Foaming of Rubber Wood Plastic Composite

FOAMING OF RUBBER WOOD PLASTIC COMPOSITES (RUBWPC)
Elton Qafaliaj [1213525]
Supervisor: Professor Mizi Fan
Individual Dissertation submitted to the Department of Civil Engineering
School of Engineering and Design, Brunel University
Confidential
ABSTRACT
This project is linked with the European project RUBWPC which is the rubber fusion of wood plastic
composites to make functional composites for building applications from waste rubber tyres, waste
plastic and waste wood. This study investigates different chemical foaming agents as a method of
weight reduction in order to produce a composite material that can be used for applications such as
interior walls or rigid thermal insulation. Two different foaming agents were tested with different sizes
of wood flour and polyethylene particles. The hot pressing method was used for the production of the
material samples. The tensile strength decreased when foaming agents were added, the moisture
absorption and the thickness swelling also increased when foaming agents are added. The SEM analysis
showed that samples foamed using sodium bicarbonate produced more uniform foaming in the
polyethylene but had a higher likelihood of producing large voids in the composites. The density of the
samples was reduced by the addition of the foaming agents with sodium bicarbonate producing a higher
density reduction than Azodicarbonamide.
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ACKNOWLEDGEMENTS
My sincerest thanks are extended to my project supervisor and mentor, Professor Mizi Fan for the
constant support, guidance and advice. I would also like to thank Katherine Cashell for her valuable
advice and assistance throughout this project.
I wish to express my sincere thanks to the lab technicians who helped me throughout the project. I
would also like to express my gratitude to Yonghui Zhou for his expert advice, guidance and assistance
throughout this project. I am extremely grateful to my family and friends for their continued support
and motivation.
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Contents
ABSTRACT ............................................................................................................................................... i
ACKNOWLEDGEMENTS ...................................................................................................................... ii
LIST OF TABLES ................................................................................................................................... iii
LIST OF EQUATIONS ........................................................................................................................... iii
LIST OF FIGURES .................................................................................................................................. iii
LIST OF NOTATIONS ............................................................................................................................ v
CHAPTER 1 INTRODUCTION .............................................................................................................. 1
1.1. Composite Material History ...................................................................................................... 1
1.2. Market Overview....................................................................................................................... 2
1.2.1. Wood ....................................................................................................................................... 2
1.2.2. Rubber ..................................................................................................................................... 2
1.2.3. Plastic ...................................................................................................................................... 2
1.3. Materials Research .................................................................................................................... 3
1.3.1. Wood ................................................................................................................................. 3
1.3.1.1. Cellulose ........................................................................................................................... 3
1.3.1.2. Hemicellulose ................................................................................................................... 3
1.3.1.3. Lignin ............................................................................................................................... 4
1.3.1.4. Other extractives. ............................................................................................................. 5
1.3.2. Tyres .................................................................................................................................. 5
1.3.2.1. Rubber ....................................................................................................................... 7
1.3.2.1.1. Synthetic rubber ........................................................................................................ 7
1.3.3. Coupling agents ....................................................................................................................... 7
1.3.3.1. Silane ................................................................................................................................ 7
1.3.3.2. Maleic Anhydride ............................................................................................................. 8
1.3.3.3. Acetylation ....................................................................................................................... 9
1.3.4. Blowing agents ........................................................................................................................ 9
1.3.4.1 Sodium Bicarbonate (NaHCO3) ........................................................................................ 9
1.3.4.2. Azodicarbonamide (AZDC) ........................................................................................... 10
1.3.4.3 Expancel .......................................................................................................................... 10
1.3.4.4. (OBSH) 4, 4 Oxybis (benzenesulfonylhydrazide).......................................................... 10
1.4. Problem Statement .................................................................................................................. 11
1.5. Research Methodology ............................................................................................................ 11
1.6. Research Objectives ................................................................................................................ 11
