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EFFECTS OF NANOFILLERS ON FLEXURAL, IMPACT ENERGY AND

WATER ABSORPTION PROPERTIES OF WOVEN HYBRID KENAF/GLASS IN


EPOXY NANOCOMPOSITES

SARINA ATIQA MSKIN

168559

A Proposal Submitted In Partial Fulfilment of the Requirement for Bachelor Degree


of Engineering (Aerospace)

Department of Aerospace Engineering

Faculty of Engineering

Universiti Putra Malaysia

Serdang, Selangor Darul Ehsan

June 2016

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ACKNOWLEDGEMENT

First and foremost I am grateful to God that had granted me good health

throughout this one year to complete my project. I would like also to express my

deepest gratitude to my parents and family who have been supported me and being a

source of motivation from beginning of this final year project until I finished writing

full thesis. Next, I wish to express my sincere thanks to my beloved supervisor, Dr

Norkhairunnisa Mazlan and examiners Ir. Dr. Mohamed Thariq bin Haji Hameed

Sultan and Dr. Chia Chen Ciang who has guide me to carry out my project, gives

thousand of helpful advice, revise my thesis draft and corrected my final draft report

until I can submit full report on time. I place on record, my sincere thanks to staff in

Department of Biocomposite at INTROP, Upm for providing me with all necessary

facilities and teach me how to use related machine used in my project. Not to forget,

I am also grateful to staff and lab technician in Department of Aerospace,

Department of Mechanical and Department of Chemical engineering Upm for letting

me used their lab and facilities related to complete my project. Finally, I took this

opportunity to express my gratitude to all my fellow friends that support, encourage

and motivate me through this venture.

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ABSTRACT

Natural fibre is getting famous nowadays due to their significant mechanical

properties that could replace the use synthetic fibre. Due to the low cost and

renewable source, there is an increase in demand of natural fibre. In this research,

Kenaf fibre is used as natural fibre and combines with synthetic fibre which is glass

fibre to make hybrid kenaf/ glass composite. Kenaf fibre is chosen due to its

significant mechanical properties compared to other natural fibre 20. Glass fibre is

added to strengthen the mechanical properties of hybrid composite. The hybrid

composite used epoxy as the matrix and silicone filler as matrix modification. In this

research, nanoclay and carbon nanotube is used as filler with percent of 1-wt%, 3-

wt%, 5-wt% and 7-wt%. From the flexural and impact test, the optimum

performance is at 3-wt% filler. For nanoclay sample, S3 the flexural strength and

modulus are 1726.69Mpa and 124.41Gpa respectively. While for carbon nanotube

sample, S7 the flexural strength and modulus are 9% and 20% lesser than S3

respectively. In addition, S3 absorb 17.063J energy and S7 absorb 13.907J energy.

As for water absorption test, all samples with addition filler give low water uptake

than S1 sample except for that sample with more voids.

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ABSTRAK

Gentian semulajadi semakin terkenal pada masa kini kerana sifat

mekanikalnya yang mempunyai potensi yang tinggi untuk menggantikan penggunaan

gentian sintetik. Disebabkan oleh kos yang rendah dan sumber yang boleh

diperbaharui, permintaan gentian asli semakin meningkat dipasaran. Dalam kajian

ini, gentian kenaf adalah salah satu gentian semulajadi akan digabungkan dengan

gentian kaca untuk membuat kenaf hybrid kaca komposit. Gentian kenaf dipilih oleh

kerana sifat-sifat mekanikalnya yang lebih baik berbanding gentian semulajadi yang

lain. Sementara itu, gentian kaca ditambah adalah untuk mengukuhkan sifat-sifat

mekanikal komposit hibrid. Dalam komposit hibrid ini, jenis maktrik yang digunakan

ialah epoksi dan silicon pengisi digunakan sebagai pengubahsuaian matrik epoksi.

Dalam kajian ini, nanoclay dan karbon nanotiub digunakan sebagai pengisi dengan

pelbagai peratus iaitu 1%, 3%, 5% dan 7% berat. Dari ujian lentur dan kesan

hentakkan, prestasi optimum dikalangan semua pengisi adalah pada 3% berat

pengisi. Untuk sampel nanoclay (S3), kekuatan lenturan dan modulus masing-masing

ialah 1726.69MPa dan 124.41GPa. Manakala bagi sampel karbon nanotiub (S7),

kekuatan lenturan dan modulus masing-masing ialah 9% dan 20% rendah daripada

sampel S3. Disamping itu, S3 menyerap tenaga 17.063J dan S7 menyerap tenaga

sebanyak 13.907J. Tambahan lagi, bagi ujian penyerapan air, semua sample dengan

adanya pengisi menunjukkan pengambilan air yang rendah berbanding S1 kecuali

sample yang mempunyai banyak lompang.

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Table of Contents

ACKNOWLEDGEMENT ....................................................................................................... i
ABSTRACT............................................................................................................................ ii

CHAPTER 1 ........................................................................................................................... 1
INTRODUCTION .................................................................................................................. 1
1.0 Problem Statement ........................................................................................................... 2
1.1 Objectives ................................................................................................................... 3

CHAPTER 2 ........................................................................................................................... 3
LITERATURE REVIEW........................................................................................................ 3
2.1 Composite Material ........................................................................................................... 4

CHAPTER 3 ......................................................................................................................... 42
METHODOLOGY ............................................................................................................... 42
3.1 Materials ......................................................................................................................... 42
3.2 Specimen preparation ...................................................................................................... 43
3.3 Flexural test ..................................................................................................................... 44
3.4 Impact test ....................................................................................................................... 45
3.5 Water Absorption Test .................................................................................................... 45
3.6 Morphology observation ................................................................................................. 46

CHAPTER 4 ......................................................................................................................... 47
RESULT ............................................................................................................................... 47
4.1 Flexural test ..................................................................................................................... 47
4.2 Impact test ....................................................................................................................... 51
4.3 Water absorption test....................................................................................................... 53

CONCLUSIONS................................................................................................................... 56
REFERENCE........................................................................................................................ 59
APPENDIX………………………………………………………………………………….65

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List of table

Table 2.1 Advantage and disadvantage of resin polymer ........................................................ 5


Table 2.2 Advantages and disadvantages of NFRPs ............................................................... 7
Figure 2.3 Examples of Natural Fibre ..................................................................................... 7
Table 2.4 Results of Natural fibre researches .......................................................................... 8
Table 2.5 Properties of natural fibres .................................................................................... 11
Table 2.6 Flexural and Impact strength result ....................................................................... 13
Table 2.7 Mechanical result of warp and weft direction........................................................ 14
Table 2.8 Mechanical properties of kenaf composite ............................................................ 16
Table 2.9 Result of resin system on mechanical properties of kenaf fibre laminates............. 17
Table 2.10 Result of mechanical properties .......................................................................... 19
Table 2.11 Result of fabricated composite ............................................................................ 21
Table 2.12 Flexural test result at 20% fibre ........................................................................... 22
Table 2.13 Samples’ Result ................................................................................................... 25
Table 2.14 Result of flexural strength and energy absorbed at different fibre orientation ..... 27
Table 2.15 Flexural result with and without CNT filer ......................................................... 32
Table 2.16 Flexural result with and without silica filler ........................................................ 32
Table 2.17 Test results .......................................................................................................... 36
Table 2.18 Density of materials ............................................................................................ 43
Table 2.19 Sample notation ................................................................................................... 43
Table 2.20 Result of Impacted Damage area ......................................................................... 52

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List of figure

Figure 2.1 Structural of reinforced part ................................................................................... 4


Figure 2.2 Variation of tensile strength and tensile modulus................................................... 6
Figure 2.3 Example of woven fabrics.................................................................................... 12
Figure 2.4 SEM images ......................................................................................................... 18
Figure 2.5 SEM images of Jute and Kenaf composite ........................................................... 20
Figure 2.6 Result of impact strength ..................................................................................... 23
Figure 2.7 Result of Flexural properties ................................................................................ 30
Figure 2.8 Microstructure of PBSu under transmission electron microscopy ........................ 31
Figure 2.9 SEM images of epoxy coated with silica at (a) 80% vol. silica (b) 95% vol. silica
.............................................................................................................................................. 33
Figure 2.10 Graph of Flexural result ..................................................................................... 38
Figure 3.1 Material used ....................................................................................................... 42
Figure 3.2 Drop weight machine ........................................................................................... 45
Figure 3.3 Scanning Electron Microscope (S-3400N)........................................................... 46
Figure 4.1 Effects of adding nanoclay or carbon nanotubes on the flexural strength of
kenaf/glass/epoxy composite................................................................................................. 47
Figure 4.2 Effects of adding nanoclay or carbon nanotubes on the flexural modulus of
kenaf/glass/epoxy composite................................................................................................. 48
Figure 4.3 SEM image of S3 (3-wt% nanoclay) .................................................................... 49
Figure 4.4 SEM image of S3 (3-wt% carbon nanotube) ........................................................ 49
Figure 4.5 Effects of adding nanoclay or carbon nanotubes on the flexural strain of
kenaf/glass/epoxy composite................................................................................................. 50
Figure 4.6 Effects of adding nanoclay or carbon nanotubes on the energy absorption of
kenaf/glass/epoxy composite................................................................................................. 51
Figure 4.7 Water absorption result of kenaf/glass/epoxy composite filled with nanoclay ..... 53
Figure 4.8 Water absorption result of kenaf/glass/epoxy composite filled with carbon
nanotube ................................................................................................................................ 54
Figure 4.9 Water absorption results of E and E-S composite ................................................ 55

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CHAPTER 1

INTRODUCTION

In the recent decades, the combination of natural fibre composite based glass

fibre has been one of the major interesting research subjects due to increase in

market demand that needed composite with low cost but has good performance.

