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1.0 PROJECT TITLE

Preparation and Characterisation of Hybrid Vacuum Assisted Resin Transfer Molding (VARTM) Kenaf

Bast Glass Fiber Unsaturated Polyester Composite

2.0 OBJECTIVES

Generally, the aim of this research is to increase the utilisation of natural fibers and to reduce the use of

synthetic fibers in composites manufacturing.

3.0 LITERATURE REVIEW

Composites are the essential part of today’s materials due to their admirable properties such as

lightweight, high strength, corrosion, moisture and chemical resistance and faster assembly. They are

substantially used as materials in producing aircraft structures, automotive applications, electronics

packaging, home building and many more.

In fiber-reinforced polymer (FRP) composites fabrication, the materials that are commonly used

are reinforcement fiber and polymer matrix. The most popular reinforcement for FRP composites are

glass, carbon, basalt and aramid fibers. The polymers are epoxy, polyester, phenol formaldehyde resins,

vinyl ester, polyamide and many more [5]. FRP composites are said to be very attractive due to their

high strength-to-weight as well as stiffness-to-weight ratios [34].

Glass fibers are the material consisting of copious extremely fine fibers of glass based on silica

with additions of oxides of calcium, boron, sodium, iron and aluminum [13]. The major advantages of

glass fibers are low cost, high tensile strength, high chemical resistance, and excellent insulating

properties [22]. The properties such as tensile, flexural and impact strength of glass fibers reinforced

composites are said to be higher compared to natural fibers reinforced composites [16,17,37]. They are

also possessing good anti-aging properties compared to mineral and natural fibers reinforced

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composites [27]. Furthermore, the elastic modulus of glass fibers shows that they are greater than

natural fibers but lower than carbon fibers [38]. However, these fibers have several drawbacks

compared to natural fibers such as higher density, non-renewability, non-recyclability, higher energy

consumption, harmful to health when inhaled and non-biodegradable [37]. Thus, over the last few years

natural fibers have gained significant attention as viable alternative for FRP composites.

Natural fibers are cellulose fiber reinforced materials as they consist of microfibrils in an

amorphous matrix of lignin and hemicelluloses [29]. Most commonly used natural fibers for polymer

composites are jute, flax, sisal, wood, oil palm, kenaf, bamboo, and etc. These natural fibers offer

renewability, biodegradability, abundance, cost-saving and low specific gravity when compared to

synthetic fibers such as glass and carbon fibers [24]. Moreover, they are also non toxicity, nonabrasive,

combustible, harmless to health and enhanced energy recovery [24,19,25].

One of the natural fibers that are currently gaining attention in FRP composites industries is

kenaf (Hibiscus cannabinus L) bast fiber. According to Malaysian Agricultural Research and Development

Institute (MARDI), kenaf fiber reinforced composites has a tremendous potential and market, estimated

at RM3 billion [6]. Kenaf bast has high potential as reinforcing fibers in FRP composites because of its

superior toughness and high aspect ratio [19]. In comparison with other natural fibers namely cotton,

sisal, jute, flax, sunhemp and pineapple, kenaf bast have showed the highest tensile strength along with

elastic modulus and specific elastic modulus as high as jute [12,29]. Many studies have been done in

order to improve the properties of kenaf bast reinforced composites especially in enhancing the

compatibility between the fibers and matrices. Based on the report, maleic anhydride treated kenaf dust

composites have shown better tensile properties in comparison to those untreated one [7]. This is as a

result of esterification where the hydroxyl group of kenaf reacted with the anhydride group of maleic

anhydride to form an ester linkage [21]. Interfacial adhesion between the fibers and matrix also can be

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enhanced through grafting. This method improves the wettability of the fiber with matrix by

hydrophobized the fiber surface and urges interfacial bonding [2].

Unsaturated polyester resin containing long chain fatty acids and styrene as cross-linking agent

and generally are prepared from dihydric alcohols and dicarboxylic acids [10]. It is a thermoset matrix

that is often used in fiber-reinforced composites production because it is easily handled or processed

and cured, low-cost, accessible and has good mechanical properties when reinforced. It is suitable for

use in various applications and can be adopted in large-scale manufacturing [4]. Curing process of

unsaturated polyester can be done through three methods: heating, at room temperature and radiation.

The properties of cured unsaturated polyester is influenced by the type and ratio of acid and glycol,

molecular weight distribution, type of end-group, the distribution of repeated units and non-saturation

[1].