CHAPTER 2 LITERATURE REVIEW.................................................................................................. 12
2.1. Introduction .................................................................................................................................. 12
2.2. Foaming of Wood rubber plastic composites ............................................................................... 12
CHAPTER 3 EXPERIMENTAL PROCEDURE ................................................................................... 14
3.1. Raw Materials .............................................................................................................................. 14
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3.1.1. Wood Fibre............................................................................................................................ 14
3.1.2. Rubber ................................................................................................................................... 14
3.1.3 HDPE ..................................................................................................................................... 15
3.1.4. Coupling Agent ..................................................................................................................... 15
3.1.5 Foaming Agent ....................................................................................................................... 15
3.2. Equipment .................................................................................................................................... 16
3.3. Initial Experimental Design ......................................................................................................... 18
3.4. Methodology ................................................................................................................................ 19
3.5. Testing Procedure......................................................................................................................... 21
3.5.1. Density .................................................................................................................................. 21
3.5.1.1. Scope .............................................................................................................................. 21
3.5.1.2. Apparatus ....................................................................................................................... 21
3.5.1.3. Procedure........................................................................................................................ 21
3.5.2. Tensile Strength..................................................................................................................... 22
3.5.2.1. Scope .............................................................................................................................. 22
3.5.2.2. Principle ......................................................................................................................... 22
3.5.2.3. Apparatus ....................................................................................................................... 22
3.5.2.4. Sampling......................................................................................................................... 24
3.5.2.5. Procedure........................................................................................................................ 24
3.5.2.6 Results ............................................................................................................................. 24
3.5.3 Scanning Electron Microscopy .............................................................................................. 24
3.5.4. Thickness Swelling and Moisture Absorption ...................................................................... 25
3.5.4.1. Scope .............................................................................................................................. 25
3.5.4.2. Principle ......................................................................................................................... 25
3.5.4.3. Apparatus ....................................................................................................................... 25
3.5.4.4. Test piece preparation .................................................................................................... 25
3.5.4.5. Procedure........................................................................................................................ 25
CHAPTER 4 RESULTS AND DISCUSSION ....................................................................................... 26
4.1 Tensile Tests.................................................................................................................................. 26
4.2. Density ......................................................................................................................................... 29
4.3 Mass change .................................................................................................................................. 32
4.4 SEM Results .................................................................................................................................. 35
CHAPTER 5 CONCLUSION AND RECCOMENDATIONS ............................................................... 49
REFERENCES ........................................................................................................................................ 51
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LIST OF TABLES
Table Page
Table 1 Composition of a tyre (WRAP) .................................................................................................... 6

Table 2 Initial experimental design ......................................................................................................... 18
Table 3 Analysis techniques used in 40 previous papers ........................................................................ 18
Table 4 Tensile test results ...................................................................................................................... 26
Table 5 Table of density and swelling results ......................................................................................... 29
LIST OF EQUATIONS
Equation 1 Density of samples ................................................................................................................ 22
Equation 2 Tensile strength ..................................................................................................................... 24
Equation 3 Swelling ................................................................................................................................ 25