Furthermore, natural fibres are lighter and cheaper which can be obtained by natural

resources compared to glass fibre which is synthetically made of 1. One of the

application that use natural fibre mats is on automotive application which is car

bumper that use hybrid kenaf/glass (Davoodi et al 2010).

In addition, natural fibres have been studied extensively to investigate its

mechanical properties and to determine which natural fibre gives superior result. In

this research, the focus is on the study of the mechanical properties which is flexural

testing, impact testing and water absorption behaviour of nanocomposite. One of the

most significant current discussions in nanotechnology is compatibility of nanofiller

with the fabricated composite.

The aim of this present work is to study the hybridization of kenaf fibre and

glass fibre mat with the inclusion of nanofiller. The study was conducted at first

varying the filler content and performing the mechanical testing and water absorption

test. Finally, a comparison is made to find out which composite gives the best

performance.

1
1.0 Problem Statement

For many years, the manufacturing of polymer composite matrix (PMC) has

been controversial due to its uses in many applications including aerospace,

automotive, medical devices and naval applications. PMCs contain matrix and

reinforce fibre in which about 50 percent reinforcing fibre by volume. The examples

of reinforce fibre carbon/graphite, glass, aramid, kenaf (natural fibre) and many

more.

A few recent years ago, natural fibre has growing extensively in term of

market demand. Due to its low weight, low density, low cost, biodegrable, higher

strength and stiffness2 3, natural fibre become one of the most popular material for

composites application. Because of PMC do not rust, it has good corrosion resistance

characteristic over steel or galvanized steel. Since both PMC and natural fibre are

used in many industries, there is a need to reinforce PMC and natural fibre with new

material for better result (materials properties). The current composites already

posses good mechanical properties, but with the idea of addition of nanofillers to the

PMC will probably increase the flexural and compressive strength.

The reason why PMC need to be improved is because to fulfil high demand

in high risk industries that need a very strong material that has ability to delay

component failure. The reinforcement of PMC and nanofillers such as carbon

nanotube, nanoclay, aerojel and nanofibre are expected to give better performance

than current reinforcement of PMC. This research will focus on polymer matrix of

kenaf/epoxy and reinforce kenaf/epoxy with nanofillers.

2
1.1 Objectives

The purpose of this paper is to study and evaluate the properties of

composites with nanofillers. The detailed objectives are as follows:

a. To investigate the effect of nanofillers in laminated composite.

b. To determine the flexural and energy absorption for newly developed

composites.

c. To understand the morphology of developed composites

CHAPTER 2

LITERATURE REVIEW

3
2.1 Composite Material

Composite material can be defined as the combination of two or more

material with purpose to obtain better properties than those of individual

components. Because of good mechanical properties posses by composite material,

there are more researches carried out to combine new types of composite material to

fulfil market demand. Composite material consists of reinforcing phase and matrix

phase. Usually, the reinforcing phase is stronger, harder and provides high stiffness

than matrix. The reinforcement is usually fibre or particles. There are several layup

of reinforced fibre such as unidirectional continuous/discontinuous, bi-

directionalcontinuous and random discontinuous. The structural of reinforced part is

as show in Figure 2.1

Figure 2.1 Structural of reinforced part 4

Meanwhile, the matrix phase will hold fibres together and acts as medium to

transfer stress between fibres. The matrix can be polymer, ceramics or metal.

4
Furthermore, matrix is responsible to ensure proper orientation and spacing between

matrix and reinforcing phase. Matrix also protect the reinforce fibre from abrasion

and the environment. The major types of composites are metal matrix composite

(MMC), ceramic matrix composite (CMC), and polymer matrix composite (PMC). 4

Polymer matrix composite is popular in natural fibre composite. There are

two types of matrix in PMC which are thermoplastics resin and thermoset resin.

Table 2.1 shows advantages and disadvantages of thermoset and thermoplastics

resin.

Table 2.1 Advantage and disadvantage of resin polymer

Thermoset resin Thermoplastic resin

Advantages

• Excellent resistance to solvents • High impact resistance compared


and corrosives. to thermoset resin
• Resistance to heat and high • Ability to reform (physical
temperature. change)
• Fatigue strength
• Tailored elasticity
• Excellent adhesion
• Excellent finishing (polishing,
painting, etc)
Disadvantages
• Once catalyzed, thermoset cannot • Naturally solid state of
be reversed or reformed thermoplastic resin makes it more
difficult to imprenate reinforcing

5
fiber.

Examples of thermoset resin are unsaturated polyesters, epoxies and vinyl

esters. At first, a thermoset will start at low viscosity resin that react and cures during

processing, forming and intractable solid between fibres. Among those types of

thermosets, epoxy is important matrix for fibres reinforced polymer which had been

used in many industries. The advantages of epoxy are it has high strength and

modulus, low shrinkage and last but not least it has excellent chemical and heat

resistance.5 Figure 2.2 shows the variation of tensile strength and modulus for

polyester, epoxy and vinyl ester. As can be seen, epoxy has relatively good tensile

strength and modulus which makes it suitable in fibre reinforced polymer.

Figure 2.2 Variation of tensile strength and tensile modulus 6

2.2 Natural fibre reinforced polymer

It has been well known about the manufacture of natural fibre reinforced

polymer because of its significant advantages. . Table 2.2 shows the advantages and

disadvantages of natural fibre reinforced composite. Generally, natural fibre is a non

6
synthetic material that is not manmade. It is originated from plants or animals.

Animal fibres contain wool, silk, and avian fibre. It includes sheep’s wool, goat hair,

feathers and so on. The plants produce cellulose fibre such as bast fibres, seed fibres,

leaf fibres, grass and reed fibres, and core fibres. The examples of that cellulose are

based on Table 2.3.

Table 2.2 Advantages and disadvantages of NFRPs

Advantages Disadvantages
• Low cost • High moisture absorption
• Low density • Lower durability than synthetic
• Good thermal and mechanical fiber composite (can be improved
resistivity with treatment)
• Environmental friendly • Lower processing temperatures
(renewable source) limiting matrix options
• Desirable fiber aspect ratio • Lower strength compared to
• High specific stiffness and synthetic fibre composite
strength

Figure 2.3 Examples of Natural Fibre

Cellulose fibre types Examples

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Bast Jute, flax, ramie, hemp, kenaf
Seed Cotton, coir, kapok
Leaf Sisal, pineapple, abaca
Grass and reed Rice, corn, wheat
Core Hemp, kenaf, jute

Fibre reinforced polymer seem to be increase in demand due to its relatively

low weight and low cost. Other significant advantages of fibre reinforced polymer

are has good mechanical properties such as tensile and flexural modulus and

renewable resources. In this study, woven kenaf fibre is chosen to be reinforced fibre

in natural fibre reinforced fibre and epoxy resin as the matrix.

There are many research conducted regarding on combination of natural fibre

with thermoset matrix including hybrid composite. In this research paper will be

focused more on flexural, impact and water absorption properties.

Table 2.4 Results of Natural fibre researches


Composite Flexural Energy Water Gap studies Ref
absorption uptake
Strength Modulus (J)
(MPa) (GPa)
1 Phormium Authors did Santulli et
/epoxy- 43.0±2.0 0.8±0.255 - - not vary the al.
manually fibre (2009)7
extracted content and
Phormium only fixed
/epoxy- 60.5±4.0 4.4±0.2 the fibre at
manually 16wt%
extracted phormium
2 Treated - - Particle Author used Anbukara
mat 50% 110.0 fibre hand layup si,.
of Luffa/ gives technique. (2014)8
epoxy low For future
Untreated - moisture work vary
mat 50% 48.0 absorptio the
of Luffa/ n technique of
epoxy fabricating
process to

8
make
comparison

3 15mm 59.69 9.13 - - Authors did Venkates


Banana/ not consider hwaran et
sisal/ for fibre al.
epoxy treatment. (2011)9
4 Treated Authors did Behnaz
yarn 100.0 11.0 - - not do fibre Baghaei
Hemp/ treatment et al.
PLA (0°) for non (2014)10
Hemp/PLA - - woven
non woven 76.0 7.8 hemp and
yarn 99.0 10.8 - - also
Hemp/ composite
PLA(0°) with
yarn 60.0 6.0 - - direction
Hemp/ 45° and 90°
PLA(45°)
yarn 32.0 4.0 - -
Hemp/
PLA(90°)
5 Jute/epoxy Authors Vivek
BJFE- 43 2.35 2.87 - focus only Mishra,
0wt% on varying Sandhyar
BJFE- 30 0.50 3.89 - fibre ani
Biswas.
12wt% loading.
(2013)11
BJFE- 35 0.60 4.26 - Further
24wt% research can
BJFE- 52 1.30 4.59 - consider
36wt% fibre
BJFE- 55 3.00 4.88 - treatmetn
48wt%
6 Glass/jute/ Authors Amit
polyester only did Bindal et
flexural test al.
J 79.38 14.60 - Very after (2013) 12
high conducting
JG 297.54 19.50 - Low water
JG 276.35 21.50 - Very low absorption
(chopped test. For
strand future work
mat) can
JG 119.61 11.90 - High compare
(surface flexural test
veil) without
conduct
water

