CHAPTER 1

INTRODUCTION

1.1 Background and problem statement

Nanotechnology research is entirely multidisciplinary and the results of such research can

be applied very quickly to real products. Nanomaterials are of great scientific and

technological interest because of their potential to exhibit new characteristics that cannot

be achieved with micromaterials (Pereira de Abreu et al., 2007). Now, at nanoscale one

enters a world where physics and chemistry meet and develop novel properties of matter.

In chemistry, this range of sizes has historically been associated with colloids, micelles,

polymer molecules, phase-separated regions of block copolymers and similar structures.

More recently, structures such as bucky tubes, silicon nanorods, and compound

semiconductor quantum dots have emerged as particularly interesting classes of

nanostructures. In physics and electrical engineering, nanoscience is most often

associated with quantum behavior, and the behavior of electrons and photons in

nanoscale structures. Biology and biochemistry also have a deep interest in

nanostructures as components of the cell; many of the most interesting structures in

biology – from DNA and viruses to sub-cellular organelles and gap junctions can be

considered as nanostructures (Namrata Singh Tomer et al., 2009).

In material technology, nanomaterial is the most important part to develop the structure

of material that can adapt under different environmental conditions. Organic nanocrystal

can be synthetic or natural. Synthetic organic nanocrystal may include perylene and

1
 anthracene. Natural organic nanocrystal include cellulose, starch etc. due to sustainable

factors, natural nanocrystal are preferred nowadays as it can be grown as continuous

supplies and easily available.

The existing challenge in the polymer fabrication is to provide a sufficiently high tensile

strength due to local stress within the nanomaterial. In other words, the response of a

material to an applied stress is strongly dependent on the nature of the bonds. The

interfacial interactions between nanoparticles and polymer–matrix play a crucial role in

the local stress transfer and determining the quality and properties of the nanomaterial

(Zhanhu Guo et al., 2007).

In addition, synthetic polymeric materials are rapidly replacing more traditional inorganic

materials, such as metals and natural polymeric materials (wood, fibers). As these

synthetic materials are flammable, they require modifications to decrease their

flammability through the addition of flame-retardant compounds. Environmental

regulations have restricted the use of some halogenated flame-retardant additives,

initiated a search for alternative flame-retardant additives. For this purpose, inorganic

nanoparticles have become attractive since they can simultaneously improve the physical,

mechanical and flammability properties. Thus, polymer–nanocomposites, in last few

decades, have become worldwide research interest for developing polymeric materials

with improved/desired properties by incorporation of these nanoscale materials into

polymer matrix (Annamalai Pratheep Kumar et al., 2009).

1.2 Significant of study

2
Organic and polymer nanocrystals, ranging in size from tens of nanometers to several

hundred nanometers, represent an intermediate phase between single molecules and the

corresponding bulk crystal. In very few systems, the nanoparticulates have been

incorporated into polymer as ‘nano-additives’ for both purposes: degradation and

stabilization of polymers. The degradation and durability of polymers is reviewed in the

presence of nanoparticles /nanocomposites under different environmental conditions

(Annamalai Pratheep Kumar et al., 2009).

A trend has been towards incorporating natural fibers into composites. This shift has been

prompted mainly due to various environmental, economic and performance issues.

Natural fillers offer a cost effective and renewable alternative to their synthetic

counterparts, without compromising performance. Cellulose-based plant fibers obtained

from cotton, flax, hemp, jute, sisal, kenaf and coir have been incorporated into polymer

composites. Other sources of cellulosic fillers include wood flour/fibers, recycled fiber-

based products like newspaper and strengthened interface agricultural residues such as

rice husks and sugarcane bagasse. These natural fibers provide several benefits over

synthetic fibers. Cellulose fibers are non-toxic, biodegradable and recyclable. Natural

plant fibers are generally of lower density and exhibit high specific strength and stiffness

that allow the production of low-density composites with higher filler concentration.

Composites made from cellulosic fibers and thermoplastic matrices have generated

interest because they promise lower environmental impact when compared with more

traditional composites based on synthetic fibers. Furthermore, the theoretical mechanical

properties of cellulose-reinforced composites are impressive because of the strength and

stiffness of crystalline cellulose (Benoît J.C et al., 2009).

