybrid filled epoxy composites. The physical properties of the
composite sample were analysed using water absorption test, density test and morphological of fracture surface of
composites has undergone Scanning Electron Microscope (SEM).

INTRODUCTION
There are vast progresses which were done for these bio-based materials in the form of research and
development by the researcher in all over the countries in order to support the greener society, and sustainable
environment [1]. As the alternative use of fiber glass and carbon fiber, these natural fibers have been widely used
due to better mechanical performance in their applications [1,2]. Thermoset such as epoxies, are usually known for
its high thermal stability, high rigidity, high dimensional stability, light weight, resistance to creep and deformation
under load, besides having high electrical and thermal insulating properties [3,4].
In order to improve the mechanical properties of the thermosets matrix, they were compounded with natural
fibers to form natural fiber filled polymer matrix composites [5,6]. The arrangement of the structure of the fibers in
the composite increase the mechanical properties of the composite by restricting the propagations of a crack which
usually occurs along the matrix phase. Better adhesion between the hydrophilic fiber and the hydrophobic polymer
matrix is achieved by modifying the properties of the fibers. Thus, chemical treatments of fibers are preferred [7-
11]. The layering sequence of kevlar fibers do gives some changes on the properties of the composite. It shows that
the more the layering occurs, the better the mechanical properties of the composite. [12-14]. Despite that, hybriding
natural fiber with synthetic fibers also help to improve natural fibers composites properties [15,16]
Two layers of winding at 45 ͦ will be produced, where the samples are glass fiber, kenaf fiber, and kenaf/glass
hybird epoxy composites. Kenaf fibers are treated using 3% of NaOH solution at three different soaking times which
are 3, 6, and 9 hours. Samples then were tested by using compression testing, three point bending test, and tensile
test to determine their mechanical properties. Water absorption test and density test were done for physical

Advanced Materials for Sustainability and Growth

AIP Conf. Proc. 1901, 030023-1–030023-8; https://doi.org/10.1063/1.5010488
Published by AIP Publishing. 978-0-7354-1589-8/$30.00

030023-1
properties analysis while fracture surface will be examined by SEM to study the adhesion between fibers and
polymer matrix. The data obtained from all the tests will then be gathered and analyzed.

EXPERIMENTAL

Preparation of kenaf fiber

The kenaf fiber and glass fiber used in this study is in the form of kenaf roving yarn, supplied by Innovative
Pultrusion Sdn. Bhd. The fiber treatment was done by using sodium hydroxide, NaOH, from Dow Chemical
Company. The kenaf fiber was treated by using 3 % of NaOH solution with different soaking time. Kenaf fiber was
weighed before it was hand washed with water. Then it was soaked in NaOH solution for 3 hours, 6 hours and 9
hours respectively, before rinsed with tap water for seven times and using distilled water for final rinse. After the
treatment, it was dried under the sunlight and followed with drying process in an oven at 70 ͦ C for 12 hours.
Equation (1) was use to calculate the volume of water needed to form a 3 % of NaOH solution.

𝟑
x Vw (ml) = NaOH (g) (1)
𝟏𝟎𝟎

where Vw is volume of water required to fully soak the kenaf fiber.

Composite Preparation
Composite samples were wound using 4-axis filament winding machine in SIRIM Berhad, to produce a
cylindrical sample that consist of two layers of reinforcement. The polymeric matrix used was D.E.R.331 epoxy
resin and 905-3S Jointmine hardener. The sequence of reinforcing fiber for the samples are listed in Table 1.

TABLE 1: Fibers layer sequence in each samples prepared using filament winding process.
Sample First Layer Second Layer
1 Untreated kenaf fiber Untreated kenaf fiber
2 3 hours of treated kenaf fiber 3 hours of treated kenaf fiber
3 6 hours of treated kenaf fiber 6 hours of treated kenaf fiber
4 9 hours of treated kenaf fiber 9 hours of treated kenaf fiber
5 Glass fiber Untreated kenaf fiber
6 Glass fiber 3 hours of treated kenaf fiber
7 Glass fiber 6 hours of treated kenaf fiber
8 Glass fiber 9 hours of treated kenaf fiber
9* Glass fiber Glass fiber
Notes: *Sample 9 is a reference sample to compare the effect of hybrid and treatment on kenaf fiber with glass fiber
samples.