9
absorption
test.
7 Kenaf/ Dry After Dr Aft Authors Osman,E
Polyester water y er focus on et al.
abs. wat untreated (2011)
test er fibre. 13
abs.
Should
test
compare
both treat
0 wt% - Very low and
- - - -
kenaf untreated
fibre
10 wt% - Low
kenaf 58 23 3.8 1.5

20 wt% 79 35 4.3 1.6 - Average


kenaf
30 wt% 56 13 4.0 1.6 - High
kenaf

40 wt% 38 25 3.6 1.3 - Very


kenaf high

8 Flax/ Authors Huner,


Epoxy Dry After Dr Aft focus on U.
water y er untreated (2015)14
abs. wat flax fibre
test er
and did not
abs.
test
do
morphology
observation
1wt% flax 42 40 3.0 3.2 - Low
5wt% flax 51 48 3.4 3.9 - High
10 wt% 75 60 4.2 4.6 - Very
flax high
9 Hybrid Authors Gupta et
sisal/glass/ focus only al
15
epoxy on untreated (2015)
sisal fibre.
S5G5 166.88 10.95 - Very low They used
S10G10 207.02 12.97 - Low same fibre
S15G15 411.43 20.81 - High length of
S20G20 331.63 18.40 - Very sisal.
high

10
2.2.1 Woven kenaf fibre

Kenaf fibre is made by or produced from a species of Hibiscus cannabinus.

Hibiscus family is a biodegradable and environmental friendly crop. There are three

types of fibre which is more related to the constituent of kenaf plant which are bast,

core and pith.

Mechanical properties of natural fibre are affected by cellulose content.

Whereas cellulose content is depend on several aspects which are fibre length, fibre

loading or volume fraction of fibres, fibre aspect ratio, fibre orientation or interfacial

adhesion between fibre-matrix.16 In addition, it has been reported that tensile and

flexural properties of biocomposite depend on kenaf fibre loading.17 Studies have

found that kenaf bast fibre possess good mechanical properties as compared to kenaf

core and kenaf pith18 19


. Table 4 shows the mechanical properties of natural fibres.

As shown in Table 2.4, kenaf exhibit good mechanical properties than other natural

fibres.

Table 2.5 Properties of natural fibres 20


fiber Tensile strength Young’s Elongation at Density (g/𝑐𝑚3 )
(Mpa) modulus (Gpa) break (%)
Bamboo 140-230 11-17 - 0.6-1.1
Coir 175 4-6 30 1.2
Oil balm 248 32 25 0.7-1.55
Bagasse 290 17 - 1.25
Ramie 560 24.5 2.5 1.5
Flax 345-1035 27.6 2.7-3.2 1.5
Hemp 690 70 1.6 1.48
Jute 393-773 26.5 1.5-1.8 1.3
Kenaf 930 53 1.6 -
Sisal 511-635 9.4-2.2 2.0-2.5 1.5

11
Pineapple 400-627 1.44 14.5 0.8-1.6
Curaua 500-1150 11.8 3.7-4.3 1.4

Natural fibres are usually used in different form of orientations in fibre-

reinforced polymer composites for instance continuous, randomly oriented and

woven fabric mat. Woven fabric is much more attractive form because it provides

excellent integrity and conformability for structural applications. Different weaving

pattern gives different mechanical properties of natural fibre reinforced polymer.

Figure 2.3 shows examples of woven fabric

Figure 2.3 Example of woven fabrics

There are several researches had been done to investigate the effect of woven

pattern to mechanical properties of composite material which are as follow.

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Alavudeen et al. (2015) conduct research to investigate the effect of weaving

pattern and random orientation on mechanical properties toward composite material.

They observed that the strength of composite depends on weave pattern, fiber

orientation and the bonding between fibre and matrix. The types of weave patterns

used are plain and twirl types. From the result obtained, plain woven gives the higher

12
tensile and flexural strength than twirl woven composite. This might be due to the

uniform distribution of stress transfer when tensile load is applied on both transverse

and longitudinal directions. The authors also stated that the fibre in plain woven

structure are interlaces one-to-one in both weft and warp direction which is not

presence in twirl woven. The experimental result of flexural and impact strength is

shown in Table 2.6. From the result, for individual fibre composites, kenaf/polyester

composite shows high flexural strength than banana/polyester composites. This is

due to the densified structure of kenaf fibre which contributed in high flexural

strength. For impact strength, it depends on the interfacial and interlaminar adhesion

between fibre and the matrix. However, for the same weaving pattern impact strength

is depend on the strength and structure of individual fibre constituent.

Table 2.6 Flexural and Impact strength result

Plain woven Flexural strength (Mpa) Impact strength (kJ/m²)


pattern
composite
Banana/polyester 80 19
Kenaf/polyester 110 23
Hybrid 170 25
banana/kenaf

22
Arifuzzaman Khan et al. (2013) done a comparison between woven jute fabric

(WJF) and non-woven with poly (L-lactic acid) (PLLA) was conducted to study its

mechanical properties which are tensile, flexural and impact. This research also

investigates the effect of treated and untreated composite toward mechanical

properties. As expected, treated WJF/PLLA composite shows the highest value of

tensile strength, tensile modulus, flexural strength, flexural modulus and impact

strength. The result also shows that the mechanical properties in warp direction is

13
highest than in weft direction. Mechanical result of warp direction is different form

weft direction because of higher yarn and low density of warp direction. The overall

result is in Table 2.7.

From Table 2.7, flexural behaviour showed higher value in warp direction

than weft direction. This is due to the short yarns in weft direction of composites

limit their distributiom of tensile stress. When the tensile stress tries to propagate

upward, delamination failure occurred and caused a reduction in flexural strength.23

For impact test, woven fabric cause fibre yarns of warp direction cross over fibre at

weft direction to create an interlocking structure.

The impact strength for both directions is higher than unreinforced PLLA.

This indicates that woven fabric is good as they interact with the crack formation in

the matrix and at the same time act as stress-transferring medium. Result of impact

strength also shows higher value in warp direction because it contained higher

aligned fibre and thus produced composites with higher resistance to impact stress.

Table 2.7 Mechanical result of warp and weft direction

Specimen Flexural Impact


Strength (Mpa) Modulus (Gpa) Strength
(kJ/ m²)
Unreinforced PLLA 42+
− 9.7 3.02+
− 0.8 8.82+− 0.9

NWJF/ PLLA 67+


− 8.4 2.83+
− 1.1 12.98+
− 1.1
composite
At warp direction:

Untreated WJF/PLLA 82+


− 12.0 4.3+
− 0.10 16.4+
− 1.8
composite
Treated WJF/PLLA 121 +
− 13.4 5.3+
− 0.10 18.1+
− 2.3
composite

14
At weft direction:

Untreated WJF/PLLA 81+


− 9.4 3.62+
− 0.08 14.3+
− 1.5
composite
Treated WJF/PLLA 111+
− 8.1 4.72+
− 0.05 16.6+
− 1.8
composite

2.2.2 Kenaf/epoxy composite

For the few decades, there was increasingly demand on product that used

kenaf material such as paper product, building material, absorbent and livestock feed.

Previous study has reported that kenaf has good strength and low density enough to

replace glass fibres that requires much higher energy to produce it. Due to low cost

of kenaf, it is often be used in natural fibres reinforcing material.

There are several research on kenaf/epoxy composite was conducted

regarding to determine flexural, impact and water absorption properties of kenaf

composite. For every research that had been done, the result is different which is due

to the environmental aspect and different fabrication process.

24
Bakar et al. (2014) reported a research on low velocity impact resistant on

kenaf/epoxy and kenaf/polyester composite. In their research, the fibre weight


15
percentages are varied in order to investigate the tensile properties for both

composites. The kenaf fibre loading is varied from 10 wt-% to 25 wt-%. From the

result obtained, the optimum performance of mechanical properties is at 25 wt-%.

Kenaf/polyester composite shows good impact resistance and stiffness than

kenaf/epoxy.

Table 2.8 shows the comparison of kenaf/epoxy and kenaf/polyester

composites based on its mechanical properties. From the result shows in Table 2.8,

impact energy increase as the fibre loading increased. This indicates good adhesion

between fibre and matrix. However, kenaf/polyester composites result in higher

strength than kenaf/epoxy because impact strength of polyester resin is higher than

epoxy. Besides, the deflection of composite at maximum load is depends on the fibre

content.

Table 2.8 Mechanical properties of kenaf composite

Kenaf content (wt-%) Energy absorbed (J)


Kenaf/epoxy Kenaf/polyester
10 1.62 2.42
15 2.83 2.94
20 2.42 4.57
25 2.80 4.58

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S. Rassmann et al. (2010) conduct a research regarding on effect of resin system

on the mechanical properties and water absorption of kenaf fibre reinforced

laminates. The resins used in this experiment were polyester, vinyl ester and epoxy.