3
 Additionally, natural fibers have flexibility and are therefore less susceptible to fracture

during processing, resulting in these fibers maintaining their specific aspect ratio.

Polypropylene (PP) is one of the most important and widely used polyolefin. Its low

density, low production costs, design flexibility and recyclability make it a popular

choice as matrix material. PP is hydrophobic, leading to compatibility issues when fillers

with polar surfaces, such as cellulose, are used (Steven Spoljaric et al., 2009).

1.3 Objectives of study

The intention of this research is to investigate the effect of incorporating organic

nanocrystal specifically cellulose microcrystal and nanocrystal into polyethylene and

polypropylene on its mechanical and thermal properties.

The specific objectives of the project include to:

1. To compound Polyethylene and Polypropylene with microcrystalline cellulose and

Nanocrystal using twin screw.

2. To fabricate resin into film using film blowing technique.

3. To test the melt flow, strength and thermal properties of the sample.

CHAPTER 2

LITERATURE REVIEW

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2.1 Organic nanocrystals

2.1.1 Perylene and anthracene

These organic nanocrystals were fabricated to investigate the effect of solvent on organic

nanocrystal growth using the reprecipitation method. Perylene and anthracene

nanocrystal were prepared by the reprecipitation method in which a dilute solution of the

compound prepared by water soluble solvent, i.e. good solvent, is injected into vigorously

stirred water as a poor medium. These nanocrystals have been the subject of much

interest in recent years due to their novel optical and electronic properties, which depend

on crystal size (Hae-Ryong Chung et al., 2006).

Diethylamine (DEA), tetrahydrofuran (THF), acetone, and dimethyl sulfoxide (DMSO)

were used as ‘good’ solvents without further purification. Ultra-pure water (18.2MΩcm)

was used as a ‘poor’ solvent. The compound was dissolved in the good solvent and the

solution (2mM, 100 µl) was injected into vigorously stirred water (10 ml) using a

microsyringe at a given temperature. Crystal size was evaluated by dynamic light

scattering (DLS) spectroscopy and scanning electron microscopy (SEM). The

nanocrystals were removed from the solution by filtration using a Millipore filter, or

deposited on a substrate using a layer-by-layer procedure, and dried in air for SEM

measurement. The crystal structure of perylene and anthracene nanocrystals was analyzed

by powder X-ray diffraction (XRD).

The resulting nanocrystals are dispersed stably in water. The perylene nanocrystal growth

process showed good solvent and temperature dependence. After 20 min, it was found that

5
crystal size increased gradually with time, and was also higher at elevated crystallization

temperatures. We should employ the experimental results at room temperature (298 K) for

the purpose of investigating effect of the good solvent in the reprecipitation method.

Actually, after 24 h crystal size became almost constant at 298 K, and this value was

defined as the pseudo equilibrium size in the present study. It was found that the average

size of perylene nanocrystals formed, as evaluated by dynamic light scattering technique,

decreased as the dielectric constant of the good solvent increased, while the size of the

anthracene nanocrystals increased with increasing dielectric constant due to association in

the aqueous dispersion liquid. The relationship between size and solvent dielectric

constant for anthracene nanocrystals is the inverse of that found for perylene nanocrystals.

Organic synthetic nanocrystal is expensive; hence organic natural nanocrystal is preferred

due to its availability of renewable recourses. Available nanocrystals include cellulose and

starch nanocrystal. Cellulose is abundant and more economic as it is edible compact

starch. The nanocomposite structure has strong potential to develop various kinds of

multifunctional materials for the energy and environment sectors. Properties which have

been shown to undergo substantial improvements include mechanical properties e.g.

strength, modulus and dimensional stability, decreased permeability to gases, water and

hydrocarbons, thermal stability and heat distortion temperature, flame retardancy and

reduced smoke emissions, chemical resistance, surface appearance, electrical conductivity,

optical clarity in comparison to conventionally filled polymers.

To date one of the few disadvantages associated with nanoparticles incorporation has

concerned toughness and impact performance. Some of the data presented has suggested

that nanoclay modification of polymers such as polyamides could reduce impact

6
performance. Clearly this is an issue which would require consideration for applications

where impact loading events are likely. In addition, further research will be necessary to,

for example, develop a better understanding of formulation, structure and property

relationships, better routes to platelet exfoliation and dispersion.