RESULTS AND DISCUSSION

Tensile Properties
The tensile test was done by using the Universal Testing Machine. The samples used were in the form of ring
with width of 8 mm and tested with the standard of ASTM 3036 with the speed of 10 mm/min. An increasing trend
of tensile strength was observed for kenaf fiber epoxy composite as shown in Figure 1. The lowest value of tensile
strength was shown by Sample 1 which is 1.58 MPa and the highest value of the fiber epoxy composite was shown
by Sample 9 which is 12.84 MPa. In figure 1, it shows that the increasing time of soaking from 3 hours to 6 hours in
3 % of NaOH solution has improved the tensile strength of the fiber. The alkali treatment has modified the surface
of the fiber by the removing the impurities on the surface of the kenaf fiber that provides better wettability and
interfacial adhesion among the matrix and the kenaf fiber, which contributes to a higher strength of the composites
[8]. However, kenaf fiber epoxy composite which has been treated for 9 hours has shown a slightly lower tensile
strength. This is expected due to degradation of kenaf fiber in the NaOH solution. The presence of glass fiber as a
hybrid material in the layers also contributes to increase the strength of composite samples, in range of 22 % to 25 %

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compared with composite with laminated kenaf fiber only. However this properties is still not significant compared
to the strength of pure glass fiber composite, (sample 9) itself, that is four times higher than pure kenaf and hybrid
kenaf and glass fiber samples. Yet, it shows that the hybrid between kenaf fiber and glass fiber does contribute to
produce a composite structure with a better mechanical properties [16].
16.00

14.00

12.00
Tensile Strength (MPa)

10.00

8.00

6.00

4.00

2.00

0.00
1 2 3 4 5 6 7 8 9
Samples

FIGURE 1. Comparison of tensile strength of sample consisting of kenaf fiber (untreated and treated), hybrid of glass/kenaf
(untreated and treated) and glass fiber reinforced epoxy composite

Figure 2 has shown an increasing pattern of elongation at break for kenaf fiber epoxy composite. Among the
kenaf samples, Sample 1 which is the pure untreated kenaf, has the highest elongation at break of 5.46 %. This is
due to poor interfacial adhesion between the reinforcement and the matrix that is cause by impurities and waxy
properties on the fiber surfaces. Treated kenaf (Sample 2) have lower elongation that is 2.96 % which shows an
improvement on the interfacial adhesion as result of better surface contact between the fibers and the matrix.
However, the longer period of soaking cause the fiber to degrade and easily deteriorated when load is continuously
applied. This trends were also displayed on the hybrid samples. Therefore, it can be concluded that, the treatment on
the kenaf fiber is to removed the impurities on the fiber surfaces to allow good interfacial adhesion and surface
contact (9).
Combining tensile and elongation data, it shows that modulus of elasticity for treated kenaf increases when
compared to untreated kenaf, as shown in Figure 3. Sample 2 and 3 have higher modulus elasticity compared to
sample 1 and the same trends were observed for the hybrid samples. The treated kenaf removed impurities and
provide surface roughness for the fibers, that allows good interfacial adhesion. This will give good strength value as
well as less strain as result from mechanical interlocking mechanism. As for the hybrid composite, the properties of
glass fiber contribute to provide better mechanical properties in terms of strength, strain and modulus of elasticity.
Longer soaking time will cause the fiber to degrade and easily deteriorate when load is continuously applied, as
resulted in sample 4 and sample 8.

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 9

7
Elongation at Break (%)

0
1 2 3 4 5 6 7 8 9
Samples

FIGURE 2. Comparison of elongation at break for sample consist of kenaf fiber (untreated and treated), hybrid of glass/kenaf
(untreated and treated) and glass fiber reinforced epoxy composite

1.8

1.6

1.4
Modulus of Elasticity (GPa)

1.2

0.8

0.6

0.4

0.2

0
1 2 3 4 5 6 7 8 9
Samples

FIGURE 3. Comparison of modulus of elongation for samples which consist of kenaf fiber (untreated and treated), hybrid of
glass/kenaf (untreated and treated) and glass fiber reinforced epoxy composite

Scanning Electron Microscopy (SEM)

Figure 4 shows the SEM image of tensile surface fracture for sample 1, 2, 4, and 7. Sample 1 shows the image of
non-wetting of kenaf fiber by the matrix. The impurities on the surface were observed of the non-treatment kenaf
fiber and the voids were caused by the fiber pull out. The treatment conducted will remove the impurities and will

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result with good surface roughness that will allow the mechanical interlocking mechanism to take place as shown by
sample 2. For sample 4, as the soaking time increased to 9 hours, the fiber tends degrade and form voids on its
surface. The fibers pull out shows the poor adhesion between fiber and matrix. Due to the presence of the voids, the
fiber mechanical properties will decrease in its values. Thus, the fiber could easily break when being exerted on a
certain force. Sample 7 shows that after being treated for 6 hours, the impurities on the surface of the kenaf fiber
have been almost gone and the mechanical properties of the fiber have improved. As the kenaf fiber wound together
with glass fiber, the mechanical properties of this hybrid epoxy composite is approaching the mechanical properties
of the glass fiber epoxy composite. Thus, this will result in a higher strength of the sample.