Table 2.9 shows the result of resin system on different kenaf fibre volume content.

From the result obtained in this research, it can be concluded here that epoxy resin

16
system has good strength values since epoxy resulted in good tensile strength and

flexural strength than polyester and vinyl ester. The authors stated that high or low

value of flexural strength is due to presence of voids in the composite. The

mechanical properties of kenaf/epoxy composite increase as the fibre content

increase.

Table 2.9 Result of resin system on mechanical properties of kenaf fibre laminates 25

Resin Fibre Tensile Flexural Impact


volume Strength Modulus Strength Modulus Energy Strength
(%) (Mpa) (Gpa) (Mpa) (Gpa) (J/cm) (Mpa)

15 49.0 3.25 72.5 3.60 0.22 14.0


Epoxy 22.5 52.5 3.99 84.0 4.40 0.34 23.0
30 63.5 4.40 92.0 4.49 0.42 24.5
15 28.0 4.25 5.99 3.95 0.36 22.5
Polyester 22.5 42.0 6.30 82.5 4.50 0.57 31.0
30 52.0 6.60 99.5 5.20 0.68 37.5
15 43.0 4.50 76.0 3.30 0.28 15.1
Vinyl 22.5 53.0 5.30 80.0 4.20 0.47 25.1
ester 30 66.5 5.55 82.5 4.60 0.62 34.0

For the polyester resin, from the result polyester has good modulus and

impact properties. For vinyl ester resin, it has good water absorption characteristics

as it absorb less water than polyester and epoxy resin. Furthermore, from scanning

microscope it is found out that epoxy resin bonds is better than the others as epoxy

laminates failed by fibre fracture while polyester laminates failed by fibre pull-out

17
and vinyl ester failed by two combination of these. Figure 2.4 shows the SEM

images of resin system.

a) Unsaturated polyester b) Vinyl ester

c) Epoxy

Figure 2.4 SEM images 25

26
Naveenkumar R et al. (2014) conducted a research to compare mechanical

properties between jute and kenaf fibre reinforced with epoxy resin. From the result

from this research, it shows that kenaf fibre possessed superior mechanical properties

than jute fibre. For the impact test, the response in each fibre composites indicates a

failure process involving crack initiation and growth in the fibre breakage, fibre pull-

out, delaminating and disbanding. The overall result is presented in Table 2.10.

18
Table 2.10 Result of mechanical properties

Composite Tensile Flexural Impact


Strength Modulus Strength Modulus strength (J/mm)
(Mpa) (Gpa) (Mpa) (Gpa)
Jute/epoxy 22.187 5.856 81.134 9.408 114.350
Kenaf/epoxy 34.831 6.692 85.600 - 121.900

By observing both composite sample under microscopy scanning electron,

from the SEM images for flexural test it show fracture in fibre bundle and

incomplete distribution of fibre and matrix. The image of jute fibre as shown in

Figure 2.5 b) shows fibre pull out that might explain low impact strength than kenaf

composite.

19
a) Kenaf fibre

b) Jute fibre

Figure 2.5 SEM images of Jute and Kenaf composite 26

Yakubu Dan-mallam et al. (2015) 27 study the behaviour of interwoven kenaf/ PET

(polyethylene terephthalate) reinforced epoxy hybrid composite. The result obtained

in Table 2.11 shows an increase of mechanical properties of hybrid kenaf/PET

composite than individual epoxy.

20
Table 2.11 Result of fabricated composite

Composite Flexural properties Impact strength Water absorption


Strength Modulus (J/cm) (%)
(Mpa) (Gpa)
Neat epoxy 32.0 1.40 3.50 0.15
Epoxy/kenaf/PET 38.0 2.00 12.50 4.00
(70/15/15)
Epoxy/kenaf/PET 80.0 4.50 32.00 2.10
(60/20/20)

The reason why the flexural strength increase when the fibre content is

increase is may be due to ability of interwoven fabric to withstand bending force.

Other factors that attribute to increase in flexural strength are due to interlocking

structure of fibre in matrix, individual reinforcement properties and fibre-matrix

interfacial adhesion. Increase in flexural modulus is may be due to strong bind

between fibre and matrix that cause short delamination which result in high flexural

modulus. For impact strength, the hybrid composite show improvement than neat

epoxy is because of incorporation of between kenaf and PET in interwoven fabric,

interlocking structure, and orientation of composite.

For percentage of water absorption, an increase in fibre content resulted in

decreasing of absorption of water. This is due to the drop in void content that cause

decrease in porosity and surface roughness, and strong interfacial bond.

28
Abu bakar et al. (2011) compared the mechanical properties of kenaf/epoxy

composite with and without liquid epoxidized natural rubber (LENR) in epoxy resin.

With the presence of LENR in kenaf/epoxy composite, the flexural properties are

higher than without LENR and neat epoxy. Based on result obtained, the optimum

performance of flexural properties was at 20% fibre. The result is show in Table

21
2.12. The flexural properties increase up to 20% fibre and decrease when further

increase the fibre content. Factor that may contribute to this increase is good

interfacial strength between fibre and matrix. With the presence of LENR in the

epoxy cause strong interface and improved the flexural strength of composite. The

result also show a decrease in flexural strength at 25% fibre which may be cause by

poor adhesion between fibre and matrix and also presence voids.

The improvement in flexural modulus is due to toughening caused by LENR

modification of LENR in the matrix. This toughening behaviour gave good energy

absorbing capacity of the composite.

Table 2.12 Flexural test result at 20% fibre

Composite Flexural properties


Strength (Mpa) Modulus (Gpa)
Kenaf/epoxy 56.33 3.4
Kenaf/epoxy + LENR 43.42 2.3

2.3 Hybrid kenaf/glass composite

In this research, kenaf fibre is hybridized with glass fibre and reinforced with

epoxy resin. Combination of natural and synthetic fibre produced composite with

good mechanical properties than single constituent natural fibre reinforced polymer.

Many researchers conducted experiment to study the mechanical properties of hybrid

natural and synthetic fibre. It is proven that hybrid natural and synthetic fibre gives

22
greater resistance to water absorption, cost saving by using of renewable fibre,
29
weight saving and improved in properties. The following researches are some

example to investigate the properties of hybrid kenaf/glass reinforced polymer.

30
Davoodi, M. M. et al. (2011) study the impact property of adding polybutylene

terephthalate (PBT) in hybrid kenaf/glass epoxy composite. They also investigate

other mechanical properties such as tensile and flexural properties. They compare

three samples which are glass/epoxy composite, hybrid kenaf/glass epoxy composite

and hybrid kenaf/glass epoxy composite with PBT.

As a result, impact strength in the presence of PBT was higher than without

the addition of PBT. This is because, the PBT particles were uniformly dispersed

which increased the interlaminate shear of epoxy resin film between plies.

Consequently energy absorption and toughness of the hybrid composite will increase.

As expected, glass/epoxy composite resulted in higher impact strength than other two

composites. The impact strength result is illustrated in Figure 2.6.

Figure 2.6 Result of impact strength 30

23
For flexural properties, hybrid kenaf/glass which is without PBT particle

show the highest value of flexural strength and modulus followed by hybrid

kenaf/glass with PBT and glass composite.

31
Atiqah et al. (2013) investigated mechanical properties of kenaf-glass (KG) fibres

reinforced unsaturated polyester hybrid composite. They compare the properties of

treated and untreated kenaf fibre toward the properties of hybrid composite. In their

work, unsaturated polyester resin and KG fibre at ratio of 70:30 by volume were

used. In addition, kenaf and glass fibre composition are varied by volume for

example (7.5/22.5 v/v), (15/15 v/v) and (22.5/7.5 v/v).

The result obtained shows that combination of (15/15 v/v) KG fibre gives

good mechanical properties than other combination. In other word, 15/15 v/v KG

fibre is the optimum and suitable combination among others. As expected, hybrid

composite with treated kenaf shows higher properties (flexural,tensile and impact)

than untreated kenaf. For flexural test, hybrid treated kenaf-glass show highest value

which is 453.22 MPa at 15/15 KG treated kenaf gives high value because of

consolidation of fibre composite which was achieved through combination of

compaction, matrix impregnation and curing.

For impact test, the result shows good impact strength at 15/15 v/v hybrid KG

which is 146.43 MPa. As mentioned before, treated kenaf give good properties than

untreated which is because treated sample did not slip into layer after impact testing.

Furthermore, fibre mat orientation which was randomly oriented can withstand the

impact force. In addition, for impact test the impact strength of the composite is

higher at higher glass fibre content. At higher kenaf fibre content, the composite

24
cannot withstand higher impact loading and resulting less toughness and more brittle

properties.

32
Muhammad et al. (2015) study the effect of adding liquid epoxidized natural

rubber (LENR) toward hybrid kenaf-glass reinforced epoxy composite. They also

compare treated and untreated kenaf fibre toward properties of hybrid composite.

Overall result of this research is in Table 2.13.