2.1.2 Cellulose nanocrystal

Cellulose is one of the most abundant natural materials, typically found in the cell walls

of plants. The crystalline form of it can be derived through the hydrolysis of a variety of

biopolymers such as wood, cotton, and tunicate in sulfuric acid. This will produce either

needle or rod shaped nanocrystals with a range of aspect ratio depending on the raw

material. A cellulose single-crystal is very strong; its stiffness is one-seventh that of

carbon nanotubes (~1 TPa). The single layer adsorption of cellulose nanocrystals was

demonstrated to be fast and produced films of very high loading. This creates a

polymer/nanocrystal film with exceptional strength. The low cost of raw material, ease of

dispersion, and adsorption quality may allow for more efficient mass production of layer-

by-layer composite films using either dipping or spraying methods (Lang Sui et al.,

2008).

The polymer/nanocrystal films are made using the layer-by-layer deposition method.

Monolayer of chitosan and cellulose nanocrystals were alternatively adsorbed onto Si

substrate to produce a thin film. The films elastic moduli were measured using Brillouin

light scattering (for films as thin as 250 nm) in the backscattering geometry. Using this

technique, elastic properties of a material are derived from the inelastic scattering of light

as it interacts with acoustic phonons. Comparison between the behaviors of surface and

7
bulk acoustic modes allowed us to elucidate the effect of the thickness of individual

layers relative to the total film thickness on the overall elastic properties of the

composite. The elastic moduli of polymer/nanocrystal composites with crystals of

different aspect ratios were measured using Brillouin light scattering. Short cellulose

nanocrystals with length of ~200 nm were produced from the hydrolysis of filter paper

powder in sulfuric acid. Long crystals with lengths of several microns were produced by

the bleaching and hydrolysis of tunicate using sulfuric acid. Layer-by-layer films are

fabricated using alternative depositions of chitosan or poly diallyldimethylammonium

chloride (PDDA) and cellulose nanocrystals. The moduli of films with long crystals are

observed to be dramatically higher than films with short crystals for both

chitosan/nanocrystal and PDDA/nanocrystal films. It is also observed that the moduli of

chitosan/nanocrystal films are higher than that of PDDA/nanocrystal films. In fact,

cellulose chains are biosynthesized by enzymes and aggregate to form microfibrils.

Depending on their origin, the microfibril section ranges between 2 and 20 nm for lengths

that can reach several tens of microns. They aggregate further to form fibers. Therefore,

each natural fiber can be considered as a string of cellulose crystallites, linked along the

chain axis by disordered domains (Gilberto S. et al., 2009).

2.1.3 Applications of cellulose nanocrystals

The nanocrystals can be used in ceramics and in biomedical applications such as artificial

joints and disposable medical equipment. Using cellulosic nanocrystals to strengthen

plastics has advantages over the glass that is often used: Glass is heavier, harder on

8
processing machinery and therefore more expensive to work with, and it stays in the

ground for centuries. The cellulose nanocrystals will break down quickly in a landfill.

Anything which is made in nature can be destroyed in nature and these cellulose particles

have a lifetime in a landfill of less than 90 days, at which time, they go back into carbon

dioxide and water. It can be reabsorbed by other plants that use it to make more cellulose

(Winter et al., 2009).

In Winter’s process, the cellulose is first purified in the laboratory as substances such as

wax and gluey lignin are removed from the biomass. The cellulose then goes through a

homogenizing process, similar to the one used with dairy products. The cellulose is

shredded into tiny particles under high pressure, rendering nanocrystals, so-called

because they are so miniscule they are measured in nanometers. The result is a viscous,

white liquid that goes into a microcompounder, where it is mixed with plastic under high

pressure. The unit produces a cord or a ribbon, depending on the die being used to shape

it of crystal-reinforced plastic that can tested for several properties. Winter’s team is

currently working on refining the surface of the crystals so they adhere better to the

plastic, and disbursing the crystals throughout the material to achieve the best results. In

the future, Winter said the process could be tied to the production of cellulosic ethanol.

When hemicellulose is removed from wood for fermentation into ethanol, it leaves

behind cellulose that can be treated with enzymes and reduced to the nanocrystals uses in

the lab. The value of those crystals in industrial uses represents a significant reduction in

the cost of producing ethanol.