Sample 1 Sample 2

Sample 4 Sample 7

FIGURE 4. Microscopy image on kenaf, glass and hybrid samples

Density Test and Water Absorption

Density test was conducted using densimeter. From the conducted test (Figure 5), it shows that the highest
density is given by sample 9 while the lowest density is given by sample 1. High density value shows that the
sample has the lowest porosity while the lowest density value shows that the sample have the highest porosity.
Samples that consists only kenaf fiber, either untreated or treated showed a difference in density about 1.2 %, while

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the hybrid sample that consists of glass fiber and kenaf fiber have a difference about 1.5 %. Therefore this analysis
does not represent a significant effect of treated fiber on the composite properties.

1.8

1.6

1.4
Density, ρ (g/cm3)

1.2

0.8

0.6

0.4

0.2

0
Sample 1 Sample 2 Sample 3 Sample 4 Sample 5 Sample 6 Sample 7 Sample 8 Sample 9
FIGURE 5. Density of Kenaf fiber, Glass fiber and Kenaf/Glass fiber hybrid epoxy composite

The water absorption test was conducted for 17 days as shown in Figure 6. Sample were immersed in distilled
water and the mass was measured daily. From this test, it shows that percentage of water absorption increased
gradually across time before constant starting from day 14. According to A.M Yaacob, 2011 [16], percentages of
water absorption is directly proportional to the value of porosity. Therefore it reflects on presence of voids and
porosity in the sample, which allow water to penetrate into the structure per day. The percentage of sample 9 is the
lowest that is 7.07 % and it start showing constant pattern after day 8 and maintains its weight throughout time. This
indicates least absorption amount of water throughout the testing duration.
As the highest percentage of the water absorption have been shown by sample 1, of 32.12 % and keep on
increasing although after day 14. It is observed that untreated kenaf fiber shows a lack of drapability during winding
on the mandrel. Therefore this condition contributes to the formation of pores between fiber layers due to cross-over
during winding process, which result with high porosity and contribute to higher percentages of water absorption.
When the kenaf fiber is treated, despite removing the impurities and increase the surface roughness, it also assist the
fiber drapability during processing. Therefore it produces less pores that result in lower water absorption
percentages. In addition, according to Fiore, 2015 [8], hemicellulose, wax and oil covering the surface of natural
fiber have been removed after the treatment. Therefore, after treatment, the hydroxyl group that is present in
cellulose and hemicellulose which could be penetrated by water will be eliminated from the surface of the kenaf
fiber. Thus, these will result to a lower porosity of the kenaf fiber. This is also shown in figure 5, where as the
treatment soaking time increase, percentages of water absorption also decrease from 27.41 % to 24.21 % for pure
kenaf fiber and from 14.04 % to 7.17 % for hybrid samples. Again, hybriding kenaf fiber and glass fiber helps to
reduce the porosity of the sample, as resulted in lower value of water absorption percentages.

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 35.00
Sample 1

30.00
Sample 2

Sample 3
Percentages of Water Absorption, %

25.00
Sample 4

20.00 Sample 5

15.00 Sample 6

10.00
Sample 7
Sample 8

Sample 9
5.00

0.00
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Immersion Day
FIGURE 6. Percentage of water absorption versus time of kenaf fiber, glass fiber and kenaf/glass fiber hybrid epoxy composite

CONCLUSIONS
Based on the analysis conducted, it shows that NaOH treatment increase kenaf fiber surface roughness that
contributes to better interfacial adhesion which result in better mechanical properties for kenaf fiber composites. It
also contributes to kenaf fiber drapability during processing with filament winding techniques. However, longer
soaking time will damage the fibers property on morphological, in which the fiber will deteriorate easily during
mechanical loading. Glass fiber is a synthetic fiber that can be hybridized with kenaf fiber to improve the properties
of the kenaf fiber in a fiber reinforced composite application, that include improving the difficulties during
processing, increase the mechanical properties and reducing the water absorption percentages.

ACKNOWLEDGEMENTS
This work was financially supported by University Malaysia Perlis, and the samples were fabricated by using
filament winding machine at Industrial Centre of Innovation, (IC-I), SIRIM Berhad in Kulim, Kedah.

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