Hybrid composites consist of two or more different types of fiber in a common resin matrix. The

potential advantages of such materials have been reported since 1970’s where the interest on that time

was glass fiber/carbon fiber hybrid [11,40,23]. In recent years, studies on hybrid composites are

increasingly carried out by researchers with the interest in hybridizing different types of fibers with

various types of polymers. There are reports on natural fiber/natural fiber hybrid reinforced composites

system [36,14,3]. From the reports, it can be concluded that the tensile strength of natural fiber/natural

fiber hybrid reinforced composites is reduced with further loading of fibers but the modulus is

increased. Therefore, in order to improve the mechanical properties, natural fiber/synthetic fiber hybrid

reinforced composites especially by using glass fiber have become the new area of interest with several

studies reporting this system [26,15,35]. However, until now there has not been a study on kenaf

bast/glass fiber reinforced composites system. Therefore, owing to the importance of reduction of

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production costs and environmental awareness, a systematic study on kenaf bast/glass fiber hybrid

reinforced composites using unsaturated polyester as a matrix polymer will be carried out.

4.0 OBJECTIVES OF THE STUDY

i. To study the potential and compatibility of kenaf/glass fiber mat reinforcement in

unsaturated polyester composite.

ii. To examine the effect of different chemical modification of kenaf bast fiber on kenaf/glass

fiber/unsaturated polyester composite properties.

iii. To determine different modified and unmodified kenaf/glass fiber mat loading on

mechanical properties of kenaf/glass fiber/unsaturated polyester composite.

iv. To characterize the properties of treated and untreated kenaf/glass fiber/unsaturated

polyester composite.

v. To investigate the effect of different chemical modification on crosslink density of

kenaf/glass fiber/unsaturated polyester composite.

5.0 METHODOLOGY

5.1 Materials

Kenaf bast fiber, glass fiber, unsaturated polyester resin, maleic anhydride (MA), glycidyl methacrylate

(GMA), ethanol, dimethylformamide (DMF), triethylamine, hydroquinone, phthalic anhydride, sodium

hydroxide (NaOH), pyridine, acetone, toluene

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5.2 Preparation of Kenaf Bast Fiber

Prior to composites fabrication, kenaf bast fiber will be oven dried for 24 hours before being treated

with MA and GMA. This is to get the initial weight before the fiber is reacted. For untreated kenaf bast

fiber, it will be used directly after the drying process.

5.3 Chemical Modification of Kenaf Bast Fiber

Maleic anhydride (MA) and glycidyl methacrylate (GMA) will be used to treat the kenaf bast fiber and

the effect of these different modifications will be studied through characterisation and mechanical

properties of the composites.

5.3.1 Maleic Anhydride (MA) Modification on Kenaf Bast Fiber

For surface treatment of the fiber, MA is dissolved in DMF with the volume ratio of 3:7. 5% of

hydroquinone is then added based on MA weight as an inhibitor. Dried kenaf bast fiber is added to the

MA solution and heated at 90°C. The reaction will be conducted for 1 hour with constant stirring. The

treated kenaf bast fiber is then filtered and rinsed with acetone to remove the unreacted MA before

being refluxed with acetone for 3 hours. The fiber is then dried in an oven. The weight percentage gain

(WPG) of treated kenaf bast fiber will be calculated using a following formula:

( )

where, is the weight of fiber before MA treatment and is the weight of fiber after MA treatment.

5.3.2 Glycidyl Methacrylate (GMA) Modification on Kenaf Bast Fiber

GMA is dissolved in DMF with triethylamine as a catalyst. Hydroquinone is then added to minimize the

risk of free radical reaction at the unsaturated ends of GMA [28]. The reaction will be carried out for 2

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hours at 90°C. After reaction, the treated fiber is filtered to eliminate the reagent before being rinsed

with acetone. The fiber is then refluxed with fresh acetone for 2 hours to make sure the unreacted

reagent is removed. Later, the kenaf bast fiber is oven dried before being weighted to determine the

WPG percentage as above.

5.4 Mat Forming of Kenaf Bast Fiber

Untreated and treated kenaf bast fiber will be formed into mat by using carding and needle punching

technique. Kenaf bast fiber is mixed, combed and mechanically entangled using a carding machine.

Then, the carded fiber is fed into the needle-punching machine to form it into unidirectional fiber mat

with different thickness that is 5mm, 10mm and 15mm.

5.5 Preparation of Hybrid Kenaf Bast/Glass Fiber Unsaturated Polyester Composites

Kenaf bast fiber in a form of mat and woven glass fiber will be cut with the dimension of 250 × 400mm.

Woven glass fiber and kenaf bast fiber is then stacked like a sandwich and placed on a mold to form the

preform. The entire lay-up is assembled in accordance to figure 1 [30].