Equation 4 Moisture absorption .............................................................................................................. 25
LIST OF FIGURES
Figure Page
Figure 1 Chemical structure of cellulose. .................................................................................................. 3

Figure 2 Chemical structure of hemicellulose ........................................................................................... 4
Figure 3 Chemical structure of a small piece of lignin polymer ............................................................... 4
Figure 4 Cross-section of modern car tyre ................................................................................................ 5
Figure 5 General formula for a silane coupling agent ............................................................................... 7
Figure 6 Reaction process for silane ......................................................................................................... 8
Figure 7 Chemical formula of MaPE ........................................................................................................ 8
Figure 8 Chemical formula of AZDC ..................................................................................................... 10
Figure 9 Wood flour ................................................................................................................................ 14
Figure 10 Rubber powder........................................................................................................................ 14
Figure 11 Heat press machine ................................................................................................................. 16
Figure 12 High temperature release wax................................................................................................. 16
Figure 13 Barbender high temperature mixing machine ......................................................................... 17
Figure 14 Samples 1-7............................................................................................................................. 19
Figure 15 Samples 7-12........................................................................................................................... 20
Figure 16 Samples 1-12 cut and prepared for the tensile tests ................................................................ 20
Figure 17 Axes layout of the samples ..................................................................................................... 21
Figure 18 Tensile testing diagram ........................................................................................................... 23
Figure 19 Instron testing machine ........................................................................................................... 23
Figure 20 Gold coated samples prepared for SEM ................................................................................. 24
Figure 21 Gold coating machine ............................................................................................................. 24
Figure 22 Graph of tensile strength against tensile extension for samples 1-6 ....................................... 27
Figure 23 Sample 3 wrinkling ................................................................................................................. 27
Figure 24 sample 9 showing the collecting of the larger wood particles ................................................ 27
Figure 25 Graph of tensile strength against tensile extension for samples 7-12 ..................................... 28
Figure 26 Density bar chart for samples 1-6 ........................................................................................... 30
Figure 27 Density bar chart for samples 7-12 including control and PE sample .................................... 31
Figure 28 Graphs of mass change over time for samples 1-8 ................................................................ 32
Figure 29 Graphs of mass change over time for samples 9-12, the control sample and PE sample ....... 33
Figure 30 Sample 1 SEM images ............................................................................................................ 35
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Figure 35 Samples 6 SEM images .......................................................................................................... 40
Figure 39 Sample 10 SEM images .......................................................................................................... 44
Figure 42 Pure Polyethylene SEM images .............................................................................................. 47
Figure 43 Control Sample SEM images .................................................................................................. 48
iv
LIST OF NOTATIONS
HDPE High Density Polyethylene

PP Polypropylene
AZDC Azodicarbonamide
RUBWPC RUBWPC Rubber Wood Plastic Composite
SEM Scanning Electron Microscopy
𝜌 Density in kg/m3
EU European Union
BERR Department for Business, Enterprise and Regulatory Reform
MaPE Maleic Anhydride-Grafted Polyethylene
MA Maleic Anhydride
UPR Unsaturated Polymer Resins
CFA Chemical Foaming Agent
PE Polyethylene
PMMA Polymethymethacrylate
OBSH 4, 4 Oxybis (benzenesulfonylhydrazide)
SBR Styrene Butadiene Rubber
FTIR Fourier Transform Infrared Spectroscopy
WPC Wood Plastic Composite
t Thickness
x Length along the x-axis
y Length along the y-axis
m Weight of sample to within 0.01g
Tensile strength in N/mm2
a Length of test sample
b Width of test sample
Fmax Breaking Load (N)
m1 Mass before submersion
m2 Mass after submersion
Wt Moisture absorption (%)
Gt Change in thickness (%)
t1 Thickness before submersion
t2 Thickness after submersion
Wt % Percentage of weight
v
CHAPTER 1: INTRODUCTION
1.1. Composite Material History
A composite material is made up of two or more individual materials with significantly different
physical or chemical properties. Matrix and reinforcement are the two main categories of constituent
materials. The reinforcement material is surrounded and supported by the matrix material. Individually,
the materials may not have very impressive or applicable properties but when combined the resulting
composite will take advantage of the superior quality of each of its constituents to produce a material
which performs better than any of its constituents alone. There is a large variety of constituent materials
allowing for the customization of the properties and the tailoring of a material to its use.
In many parts of the world steel rods are used in concrete columns, beams, floors and bridges as
reinforcement against bending loads. Composites have in fact outperformed most metals and other non-
reinforced metals in terms of specific strength and stiffness of materials (Strong 2000).