Table 2.13 Samples’ Result

Sample Impact strength (kJ/m²) Flexural properties


Strength Modulus
(MPa) (Gpa)
Neat epoxy 5.2 33.0 1.7
Hybrid kenaf/glass
Untreated fibre 7.0 59.0 2.8
Treated fibre 9.3 65.0 3.6
Hybrid kenaf/glass+LENR
Untreated fibre 10.6 68.5 3.8
Treated fibre 13.1 71.5 4.3

Based on Table 2.13, mechanical properties of hybrid kenaf/glass with and

without LENR are higher than neat epoxy. In addition, with the presence of LENR

both impact and flexural properties show an increment compare with hybrid

composite without LENR. The fibre treatment enhances the impact property which is

due to better interfacial adhesion between fibres and matrix. Presence of LENR plays

an important role as an impact modifier in the composite. Impact strength is depends

on many factors such as toughness of the reinforcement, frictional work for example

fibre pulling and nature of interfacial region. Furthermore voids, bubbles or any

impurities could affect the impact strength.

25
For flexural test, the plasticising effect of LENR increases the flexibility of

the composite and consequently more force was needed for debonding. This resulted

in high flexural strength value. Flexural modulus value of hybrid composites also

increase with the addition of LENR. This might be due to toughening effect of LENR

modification in the matrix which resulted in good energy absorbing capacity. In

addition, better mechanical performance of composite is resulted from cross linking

during the reaction which produced higher chain extensions.

33
Salleh et al. (2012) investigated water absorption test of hybrid kenaf/glass

reinforced unsaturated polyester resin under three different environmental conditions

which are rain water, distilled water and sea water.

From the result obtained, moisture content increases with immersion time.

After 3rd week, the highest moisture content of hybrid long kenaf/glass is the one that

immersed in rain water which is 10.95 wt% followed by distilled water 9.99 wt% and

sea water 9.01 wt%. Composite that was immersed in sea water show the lowest

weight gain due to presence of ionic salt in the sea water. This ionic salt blocks the

diffusion path after a long exposure and thus slowing down the absorption process.

34
Sathish et al. (2014) investigate the mechanical properties of hybrid banana-

kenaf/glass reinforced epoxy composite. They study the effect of varying fibre

orientation toward mechanical properties of hybrid composite. The fibre orientations

used in this research are vertical, horizontal, and 45° inclination. Stacking sequence

for the hybrid composite was glass/banana/kenaf/banana/glass. From the result

26
obtained, at 45° inclination of banana and kenaf fibre the hybrid composite shows

good mechanical performance.

For flexural test, hybrid composite score 24Mpa strength at 45° inclination

followed by vertical banana and horizontal kenaf orientation (40 banana/50 kenaf

fibre content) which is 21Mpa. The overall result is shown in Table 2.14. As can be

seen in Table 2.14, at higher kenaf fibre content, the flexural strength is higher. It is

probably because of kenaf possessed good strength than banana fibre.

Table 2.14 Result of flexural strength and energy absorbed at different fibre
orientation

Fibre orientation Fibre content (%) Flexural Energy


strength absorbed
banana kenaf banana kenaf (Mpa) (J)
Vertical Horizontal 50 50 19 14.6
Horizontal Vertical 45 55 21 12.90
45° 45° 40 60 24 15.81
Vertical Vertical 55 45 19 12.95
Horizontal Horizontal 60 40 18.5 13.25

For impact test, maximum energy absorbed of hybrid composite was at 45°

which is 15.81J. Combination of high kenaf content and glass fibre on top of the

specimen resulted in good strength and high energy absorption than other fibre

orientation.

35
Sharba et al. (2015) investigate the effect of varying fibre orientation on flexural

properties of hybrid kenaf/glass composite. Resin used in this research was

unsaturated polyester. They used three types of fibre orientation which are

unidirectional twisted yarn, non-woven random mat and plain woven kenaf.

27
They found out that flexural properties of hybrid kenaf/glass are depends on

fibre orientation. From the result obtained, woven kenaf hybrid composite scored the

highest flexural strength and modulus which approximately 295.0 MPa and 210.0

GPa respectively. Unidirectional kenaf hybrid scored the second highest followed by

non-woven kenaf hybrid composite.

They also stated that the flexural properties showed a non-linear behaviour

that can be divided into three stages. First stage was linear and gave modulus with

interruption at unidirectional fibre which is caused by single failure of single kenaf

fibre. Second stage is related to failure of kenaf fibre due to low elongation value.

This cause load fell to a specific value than rose up for a short period. At last stage,

the remaining glass fibre which started to carry load but could only do so for short

time that resulting in complete failure.

2.4 Fillers in composites

In the recent years, combination of polymer matrix with nano modified

polymer is increasingly in demand. Examples of nanofillers are nanoclays, carbon

nanotube, nanosilica, aerojel and so on. The purpose of adding nanofillers to

composite material is to improve material stiffnes, toughness, strength, thermal

properties and dimensional stability. Because of these advantages, nanofillers has

high potential for the improvement of mechanical properties of polymer matrix. 36

However, the properties of nanocomposite depend on several things such as

compatibility of nanofillers with polymer matrix, dispersion of nanofillers, and

interfacial bonding of nanofillers with polymer matrix. 37 38 The effect of having poor
28
dispersion of nanofillers is lead to premature failure of nanocomposite system. In

addition, having weak bonding between nanofillers and polymer matrix will cause

reduction in capability and stress transfer of nanocomposite.

Furthermore, combination of matrix-fillers will result in high interfacial area

which is due to uniform and homogenous dispersion of nanoparticles. The interfacial

area is responsible for changing relaxation behaviour, mechanical, molecular

mobility, and thermal properties.39 Some of the researches are as follow.

40
Sapiai et al. (2015) .In this study, the weight percentage of carbon nanotubes

(CNTs) is varied from 0.5wt-% to 1.0wt-%. The CNTs were added into epoxy resin

which is then used in the production in kenaf/glass hybrid composites. Based on

Figure 2.7, as the CNT content increase the flexural strength of composites

decreased. It is because of poor dispersion of CNTs in epoxy resin. It is believed that

poor dispersion of nanofillers cause poor mechanical strength.

Furthermore, as can be seen that the flexural modulus of kenaf/glass increase

with increasing of CNT content due to high stiffness of CNT which gives good

performance of composite material. Due to the entanglement of CNT tubes in the

matrix, it acts as stress concentration points that lead to composites failure. As a

result, the flexural strength will decrease.

29
Figure 2.7 Result of Flexural properties 40

Dimitrios et al. (2014).41 In this research, nanofillers used are silver, Ag, silica

(Si𝑂2 ), multi-walled carbon nanotube (MWCNTs) and graphene oxide (GO). This

study investigates the effect of size, shapes and geometries of nanofillers on

morphology of poly (butylenes succinate) (PBSu). Figure 2.8 shows the

microstructure of PBSu composite with different nanofillers.

PBSu with Si𝑂2 PBSu with Ag

30
PBSu with GO PBSu with MWCNT

Figure 2.8 Microstructure of PBSu under transmission electron microscopy 41

It clearly shown from Figure 2.8, Si𝑂2 and Ag show little agglomeration on

the composite while GO and MWCNTs have big agglomerates in the matrix. This

indicates that both Ag and Si𝑂2 are well dispersed in the matrix. Other factor of filler

dispersion is the shape. Spherical shapes of Ag and Si𝑂2 were dispersed more

uniformly in the matrix compared to nanosheets of GO and carbon nanotubes which

affect the crystallization behaviour.

Zhou et al. (2007) 42 reported mechanical properties of epoxy by filling with carbon

nanotube (CNT). The weight percent of carbon nanotube was varied from 0.1% to

0.4%. The result for flexural test is in Table 2.15. From Table 2.15, the flexural

modulus continued increasing as the weight percent of CNT increase. However, for

flexural strength, it showed decreasing of value at 0.4% CNT. The decrease in

strength is caused by two factors. Firstly, the dispersion of CNT filler is not uniform

in the epoxy at higher loading systems. Secondly, presence of voids in the system

also affected the flexural strength. More voids caused decreasing in strength.

31
Table 2.15 Flexural result with and without CNT filer

Sample Flexural properties


Modulus (Gpa) Strength (Mpa)
Neat epoxy 2.46 93.5
0.1% CNT 2.54 109
0.2% CNT 2.60 115
0.3% CNT 2.65 121
0.4% CNT 2.75 113

43
Teh et al. (2006) study the properties of epoxy resin coated with silica fillers

composite. The volume percent of silica was varied from 80% to 95% volume. The

result shows that flexural properties increase in the presence of silica compared to

neat epoxy. The flexural test result is I Table 2.16.

Table 2.16 Flexural result with and without silica filler


Sample Flexural properties
Strength (Mpa) Modulus (Gpa)
Neat epoxy 68.0 3.0
80% volume of silica 98.0 23.0
85% volume of silica 72.5 26.5
90% volume of silica 70.0 27.5
95% volume of silica 30.0 29.0

For flexural strength, the best value is at 80% volume of silica and increasing

of filler volume resulting in decreasing of strength. This is because, the epoxy is

insufficient to coat with the silica fillers at higher volume. Consequently, it resulted

in poor interfacial properties and presence of high void content which reduces the

flexural strength. Figure 2.9 shows the image under scanning electron microscope

(SEM) of 80% volume and 95% volume. It clearly showed in Figure 2.9 a)

homogenous dispersion of silica filler in the epoxy. At 95% volume in Figure 2.9 b),

the image shows the epoxy is insufficient to coat silica filler which gives weak filler-

matrix interfacial properties and voids.