9
2.2 Polypropylene

2.2.1 Chemical and physical properties

Most commercial polypropylene is isotactic and has an intermediate level of crystallinity

between that of low density polyethylene (LDPE) and high density polyethylene (HDPE);

its Young's modulus is also intermediate. PP is normally tough and flexible, especially

when copolymerized with ethylene. This allows polypropylene to be used as an

engineering plastic, competing with materials such as ABS. Polypropylene is reasonably

economical, and can be made translucent when uncolored but is not as readily made

transparent as polystyrene, acrylic or certain other plastics. It is often opaque or colored

using pigments. Polypropylene has good resistance to fatigue.

Polypropylene has a melting point of ~160°C (320°F), as determined by Differential

scanning calorimetry (DSC). The MFR (Melt Flow Rate) or MFI (Melt Flow Index) is a

measure of PP's molecular weight. This helps to determine how easily the molten raw

material will flow during processing. Higher MFR PPs fill the plastic mold more easily

during the injection or blow molding production process. As the melt flow increases,

however, some physical properties, like impact strength, will decrease.

There are three general types of PP: homopolymer, random copolymer and block

copolymer. The comonomer used is typically ethylene. Ethylene-propylene rubber or

EPDM added to PP homopolymer increases its low temperature impact strength.

Randomly polymerized ethylene monomer added to PP homopolymer decreases the

polymer crystallinity and makes the polymer more transparent.

10
2.2.2 Degradation of Polypropylene

Polypropylene is liable to chain degradation from exposure to UV radiation such as that

present in sunlight. For external applications, UV-absorbing additives must be used.

Carbon black also provides some protection from UV attack. The polymer can also be

oxidized at high temperatures, a common problem during moulding operations. Anti-

oxidants are normally added to prevent polymer degradation. The activation energy

estimated for the polypropylene degradation at 250-300°C was not significantly different

from that determined by volatilization measurements at higher temperatures (Thomas E.

Davis et al. 1961).

Cavitation results in generation of hot spots as well as turbulence associated with liquid

circulation which can result in degradation of polymeric compounds. In the present work

cavitation generated using ultrasound has been utilized for degradation of polypropylene

and effect of different operating parameters on the extent of degradation has been

investigated. It was found that extent of degradation increases with a decrease in reaction

volume and concentration. Use of p-xylene as a solvent resulted in higher extent of

degradation. It was also observed that a constant solution viscosity is reached beyond

which ultrasonic irradiation could not further degrade polypropylene. The limiting

viscosity was also observed to depend on the volume and concentration of polypropylene

(Vaibhav Desai et al., 2007).

2.2.3 Significant of polypropylene

11
It is a linear structure based on the monomer CnH2n. It is manufactured from propylene

gas in presence of a catalyst such as titanium chloride. Beside PP is a by-product of oil

refining processes. Most polypropylene used is highly crystalline and geometrically

regular (i.e. isotactic) opposite to amorphous thermoplastics, such as polystyrene, PVC,

polyamide, etc., which radicals are placed randomly (i.e. atactic).

It is said that PP has an intermediate level of crystallinity between low density

polyethylene (LDPE) and high density polyethylene (HDPE); On the other hand PP has

higher working temperatures and tensile strength than polyethylene.

Additives are used in Polypropylene to prevent polymer degradation, resulting from

exposure to heat, shear and light. They broaden the property and application range by

providing higher functionality and enhanced performance. As colorants, Organic

Pigments provide solutions of high technical standard and are most suitable for

Polyolefins. With Polypropylene applications, the requirements for organic pigments

broaden and demand excellent processing properties like heat resistance or dispersibility

and durable end-use properties like heat and weather fastness.

In general homopolymers (i.e. with only one type of monomer) can be used for housing,

housewares, packaging, cassette holders and fibers, monofilaments and film tapes;

copolymers (i.e. different monomers are involved) are preferred for all applications

exposed to cold and they are widely used for pipes, containers, boat hulls, seat shells and

automotive parts e.g. battery cases and bumpers. Polypropylene can be manufactured to a

high degree of purity to be used for the semiconductor industry. Its resistance to bacterial

growth makes it suitable to be used in medical equipment. Polypropylene is used in most

of our nonwoven fabrics such as rope used in a variety of industries, including fishing

12
 and agriculture. PP can be used for flexible packaging applications (e.g. yogurt

containers, syrup bottles, straws, etc.), construction sector (e.g. drainage pipes, pumps,

etc.), automotive sector, etc.