Figure 1

Before infusion, unsaturated polyester resin is degassed under vacuum to reduce the air content

in the resin. After degassing, ambient pressure is then applied to force the resin to move into clamped

inlet tube. At the time of unclamping of the inlet tube, the resin will flow through distribution media and

impregnated the preform. After the resin has reached the end of preform, pressure at the inlet and vent

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will be applied and the condition is maintained until the resin is cured at room temperature for 24

hours. This technique is repeated for all untreated and treated kenaf bast fiber with different fiber

thickness and glass fiber loading.

5.6 Characterisation of Hybrid Kenaf Bast/Glass Fiber Unsaturated Polyester Composites

Products that have been produced will undergo a series of tests to determine its characteristic. It will be

preceded by fourier transform infrared (FTIR) spectroscopy analysis to identify the presence of the

functional groups in a molecule, to confirm the identity of a pure compound or to detect the presence of

specific impurities [20]. This method is also use to evaluate the modification degree on the fiber [8].

Data will be obtained in the form of spectrum which will then be analyzed to determine the compounds

in the mixture. Scanning Electron Microscopy (SEM) analysis is conducted to determine the details of the

fiber surface, fiber-matrix interaction and cracks within the composites [9]. Data will be shown in the

form of high-resolution images with details less than 1nm in size. To determine the thermal stability of

the products, thermal gravimetric analysis (TGA) is carried out and weight loss occurring or degradation

of fiber will be observed as a function of constant increasing temperature [18]. The result will be

presented as a TGA curve. In order to understand the crystallizing behavior and to identify the chemical

activity occurring in the composite, a differential scanning calorimeter (DSC) will be measured and result

will be displayed in the DSC curve. Determination of the hydroxyl (OH) content of kenaf bast fiber

involves esterification of OH group by phthalic anhydride in pyridine and titration of sodium hydroxide

(NaOH). OH number and OH content are then calculated as the following equations:

( ) ( ) ( )

( )

( ) ( )

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Gel content of the composite is determined using Soxhlet extraction with xylene [32]. The gel content is

calculated as the ratio of the weight of dried sample after extraction ( ) to the weight of the sample

before extraction ( ) as below [31]:

Water absorption test is conducted according to ASTM D5229/D5229M-14. The water absorption is

calculated by the weight difference as [33]:

( )

where is the initial weight and is the weight of the swollen sample.

5.6.1 Determination of Crosslink Density

The crosslink density of the hybrid composites is determined by equilibrium solvent-swelling

measurement. The samples will be immersed in toluene for 72 hours. The swollen samples will be

removed and dried [33]. Crosslink density (v) is determined using Flory-Rehner’s equation *39]:

( )

(

)

where is the molar volume of solvent, is the volume fraction of polymer in the mixture, is the

polymer-solvent interaction parameter. , can be obtained by following equation [39]:

⁄

⁄

⁄

and can be obtained by equation [39]:

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( )

where and are the solubility parameters of polymer and solvent, respectively. R is the universal

gas constant and T is the absolute temperature.

5.7 Mechanical Properties of Hybrid Kenaf Bast/Glass Fiber Unsaturated Polyester Composites

In order to determine the mechanical properties of the hybrid composites, several types of tests will be

performed based on ASTM standards (see table 1 for specific standards). The first test to be performed

is tensile test which to evaluate the ability of the material to withstand forces that tend to pull it apart.

Tensile properties to be acquired are tensile strength, elongation at break and tensile modulus. Next,

the hybrid composite will be tested with the flexural test where it evaluates the ability of material to

withstand the forces applied in the perpendicular direction (90°). The test will be conducted by using

Instron Universal Testing machine and flexural strength as well as flexural modulus will be calculated.

Impact tests will be performed in accordance to Izod impact resistance test method by using Zwick

Pendulum Impact. The load used to test the impact resistance is in unit of Joules. The durability strength

of the hybrid composite will be tested using tensile cyclic test method. It will be carried out using Instron

Universal Testing machine under a load-controlled at ambient temperature. Tension-tension cyclic load

is applied and fatigue resistance of the sample will be examined.

Table 1: Standard used for samples testing

Types of Testing Standards

Tensile test ASTM D3039/D3039M-14

Flexural test ASTM D7264/D7264M-07

Impact test ASTM D256-10

Durability test ASTM D3479/D3479M-12

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The whole research progress can be visualized in a flow chart as shown below in figure 2.