32
(a) (b)
Figure 2.9 SEM images of epoxy coated with silica at (a) 80% vol. silica (b) 95%
vol. silica 43

44
Tay et al. (2012) reported effect of addition of montmorillonite filler of flexural

and impact properties of kenaf-polypropylene composites. They also investigate the

effect of using compatibilizer which is Epolene E-43P toward flexural and impact

properties. They used two ranges of kenaf sizes which are 250-500μm and 53-150μm

noted as 250μm and 53μm respectively. As expected, for flexural test combination of

compatibilizer E-43P with montmoriilonite (MMT) filler show higher results than

without E-43P.

Flexural strength of composite with E-43P show increasing in value. Kenaf

size of 53μm shows the highest strength than 250μm size and neat polypropylene. It

is because smaller filler size which is 53μm kenaf and MMT resulted in more

homogenous filler distribution. Consequently, it gives better stress distribution from

matrix to filler. For flexural modulus, composite with MMT and E-43P shows

increase in value.

For impact strength neat polypropylene (with and without E-43P) shows the

highest value than composite with MMT and E-43P. This is because, kenaf has non

uniform shapes and sizes which is unable to efficiently absorbing stress transferred

from matrix. When compare sample with kenaf/PP/MMT, sample with E-43P

33
resulted in higher impact strength. This indicates an enhanced in compatibility and

stress distribution in the composites.

45
Alsagayar et al. (2014) study the effect of montmorillonite (MMT) nanoclay filler

on flexural properties of its nanocomposite. They used epoxy resin as the matrix. The

MMT filler loading was varied starting from 0.5, 1.0, 1.5 and 2.0 phr. The result

stated that the optimum amount of MMT filler was at 1 phr. The flexural properties

of MMT/epoxy nanocomposite was slightly increased when the filler is add up until

1 phr. Further increase of filler resulted in reduction of mechanical properties. For

flexural test, flexural strength of MMT/epoxy nanocomposite increase from 0.5 to 1

phr. The maximum value of flexural strength is 110.35 Mpa.

Same goes to flexural modulus of the nanocomposite which scored 3186.85

Mpa at 1 phr. After 1 phr loading, the flexural strength and modulus decrease. This is

might due to incomplete dispersion of filler and presence of filler agglomeration. By

adding more filler in the epoxy matrix, the viscosity of the nanocomposite increased

and probably increases the creation of air-traps and micro voids. These defects can

lead to increase in stress concentration during test and led to early failure of the

specimens.

46
Glaskova et al (2009) investigate the effect of adding nanoclay filler on water

absorption of epoxy nanocomposite. They stated that epoxy resin has major

drawback of high moisture absorption which can degrades the functional, structural

and mechanical properties of the composites. They believed the addition of

nanoparticles can minimize the negative effects of water uptake such as reduces the

34
elastic characteristics of hydrophilic polymers. Lesser water uptake resulted in low

internal damage and may improve long-term performance of the nanocomposite.

From the result obtained, at high content of nanoclay it reduces at

approximately half of diffusivity than pure epoxy resin. Clay nanoparticles in the

nanocomposite act as efficient barrier against moisture transport. Consequently can

reduce the negative effect of moisture absorption.

47
Ozsoy et al. (2015) investigate the effect of micro and nanofiller size toward

mechanical properties of epoxy composite. The micro filler that they used are

aluminium oxide (𝐴𝑙2 𝑂3 ), titanium oxide (Ti𝑂2 ) and fly ash varied from 10% to 30%

weight ratio. While the nanofiller used are aluminium oxide (𝐴𝑙2 𝑂3 ), titanium oxide

(Ti𝑂2 ) and clay varied 2.5% to 10% weight ratio.

They stated that nano-filler size gives good mechanical properties than micro-

filler size. For both sizes, at higher filler content agglomerations occur and decrease

the properties of the composite. The flexural strength of nanocomposite increases up

to 5 %wt content and show decreasing in value above 5% content. The decrease in

strength is due to non-homogenous distribution of fillers at high filler content which

lead to agglomeration. For flexural modulus, it also show an increase up to certain

point because increase in filler content will increased the rigidity and stiffness

behaviour of the polymer.

35
48
Loos et al (2008) investigate the effect of short wall carbon nanotube (SWCNT)

addition on mechanical properties of epoxy matrix with the use of acetone to increase

diffusion of SWCNT in the solution and reduce resin viscosity. They stated that

small addition of nanotube in epoxy leads to slight structural changes. Flexural and

impact test was carried on in this research. From the result obtained, in 0.1%

SWCNTs addition the flexural properties show a bit decrease in value compared to

pure epoxy. But, flexural properties show an improvement at 0.25% SWCNT. From

other research, higher addition of CNT content lead to a decrease in flexural

properties. This is because from SEM analysis, nanotube is easily pulled out during

flexural testing due to poor bonding between nanotube and epoxy.

From impact test, it shows decrease in impact value for both 0.1% and 0.25%

SWCNT. This is due to nano-inclusion occurred when the epoxy become excessively

viscous and also poor interaction between nanotube and epoxy. The overall result is

in Table 2.17.

Table 2.17 Test results

Sample Flexural test


Impact strength (kJ/m²
Strength(Mpa) Modulus (Gpa)
Pure epoxy 76.8±3.3 3.0±0.2 2.2±0.2
0.1% SWCNT 76.2±3.1 2.9±0.2 1.6±0.2
0.25% SWCNT 80.1±4.6 3.0±0.2 1.6±0.1

Deepak et al. (2015) 49 study the influence of nanoclay in polyester resin reinforced

coir fibres. They compare coir composite with and without nanoclay. The nanoclay

used is fixed at 3%-wt. Impact test had been conducted and it is proven that energy

absorbed increase with the addition of nanoclay. The energy absorbed for coir

36
composite without nanoclay was 1.5J while coir composite with nanoclay was 2J. By

adding nanoclay, some reinforcement is added to the fibres. The storage modulus

increase in the composite is due to the reinforcement produce by the fibres which

allowed greater stress transfers at the interface. That is why energy absorbed increase

with the addition of nanoclay.

50
Karippal et al. (2011) had done the research on mechanical properties of

epoxy/glass/nanoclay hybrid composites. They varied the nanoclay filler from 1-wt%

to 6-wt%. From the result obtained the mechanical properties of hybrid composite

show an improvement up until 5-wt% and decreased at 6-wt%. Figure 2.10 shows the

graph of flexural strength and modulus. From the graph, the maximum performance

of hybrid composite is at 5-wt%. At 5-wt% there was a strong adhesion between

nanoclay-resin and the glass fibre which is stronger than at 2-wt% and 3-wt%. Well

dispersion of nanoclay filler also contribute to maximum performance of hybrid

composite. A decrease in flexural properties was shown at 6-wt% which because of

poor interaction between resin and nanoclay filler. Furthermore, there was also fibre

pull out of 6-wt% composite which is caused by high viscosity of resin that

contributed to the agglomeration of nanoclay. To conclude, the mechanical

properties of epoxy/glass/nanoclay hybrid is better than epoxy/glass composite.

37
Figure 2.10 Graph of Flexural result 50

51
Sivasaravanan and Bupesh Raja (2014) investigated the impact properties of

epoxy/glass fibre/nanoclay composite by varying the nanoclay percentage. They

varied nanoclay from 1-wt% to 5-wt%. The result showed the maximum impact

strength occurred at 5-wt% nanoclay. As the percentage of nanoclay increase the

impact strength also shows an increased. The average value of impact strength at 5-

wt% was 10.75J/m which is the best combination among others followed by 4-wt%

(10.05J/m), 3-wt% (9.58J/m), 2-wt% (10.20J/m) and 1-wt% (9.78J/m).

52
Kushwaha et al. (2014) compare the mechanical properties of bamboo fibre with

epoxy modified carbon nanotube (BECN) and treated bamboo fibre/epoxy composite

(BTEc). They investigate flexural properties, impact properties and water absorption

38
test. Generally, composite with carbon nanotube showed greater performance than

treated bamboo composite. For flexural test, the flexural strength for BECN and

BETc are 163Mpa and 154Mpa respectively. From the discussion, they found that

untreated bamboo has weak interfacial adhesion between matrix epoxy so that the

composite cannot withstand applied load transferred from the epoxy. From that, the

composite resulted in an inferior stiffness property. High flexural strength of BECN

resulted from good interfacial adhesion between bamboo and matrix.

For flexural modulus, BECN got 12420 Mpa while BETc got 9500 Mpa.

Factors that attribute to the higher moduli of BECN are good dispersion of CNT and

improved in interfacial bonding between CNT and epoxy.

For impact test, BECN has higher impact strength than BETc which is 84.5%

higher. This is due to better interlocking between fibres and matrix aided by CNT.

For water absorption test, for both composite, the weight gain decrease which is

because of good interfacial bonding within the composite.

53
Wulan et al (2014) investigated the effect of adding carbon nanotube (CNT)

towards mechanical properties of fruit bunch palm oil. The fruit bunch palm oil

contained cellulose fibre which is well-known natural fibre. From the result obtained,

addition of CNT affects the flexural properties of fibre of fruit bunch palm oil with

epoxy matrix composite. They varied CNT by weight percentage of 0.1, 0.5 and 1%.