In 1500 B.C., The first composite materials were used by the Egyptians in the form of straw fibres in
clay bricks for building construction and structural applications. Another early example of composite
use is concrete. It is a mix of aggregate, cement and sand which has a good compressive strength. In
more recent times, metal rods and wires are added to the concrete to increase its tensile strength
(Reinforced Concrete). In 1200 A.D. The first composite bow was introduced. It consisted of wood,
bone and animal glue. The composite bow was far superior to its wood only predecessor in both
accuracy and strength and was considered the most lethal weapon in the world until the invention of
gunpowder.
Each age in human history is classified by the type of material used in that age. Starting from the Stone
Age, the Bronze Age and the Steel Age however now that composite materials are so heavily
incorporated into our daily lives future generations may refer to our time as the Composite Age.
Composite materials are designed with particular benefits in mind such as low weight yet maintaining
high strength. High strength properties and weight reduction are important in transportation and
aerospace applications as it enhances the fuel consumption property of a vehicle. Carbon fibre
composites are several times stronger than steel and aluminium but only have half the weight. However
the cost of producing them is still high. Fibre reinforced plastics are the prime candidates for consumer
products such as sports equipment, appliances, electronics and corrosion resistant equipment (Ko et al
1999).
‘Composite materials also display good resistance to wear and tear. Fibre reinforced plastics perform
better in situations like severe weather and environmental conditions, corrosion and fatigue compared to
aluminium alloys. Another main drive for the development is the ease of manufacturing and production
compared to conventional forms’ (Rijswijk et al 2004).
Although it has only been just over 50 years since composite materials were first developed, they still
offer many more new potential applications especially as it is becoming a more important issue to
preserve the earth’s environment. The development of composite materials is expected to continue in
the future and it is also possible for them to become ecological materials due to their good properties.
Nonetheless, further research and development is required for their potential to be realized.
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1.2. Market Overview
1.2.1. Wood
The increase in demands from the human population across the world are resulting in the requirement
for advance waste management and increased recycling solutions which are required in both the
industrial and residential areas. The processing of the raw materials including timber and rubber product
manufacturing is one of the major areas of waste production in the UK. The UK itself is the fourth
largest economy. Despite the recent economic crisis around the world the UK economy has continued
to grow throughout the course of 2009 (National Statistics Online). Construction was the largest
contributor to the recent UK economic expansion representing 8.5% of the second quarter of
2010[REF]. The manufacturing and construction sectors consume a vast majority of the raw and
processed wood produced in the UK. The forestry commission estimates that a total of 10.6 million
tonnes of round wood were removed from the forests in the UK in 2012.
1.2.2. Rubber
In 2003 the EU Landfill Directive introduced a ban on whole tyres and in July 2006 on shredded tyres.
The disposal of both whole and shredded tyres is banned from landfill from 16th July 2006. More than
48 million tyres are disposed of each year in the UK alone according to BERR which presents a major
opportunity for the use of reprocessed tyres. A significant and rapid re-use or recycling trend is being
introduced by various companies. Considering the UK’s strong economy and individual wealth, access
to personal vehicles and transportation is really easy. According to the RAF Foundation the number of
cars in the UK has hit a record high of 29.2 million up from 29 million three months earlier. This
directly results in the increase in tyre consumption due to car ownership. Moreover, the annual average
travel distance for 2012 was 6691 miles with 66% of this being done using a car (National Statistics
Online).
1.2.3. Plastic
The UK plastics manufacturing sector is large and it constitutes an important UK economic strength. It
is estimated that the UK produces approximately 2.5 million tonnes of plastic raw material annually
[REF]. In the UK about 275000 tonnes of plastic are used each year, that’s about 15 million bottles per
day. The use of plastic in Western Europe is growing about 4% each year and most families throw away
about 40kg of plastic each year. Besides, 75% of post-consumer plastic waste is sent to landfill where it
can take up to 500 years to decompose which cause a negative effect on the environment. Also,
according to the International Plastics Task Force, plastic wastes can break down and release toxins that
harm the environment, animals and the general public.