Figure 2

6.0 RESEARCH HYPOTHESIS

This research is covering on hybrid kenaf bast/glass fiber preparation and characterization with different

chemical modification and fiber loading. It is expected that the composite produced from this method

will possesses high mechanical properties and suitable for heavy duty application mainly as a man-hole

cover, septic tank, water tank, automobile parts and as reinforcement in concrete.

Preparation of kenaf bast fiber

- untreated

- maleic anhydride (MA) treatment

- glycidyl methacrylate (GMA) treatment

Mat forming of kenaf bast fiber

- carding and needle punching technique

- different fiber mat thickness

VARTM technique

Preparation of kenaf bast fiber-reinforced unsaturated polyester composite with 1 layer of glass fiber - with different kenaf bast fiber loading

Preparation of kenaf bast fiber-reinforced unsaturated polyester composite with 2 layers of glass fiber - with different kenaf bast fiber loading

Preparation of kenaf bast fiber-reinforced unsaturated polyester composite without glass fiber - with different kenaf bast fiber loading

Characterisation

-OH Number -FTIR

-SEM -TGA

-DSC -Gel content

-Crosslink density -Water absorption

Mechanical testing

-Tensile test -Flexural test -Impact test -Durability test

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7.0 EQUIMENTS USED

i. Instron Universal Testing Machine

ii. Fourier Transform Infrared (FTIR)

iii. Scanning Electron Microscopy (SEM)

iv. Thermogravimetric (TGA)

v. Differential Scanning Calorimeter (DSC)

vi. Zwick Pendulum Impact

8.0 GANTT CHART (refer to Appendix)

9.0 EXPECTED OUTCOMES

i. Producing hybrid kenaf bast/glass fiber reinforced unsaturated polyester composites by

using vacuum assisted resin transfer molding (VARTM) technique with different chemical

modification and fiber mat loading.

ii. Understanding the compatibility, characteristics and mechanical properties of hybrid kenaf

bast/glass fiber reinforced unsaturated polyester composites.

iii. Publishing at least three research papers in ISI indexed conference journals on the

characteristics, mechanical properties and crosslink density of hybrid kenaf bast/glass fiber

reinforced unsaturated polyester composites.

10.0 CONTRIBUTION OF RESEARCH OUTCOME TOWARDS THE COUNTRY

This study is expected to benefit various parties in Malaysia from kenaf planters, manufacturers,

suppliers, consumers to Malaysia government statutory bodies such as MARDI and National Kenaf and

Tobacco Board (LKTN).

The production of this product is expected to be substantial because the materials and method

used is suitable for large-scale manufacturing. The demand for kenaf fiber will be increased and it will

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improve the livelihood of kenaf planters. Furthermore, kenaf is an herbaceous plant that can be grown

under a wide range of weather conditions and can be harvested within three to four months. Hence, it

will not only benefit planters in certain parts of Malaysia but all with quick income returns. As for

suppliers and manufacturers, this product will benefit them through high profit income because this

natural fiber is cheap and abundance. The mobility to transport the raw materials is also economical

because the fiber is low weight and requires minimum men power for handling. The manufacturing

process is easier and safe as kenaf fiber is harmless to workers and non-abrasive on tooling and

machinery. Therefore, consumers will enjoy end products which are high in quality but low-priced. Apart

from environmental and economic contribution to the nation, the methodology applied in this research

can be used as technical guidelines for MARDI, LKTN, local research institutions or manufacturer to

implement hybrid FRP composites. Moreover, the research report is expected to be a reference for

future research and product improvement.

11.0 CONCLUSION

Hybrid VARTM kenaf bast/glass fiber reinforced unsaturated polyester composite is a new field of

research that has never been studied before. There will be a lot of new findings that can be generated

throughout this research. The different types of chemical modification on kenaf bast fiber will determine

the most compatible fibers with resin. The morphological studies will reveal the characteristics of the

product which will give ideas for the future improvement. Result of mechanical and physical strength

collected from this research can be used as a guideline or references for further researches in the

future. Moreover, methods used throughout the research are suitable for large-scale production and

can be used by manufacturer for mass production. In addition, it is hoped that the resulting product will

be able to replace the existing conventional products where it is more environmentally friendly, cost

effective and lightweight.

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APPENDIX

8.0 GANTT CHART

Activities

2014 2015 2016 2017

Ap

r M

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Jun

Ju

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Sep

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Oct

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Literature review

Preparation of materials

Preparation of untreated kenaf bast fiber/glass fiber composite

Preparation of MA treated kenaf bast fiber/glass fiber composite

Preparation of GMA treated kenaf bast fiber/glass fiber composite

Characterization

Mechanical properties testing

Conferences and publications

Report writing