The optimum performance of flexural properties of the composite was at 1%-wt. The

flexural strength of composite at 0.1, 0.5 and 1%-wt increased by 51.64%, 65.8% and

105.9% respectively. The increasing in value of strength is due to prevention of

39
cracks propagation by CNT that can lead to failure. Besides, due to nano size of

CNT, it can easily fill the gaps between matrix and fibre.

54
Islam et al (2015) studied the effect of fibre mixing and addition of clay toward

water uptake properties. They fabricate the sample at ratio 70:30 which is 70% resin

and 30% fibre. They differentiate their sample by vary fibre composition of wood to

coir fibre 0/30%, 30/0% and 15/15% with and without clay filler. The matrix used is

polypropylene (PP).

From water absorption test, composite of 0/30% (coir/PP) without MMT

shows the highest water uptake. This is due to numerous number of –OH groups that

present in the coir fibre. In addition in the 0/30% composite, there are increased in

micro-voids which enhance the amount of water uptake. For composite of 15/15%

(hybrid wood/coir/MMT), it has the highest rate of water absorption compared to

other combination. This is because, increasing in fibre in the composite resulted in

increased in hydrophilic nature of the hybrid nanocomposite and addition of MMT as

well. Hybrid composite (15/15%) without MMT has the lowest water uptake because

coir composition is decrease which also indicates the hydroxyl group is lesser and no

MMT addition.

Shen et al (2014) 55 investigate the effect of carbon nanotube addition toward flexural

properties of ramie/epoxy composite. They varied carbon nanotube content from 0.1-

wt% to 0.6-wt%. From the stress-strain curve, the failure strain increase at increasing

nanotube content up until 0.6-wt%. They mentioned that a further increased in

nantube content will not increase the failure strain due to stiffening effect of

nanotube. For flexural strength, ramie/epoxy composite is depends on compressive

40
strength of the composite which is as a function of modulus matrix. Basically, the

strength comes from ultra high strength and modulus of nanotube itself. Presence of

nanotube will strengthen and stiffened of fibre and the matrix thus makes it more

difficult for the composite to buckle.

41
CHAPTER 3

METHODOLOGY

3.1 Materials

The main materials used in this study were woven kenaf fibre with density of

1.44 g/cm³, E-600 glass fibre and epoxy resin with density of 1.1 g/cm³. For the

nanofillers, the fillers used are nanoclay and carbon nanotubes. The weight

percentage of nanofillers is varied from 1wt-%, 3wt-%, 5wt-%, and 7wt-%. Table

2.18 shows density of each material.

Figure 3.1 Material used

42
Table 2.18 Density of materials
Material Density (g/cm³)
Epoxy (100A:28.4B) 1.10
Slow hardener (103) 1.10
Kenaf (Bangladesh) 1.44
Glass (E-800) 2.50
Silicone filler 1.00
Carbon nanotube 2.10
Nanoclay 200-500 kg/m³ (bulk density)

Table 2.19 Sample notation


Notation Composition
NE Neat epoxy
ES Neat epoxy with silicone filler
S1 Kenaf/glass/epoxy
S2 Kenaf/glass/epoxy+1% nanoclay
S3 Kenaf/glass/epoxy+3% nanoclay
S4 Kenaf/glass/epoxy+5% nanoclay
S5 Kenaf/glass/epoxy+7% nanoclay
S6 Kenaf/glass/epoxy+1% carbon nanotube
S7 Kenaf/glass/epoxy+3% carbon nanotube
S8 Kenaf/glass/epoxy+5% carbon nanotube
S9 Kenaf/glass/epoxy+7% carbon nanotube

3.2 Specimen preparation

The specimens decided in this experiment are neat epoxy, kenaf/glass/epoxy,

and kenaf/glass/epoxy with nanofillers. Total specimens in this experiment are ten

specimens. The experimental steps are as follow.

a. Firstly, the woven kenaf and glass fibres are cut for 300x300mm dimension.

After that, the weight of the woven kenaf and glass fibres are measured. From

that weight, we can calculate the needed weight for resin based on decided

ratio. The example of calculation is in Appendix.

b. To get resin solution, the epoxy and hardener are mixed. Stir slowly until the

solution is fully mixed. Then nanofiller are added into the resin solution.

43
c. Next, wax is applied on the needed surface for specimen layup. Leave the

surface for approximately 5 minutes.

d. The first layer of glass fibre is placed on the wax surface. Resin solution is

applied on top of it. Make sure that the entire layer is fully applied with resin.

e. Then, the next 2 plies woven kenaf layer is placed on top of first layer. Step

(c) and (d) are repeated with the last layer of glass fibre. There are seven plies

to make one sample of kenaf/glass/epoxy composite.

f. After finish the layup process, a plate is placed on top of the sample. The

sample is then put into a 40 tonne compression molding with 5 minutes pre-

heat, 20 minutes full press and 3 minutes cold press.

g. Next, every sample is cut according to ASTM standard for flexural, impact

and water absorption test. Then these entire tests are conducted and the

morphological properties are observed.

h. Record all the data needed.

3.3 Flexural test

Flexural test is carried out according to ASTM D790 with sample dimension

of 127x12.7x3.2mm. Machine used to conduct flexural test is 5kN INSTRON 3365.

From flexural test, there are two mechanical properties are obtained which are

flexural modulus and flexural strength.

44
3.4 Impact test

Impact test is carried out according to ASTM 7136 with sample dimension of

150x100x3.2mm. Machine used to conduct impact test is Drop Weight machine

which is located at Makmal Struktur Aeroangkasa of Universiti Putra Malaysia.

From impact test, impact strength is evaluated for every sample.

Figure 3.2 Drop weight machine

3.5 Water Absorption Test

Water absorption test is carried out according to ASTM 570 with sample

dimension of 76x25x3.2mm. Before the test is conduct, original weight is measured

and recorded. Water uptake is calculated using formula below.


𝑤𝑓 − 𝑤0
× 100%
𝑤0

Where 𝑤𝑓 is the weight of sample after immersed in water for several time.

45
3.6 Morphology observation

Morphology test is a test that requiring sample observation using scanning

electron microscope at chemical lab of Universiti Putra Malaysia. The purpose of it

is to observe sample behaviour after carried out flexural test. Some criteria that need

to be observed are fibre pull-out, presence of filler agglomeration and dispersion of

filler in matrix.

Figure 3.3 Scanning Electron Microscope (S-3400N)

46
CHAPTER 4

RESULT

4.1 Flexural test

2000
1404.59
1726.69 1575.53
1800
1541.59
1600 1380.10 1496.42 1399.51
1275.97
Flexural strength (MPa)

1400

1200 1159.45
591.74
1000

800 558.40

600

400

200

0
E E-S S1 S2 S3 S4 S5 S6 S7 S8 S9
Sample

Figure 4.1 Effects of adding nanoclay or carbon nanotubes on the flexural strength of
kenaf/glass/epoxy composite

47
140
103.56 124.41
120 104.24
94.43 99.33

Flexural modulus (GPa)


100 81.36
77.26 80.88
80

60 52.09
32.73
40
15.58
20

0
E E-S S1 S2 S3 S4 S5 S6 S7 S8 S9
Sample

Figure 4.2 Effects of adding nanoclay or carbon nanotubes on the flexural modulus
of kenaf/glass/epoxy composite

Generally, all sample show an improvement of flexural properties compared

to neat epoxy. The optimum performance of flexural properties is at 3-wt% of

nanofiller. From Figure 4.1 the flexural strength increase up to 3-wt% filler and show

decreasing in value when further adding the filler content. Increasing in strength is

due to good interfacial adhesion between fibre and matrix (Kushwaha et al. 2014).

Furthermore, uniform dispersion of filler leads to good flexural strength. Above 3-

wt% filler, flexural strength decrease because of insufficient of epoxy to coat with

filler that resulted in poor interfacial properties (Teh et al. 2006).

Figure 4.2 shows the flexural modulus that gives same trend as flexural

strength. Increase in filler content will increase the rigidity and stiffness of the

polymer (Ozsoy et al 2015) and resulted in improved modulus up to certain point.

For nanoclay sample which is from S2 to S5, sample S3 showed the highest flexural

strength and modulus that is 1726.69MPa and 124.41GPa respectively. S3 gives 23%

48
and 20% improvement of strength and modulus respectively when compared to S1.

In addition, S3 show great performance compared to S7. S7 gives 1575.53MPa of

strength and 99.33GPa modulus. This can be proven by SEM observation in Figure

4.3 and Figure 4.4. Figure 4.3 shows good adhesion between fibre and matrix (with

clay) while Figure 4.4 shows poor adhesion. Furthermore, as can be seen in Figure

4.3 there is also clay agglomeration in the matrix but not significant.

When compared to carbon nanotube filler, nanoclay filler is treated clay.

Treated clay gives better interfacial adhesion with the matrix which resulted in good

flexural properties than carbon nanotube. Moreover, carbon nanotube is untreated

type which gives poor interfacial.