2
1.3. Materials Research
1.3.1. Wood
Wood is an organic material, a natural composite of cellulose fibres (which are strong in tension)
embedded in a matrix of lignin which resists compression. It is a natural polymeric, cellular, fibre
composite with four primary constituents (Jayne 1959). It is also a heterogeneous hygroscopic, cellular
and anisotropic material composed mainly of hollow, elongated spindle shaped cells arranged in
parallel to each other along the trunk of a tree.
1.3.1.1. Cellulose
Cellulose consists of long, straight chains of glucose molecules. It forms the skeleton of the plant wall
and has the most desired properties for making paper. These fibres are long, strong and translucent.
Cellulose (C6H10O5) is the main constituent of wood accounting for around 50% of wood by weight.
Cellulose is the main reason for wood having great strength properties in tension due to the presence of
strong covalent bonds both within and in between the glucose units. It occurs in the form of long
slender filaments or chains that build up slowly within the cell wall. The average chain length is
approximately 5µm.
Figure 1 Chemical structure of cellulose.
As shown in figure 1, the links in the cellulose chain are a type of sugar: B-D-glucose. Two unlinked
molecules of B-D-glucose are pictured above. The sugar units are linked when water is eliminated by
combining the -OH group and H highlighted in grey. Linking just two of these sugars produces
a disaccharide called cellobiose. Cellulose is a polysaccharide produced by linking additional sugars in
exactly the same way. The length of the chain varies greatly, from a few hundred sugar units in wood
pulp to over 6000 for cotton. [REF-http://antoine.frostburg.edu/chem/senese/101/consumer/faq/what-is-
cellulose.shtml]
The linear cellulose molecules form highly ordered strands called fibrils during the growth of a tree.
Fibrils are arranged into the layer structural elements comprising of the cell wall and wood fibres. The
highly ordered structure with strong intermolecular forces and crystalline structure are what set wood
fibres apart from synthetic textile fibres.
1.3.1.2. Hemicellulose
Hemicelluloses are short branched chains of glucose and other sugar molecules which fill in the space
in the plant wall. They are soluble in water and are thus often removed during the pulping process.
Hemicellulose consists of mixtures of polysaccharides which include glucose, xylose, arabinose and 4-
0-methylglucironic acid (Figure 2). These mixtures are generally low in crystallinity and have chain
lengths in the region of 150 to 200 units
3
Figure 2 Chemical structure of hemicellulose
The most common hemicellulose in softwoods is galactoglucomannan accounting for 15-20% of the
wood mass. Arabinoglucuronoxylan is the second most common accounting for approximately 10% of
wood mass. In hard woods Arabinoglucuronoxylan is the most common hemicellulose accounting for
around 20-30% of wood mass with galactoglucomannan being the second most common accounting for
around 5% of wood mass.
1.3.1.3. Lignin
Lignin is a complex three dimensional phenolic polymer network that holds cellulose fibres together
and makes them rigid. Lignin accounts for approximately 25-35% of wood mass of soft woods and 15-
25% of the mass of hard woods. The composition of Lignin varies from species to species. Generally it
consists of hydroxyl- and methoxyl-substituted phenyl propane units.
Figure 3 Chemical structure of a small piece of lignin polymer
4
Lignin forms covalent bonds with hemicellulose and therefore cross links different polysaccharides
giving mechanical strength to the cell wall and by extension to the whole wood structure.
1.3.1.4. Other extractives.
Extractives make up between 1% and 5% of wood and comprise of the non-cell wall components such
as plant hormones, resin and fatty acids. They are removed during the processing of commercial woods
with the use of solvents such as water, alcohol, acetone and ether.
1.3.2. Tyres
The very first tyres were bands of iron placed on the wooden wheels of carts and wagons. Luckily, with
the discovery of rubber things changed. It was in the mid 1800’s that the first tyres made using rubber
appeared. They were simple tyres; the rubber carried the load entirely.
It was in 1845 that the pneumatic or air-filled tyre - which works by air within the tyre absorbing the
shocks of the road, was invented and patented by RW Thomson. The industrialization of Western
Europe and North America provided a platform for the tyre to evolve from a simple rubberised canvas
to the modern complex fabric, steel and elastomeric composite found in modern tyres.