2.3 Polypropylene, microcrystalline cellulose composites with enhanced compatibility

and properties.

Polypropylene (PP) microcrystalline cellulose (MCC) composites were prepared

containing Poly (propylene-graft-maleic anhydride) (PP-g-MA) and MCC treated with

silicone oil, stearic acid or alkyltitanate coupling agent to promote matrix–filler dispersion

and compatibility. The aim was to prepare and characterize PP–microcrystalline cellulose

(MCC) composites, through modification of fiber surface and the addition of PP-g-MA as

a compatibilising agent. Surface treatment of the MCC involved the use of a fatty acid, a

silane coupling agent and an alkyltitanate. The objectives were to characterize the thermal

stability and morphology of the resulting composites and to evaluate the effect of the

compatibilisation or surface treatment on the thermomechanical behavior of the matrix.

The extent of effectiveness for each treatment on the cellulose fibers was evaluated to

identify its impact on the composite performance (Steven Spoljaric et al., 2009).

The thermal stability of PP was marginally (~2 oC) enhanced by increasing the MCC

concentration. The thermal stability of MCC increased significantly following

incorporation of the cellulose fibers into the PP matrix. PP-g-MA increased the thermal

stability of PP by 10 oC and lowered the mass loss rate resulting in degradation occurring

over a broader and higher temperature range. MCC increased the crystallization

temperature (Tc) of the composites, demonstrating MCC is an effective nucleator of PP.

13
 PP-g-MA further increased the Tg of the composites by 2 oC, verifying that PP had

decreased mobility in the composites. Crystallinity was observed to decrease with

increasing MCC content. This was attributed to the MCC having cellulose II form that does

not transcrystallise PP.

The modulus (E) of the composites increased with MCC content, confirming effective filler

reinforcement. E was further increased by incorporation of alkyltitanate and stearic acid

coupling agents and PP-g-MA that provided enhanced compatibility and allowed greater

stress transfer. Creep deformation decreased and permanent strain increased with MCC

content. This was due to adsorption of the matrix onto MCC, restricting molecular motions

of the PP chains.

CHAPTER 3

METHODOLOGY

3.1 Materials

The lists of materials used are:

Polypropylene

Microcrystalline cellulose (MCC)

Cellulose Nanocrystal (NCC)

Kenaf fiber

14
3.2 Formulating by varying ratio of PP.MCC and PP.NCC and kenaf fiber

Before we prepare the sample, we must make a formulating the composition to produce a

sample. We use the various ratio of composition is aim to compare the different ability of

the sample during testing. The formulating composition is shown in the table. Table 3.1

shows the composition of the polypropylene with the microcrystalline cellulose; table 3.2

shows the composition of the polypropylene with the nanocrystalline cellulose: table 3.3

the composition of the polypropylene, microcrystalline cellulose, nanocrystalline

cellulose and adding of kenaf fiber.

Table 3.1 Composition of polypropylene and microcrystalline cellulose

Sample Polypropylene(g) Microcrystalline cellulose (%)

F1 1000 10

F2 1000 20

F3 1000 30

F4 1000 40

Table 3.2 Composition of polypropylene and nanocrystalline cellulose.

Sample Polypropylene(g) Nanocrystalline cellulose (%)

F1 1000 0.2

F2 1000 0.5

F3 1000 1.0

15
 F4 1000 1.5

Table 3.2 Composition of polypropylene, microcrystalline cellulose and nanocrystalline cellulose

with kenaf fiber.

Sample Polypropylene(g) Microcrystalline Nanocrystalline Kenaf fiber (g)

cellulose (%) cellulose (%)

F1 100 - 0.2 200

F2 100 - 0.5 200

F3 100 20 - 200

This formulating ratio will use to prepare the sample by using twin screw extruder. Twin screw

extrusion is used extensively for mixing, compounding, or reacting polymeric materials.