Figure 4.3 SEM image of S3 (3-wt% nanoclay)

Figure 4.4 SEM image of S3 (3-wt% carbon nanotube)

49
For flexural strain, S4 and S8 show the highest strain which is 5-wt% of

nanoclay and carbon nanotube respectively. By increasing the filler content, the

flexural strain will increase up to certain limit. This is due to stiffening effect of the

filler itself (Ozsoy et al 2015). As can be seen in Figure 4.5, the epoxy modified

silicone sample show an improvement than neat epoxy. The cross-linked silicone

core gives an additional strength to the matrix and stiffens the matrix. Figure 4.5

shows the result of flexural strain.

25

17.17
20
Flexural Strain (%)

15
11.93
10.07 8.27
9.4 8.17
9.0
10
6.67 6.53
5.3 5.5
5

0
E E-S S1 S2 S3 S4 S5 S6 S7 S8 S9
Sample

Figure 4.5 Effects of adding nanoclay or carbon nanotubes on the flexural strain of
kenaf/glass/epoxy composite

50
4.2 Impact test

20
18 17.06 15.92
15.89 15.96
16 14.76
13.41 13.91 13.08
14
Energy Absorption (J)

12.36
12
9.54
10
8
6
4
0.92
2
0
-2 E E-S S1 S2 S3 S4 S5 S6 S7 S8 S9
Sample

Figure 4.6 Effects of adding nanoclay or carbon nanotubes on the energy absorption
of kenaf/glass/epoxy composite

From Figure 4.6 the optimum performance of energy absorption value is at 3-

wt% filler. 3-wt% nanoclay composite (S3) exhibit the highest energy absorption

than 3-wt% carbon nanotube composite. When compared to S1, S3 gives 7%

improvement of energy absorption while S7 gives 12% lesser energy absorption than

S1. At filler content above 3-wt% energy absorption decrease which is because of

nano-inclusion occurred when epoxy become excessively viscous (Loos et al 2008).

To compare neat epoxy and modified epoxy-silicone (ES), the ES composite

gives significant higher energy absorption than neat epoxy. This is due to the high

brittleness of epoxy than ES composite that resulted in low energy absorption. With

the addition of silicone to the matrix epoxy, some reinforcement is added to the resin

system. The silicone filler act as a good binder between matrix and matrix bonding

which gives higher energy absorption.

51
Table 2.20 shows the overall damage area for sample S1 to S9. As can be

seen, the variation of damage area for nanoclay sample show different trend from

carbon nanotube sample.

Table 2.20 Result of Impacted Damage area


Damage area Damage area (mm²) Damage area (mm²)

(mm²) for S1 Nanoclay sample Carbon nanotube sample

S2 1455 S6 390

611 S3 402 S7 804

S4 367 S8 419

S5 953 S9 297

Due to properties of nanoclay filler, it is surface modified filler which gives

better matrix to fibre adhesion. At 3-wt% nanoclay, S3 gives highest energy

absorption and small damage area. It is different for carbon nanotube sample where

the highest energy absorption which is S7 but has bigger damage area. This is

because carbon nanotube filler used in this project is not modified and gives low

performance and poor adhesion. Mixing of untreated nanofiller without a

compatibilizer, can lead to a bad dispersion and lead to filler agglomeration which

decrease the strength of the interphase region (Zoukrami et al 2008)56.

As stated by previous research, bigger damage area indicates that the


57
composite has higher energy absorption and energy dispersion (Hawa et al 2015 ,

Ye L. et al 2004 58). But at the addition of filler in composite the energy dispersion or

absorption is depend on properties of nanofiller.

Furthermore, as mention before the filler gives an additional reinforcement to

the fibre itself. This reinforcement gives higher storage modulus that allows greater

52
transfer of stress at between fibre and matrix (Deepak et al 2015). The energy

absorption of S3 and S7 are higher with interlocking structure of woven kenaf and

glass fibre that require more energy to break the coupling between the fibre bundles.

4.3 Water absorption test

water absorption of nanoclay


20
18
16
14
water uptake (%)

12 S1
10 S2
8 S3
6 S4
4 S5
2
0
0 10 20 30 40 50
Day

Figure 4.7 Water absorption result of kenaf/glass/epoxy composite filled with


nanoclay

53
water absorption of CNT filler
12

water uptake (%) 10

8
S6
6 S7
S8
4
S9
2 S1

0
0 10 20 30 40 50
Day

Figure 4.8 Water absorption result of kenaf/glass/epoxy composite filled with carbon
nanotube

Based on Figure 4.7 there was a rapid water uptake at the first three days. For

sample with nanoclay, S4 gives the highest water uptake which is 9% more at the

compared to S1 followed by S3, S2 and S5. As can be seen in Figure 4.8 which is

sample with carbon nanotube filler, S8 gives the highest water uptake among sample

with nanotube filler but, S8 show lesser water uptake compared to S1 which is 1.0%

less. Highest water uptake of sample with nanoclay is might related increase in

hydrophilic nature in the hybrid nanocomposite due to addition of nanoclay (Islam et

al. 2015). Increase in hydrophilic nature will increase the water uptake.

In addition, all samples shows higher water uptake compared to neat epoxy

and modified epoxy-silicone. This is because sample S1 to S9 contain fibre which

also increase the hydrophilic nature that contribute to more water uptake. Besides, as

can be seen in Figure 4.9 that modified epoxy-silicone gives a bit higher water

54
uptake compared to neat epoxy. From the Figure 4.9 at the first three days, modified

epoxy-silicone absorbs water 0.3% more compared to neat epoxy.

water absorption of neat epoxy and epoxy


modified silicone
1.4
1.2
1
Water uptake, %

0.8
E-S
0.6
E
0.4
0.2
0
-0.2 0 5 10 15 20 25 30
Day

Figure 4.9 Water absorption results of E and E-S composite

When compared all hybrid kenaf/glass composite, sample with nanoclay and

carbon nanotube filler show lower water uptake than S1. This is because addition of

filler can minimize water uptake by reducing hydrophilic characteristic of polymer

(Glaskova et al. 2009).

As a conclusion, presence of fibre in composite will increase the hydrophilic

nature and increase water uptake. An agglomeration of filler and presence of voids

will also lead to high water uptake. An illustration of presence of filler agglomeration

and voids is as in Figure 5.0.

55
CHAPTER 5

CONCLUSIONS AND RECOMMENDATIONS

For this study, flexural and impact properties were the main concerns with water

absorption behaviour as a test to identify which sample gives highest water uptake. For

flexural test, S3 gives the highest flexural strength and flexural modulus. The reason of

highest strength is due to good interfacial adhesion between fibre and matrix. Another

possible reason that leads to good flexural strength is well dispersion of filler in the matrix.

Besides, factor that contributes in good flexural modulus is increase in rigidity and stiffness

of the polymer which is due to the presence of filler. After flexural test, a morphology

observation is done under scanning electron microscope. The purpose of morphology

observation is to study the surface of the composite and identify possible factors of flexural

performance. Sample S3 and S7 were chosen to be investigated under SEM. It is proven that

S3 gives good interfacial adhesion between fibre and matrix while S7 gives poor adhesion.

As mentioned in the discussion part, carbon nanotube is not treated filler and it gives poor

adhesion between fibre and matrix. More images of SEM result are attached in Appendix B.

For impact test, S3 and S7 gives high energy absorption compared to other samples.

The presence of filler in the compoite gives an additional strength that gives higher storage

modulus that allows greater transfer of stress at between fibre and matrix which

resulted in high energy absorption. Furthermore, after impact test is done a non-destructive

test which is dye penetrant test is conducted. The purpose of it is to allow dye to penetrate

the impacted surface for clear observation of damage area. As for damage area, generally if

56
the damage area is bigger there is more energy is being dispersed. But in the inclusion of

filler it restricted the crack propagation and resulted in small area. The pictures of all impact

samples after dye penetrant test are attached in Appendix C.

For water absorption test, it is conducted until all samples show constant weight. At

the first 10 days all samples shows rapid water uptake. After several days, S4 gives the

highest water uptake compared to S1 and other nanoclay sample. While for carbon nanotube

samples, S8 gives the highest water uptake. The addition of nanofiller could minimize water

uptake and decrease hydrophilic nature. But S4 and S8 with 5-wt% nanoclay and 5-wt%

carbon nanotube respectively gives highest water uptake which is due to present of voids and

error in fabrication.

RECOMMENDATIONS

Non-uniform dispersion of filler will lead agglomeration of filler which

decrease mechanical properties and high water uptake. To enhance dispersion of

filler, during mixing process student should put the filler in the resin solution evenly

using a filter and avoid put the filler all at once. The reason of using filter is to avoid

foreign objects from entering the resin solution. Furthermore, student can increase

the speed of the homogenizer to enhance filler dispersion.

During hand layup process, student should not delay too much time because

as the hardener is mix with the resin, the curing process occurred rapidly and lead to

agglomeration. In addition, while using compression molding, the machine

sometimes could not function well. If full press did not occurred the sample will

resulted in increase in thickness which affected the water absorption test later on.

57
Student should repeat the sample to avoid high error in test results and inconsistent in

reading.

As for impact test, after conducting one impact sample student should left the

drop weight machine for about 7 minutes before continue for other samples. This is a

precaution to avoid instrument error. After one impact sample the machine still has

residual effect and to avoid this residual effect affect the result for next sample,

student should left the machine for rest.

58
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