The flexibility of twin screw extrusion equipment allows this operation to be designed

specifically for the formulation being processed. For example, the two screws may be co-

rotating or counter rotating, intermeshing or nonintermeshing. In addition, the

configurations of the screws themselves may be varied using forward conveying

elements, reverse conveying elements, kneading blocks, and other designs in order to

achieve particular mixing characteristics. The extruder has two zones that the first zone is

feed zone having uniform screw root diameter and the compression zone with continuously

increasing root diameter. The temperature was measured by using a PT-100 precision

thermocouple and the screw speed was measured by using a proximity switch. One

technique for orienting some polymers, such as polyethylene, is by plastic flow at

temperatures below the melting point. The degree of orientation in such polymers is

indicated by the increase in tensile modulus of the oriented polymer over the tensile

modulus of the unoriented polymer. GRP was extruded at a constant feed rate of

16
 50cm/min and the extrudate has been designated as extrusion processed polypropylene

powder.

3.3 Mechanical testing

3.3.1 Tensile and impact test

The samples will bring to test with tensile and impact testing. Tensile test is probably the

most fundamental type of mechanical test you can perform on material. First of all, the

sample must be form into dumbbell shape or straight shape to perform in tensile test

machine. The rate at which a sample is pulled apart in the test can range from 0.2 to 20

inches per minute and will influence the results. As the material is being pulled, you will

find its strength along with how much it will elongate.

The impact then will be implementing to measure a materials resistance to impact from a

swinging pendulum. The specimen is clamped into the pendulum impact test fixture with

the notched side facing the striking edge of the pendulum. The pendulum is released and

allowed to strike through the specimen. If breakage does not occur, a heavier hammer is

used until failure occurs. Since many materials (especially thermoplastics) exhibit lower

impact strength at reduced temperatures, it is sometimes appropriate to test materials at

temperatures that simulate the intended end user environment. The standard specimen for

ASTM is 64 x 12.7 x 3.2 mm (2½ x ½ x 1/8 inch). The most common specimen thickness

is 3.2 mm (0.125 inch), but the preferred thickness is 6.4 mm (0.25 inch) because it is not

as likely to bend or crush. The depth under the notch of the specimen is 10.2 mm (0.4

inches).

17
 3.3.2 Melt flow index

Then the samples are bringing to melt flow indexer to test a measure of the ease of flow

of the melt of a thermoplastic polymer. It is defined as the mass of polymer in grams

flowing in 10 minutes through a capillary of specific diameter and length by a pressure

applied via prescribed alternative gravimetric weights for alternative prescribed

temperatures. The method is given in ASTM D1238 and ISO 1133. The samples are

prepared in pellet form to carry out this testing.

3.4 Thermal characterizations

3.4.1 Differential scanning calorimetry (DSC)

Differential scanning calorimetry will operate to study what happens to polymers when

they are heated. There are two pans. In one pan, the sample pan, you put your polymer

sample. The other one is the reference pan. You leave it empty. Each pan sits on top of a

heater. Then you tell the nifty computer to turn on the heaters. So the computer turns on

the heaters, and tells it to heat the two pans at a specific rate, usually something like 10 oC

per minute. The computer makes absolutely sure that the heating the rate stays exactly the

same throughout the experiment.

3.4.2 Thermogravimetry (TGA)

18
 Then the sample is carrying out with TGA to measure the weight changes in the sample.

TGA is a technique in which the mass of a substance is measured as a function of

temperature, while the substance is subjected to a controlled temperature programme.

The temperature programme means the heating or cooling at a linear rate and isothermal

measurements. It also can be combinations of heating, cooling and isothermal stages and

other more modern approaches in which the temperature profile is modified according to

the behaviour of the sample.

3.5 Morphology

3.5.1 Scanning electron microscopy (SEM)

This study also interest to know the morphology of the sample that will carry out by

using scanning electron microscopy (SEM). The SEM is a microscope that uses electrons

instead of light to form an image. The SEM is an instrument that produces a largely

magnified image by using electrons instead of light to form an image. A beam of

electrons is produced at the top of the microscope by an electron gun. The electron beam

follows a vertical path through the microscope, which is held within a vacuum. The

beam travels through electromagnetic fields and lenses, which focus the beam down

toward the sample. Once the beam hits the sample, electrons and X-rays are ejected from

the sample.

Figure 3.1 Flowchart of methodology

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