Figure 4 Cross-section of modern car tyre
Brief descriptions of the parts of a tyre:
Tread-
The tread is the part of a tyre that contacts the road surface. The tread consists of a layer of rubber
compounded to suit the application of the tyre and the thickness serves to protect the belt and carcass.
The tread pattern serves the purpose of improving water drainage, providing traction, braking and
cornering characteristics and long tread life. [18]
Sidewall-
The sidewall on each side of the tyre, between the shoulder and the bead is the section that deflects
most during running. The rubber coating serves to protect the carcass. On the sidewall of every
5
passenger-car and light-truck tyre is an alphanumeric code that describes the dimensions of the tyre.
[18]
Shoulder-
Provides continuous contact with the road while manoeuvring. Shoulders wrap slightly over the inner
and outer sidewall of a tyre. [18]
Rim-
Also known as the curb guard, it acts as a scuff guard to protect the tyre against wear due to curb
contact. It is commonly apparent in the form of a protrusion of rubber sidewall running
circumferentially around the tyre. [31]
Textile cord ply-
Controls internal pressure and maintains the tyres shape. [31]
Inner liner-
Seals the air-filled inner chamber and acts as a tube in tubeless tyres [31]
Bead reinforcement-
Enhances directional stability and gives steering precision [31]
Steel cord for belt plies-
Enhances shape retention and directional stability, reduces the rolling resistance and increases the tyres
mileage performance. [31]
Table 1 Composition of a tyre (WRAP)
6
1.3.2.1. Rubber
1.3.2.1.1. Synthetic rubber

The rubber industry really started booming with the invention of the automobile. All those tyres created
and still create a huge market for vulcanized rubber. In the early 20th century, most tyres were made
from vulcanized latex rubber which was derived from trees. [31]
It was only a matter of time before scientists asked if rubber could be made artificially. As early as 1860
they had already worked out the chemistry of rubber and its vulcanization process. Chemists had heater
rubber to break it apart and found that it produced isoprene, oil and tar. They could make isoprene from
oil and then combine isoprene artificially to make rubber. [31]
1.3.3. Coupling agents
1.3.3.1. Silane
Silane coupling agents are compounds whose molecules contain functional groups that bond with both
organic and inorganic materials. A silane coupling agent acts as a sort of intermediary which bonds
organic materials to inorganic materials. It is this characteristic that makes silane coupling agents useful
for improving the mechanical strength of composite materials, for improving adhesion and for the resin
modification and surface modification. [67]
Figure 5 General formula for a silane coupling agent
As shown in the image above, the general formula for a silane coupling agent typically shows the two
classes of functionality. X is a hydrolysable group typically alkoxy, acyloxy, halogen or amine. The R
group is a non-hydrolysable organic radical that may poses a functionality that imparts desired
characteristic.
Silane coupling agents react with water (hydrolysis) to form silanol groups and oligomers are formed
through partial condensation. The silanol oligomers then form hydrogen bonds to the surface of the
inorganic material. Finally, the inorganic material is put through a drying process and robust chemical
bonds are formed through a dehydration chemical reaction. This process is represented in the image on
the following page
7
Figure 6 Reaction process for silane
When silane coupling agents are used for surface treating an organic material to promote adhesion
between the inorganic material and an organic material, it acts in the following ways.
 By improving the wettability of resins

 By improving the miscibility of resins
 By forming chemical bonds with resins
 By hydrogen bonding with resins
1.3.3.2. Maleic Anhydride

Maleic anhydride (MA) is an organic compound which is the acid anhydride of maleic acid. It is a
colourless or white solid with an acrid odour. Around 50% of maleic anhydride production is for the
production of unsaturated polymer resins (UPR). These resins are used to coat meshes of different
fibres to produce composites of varying properties.
Figure 7 Chemical formula of MaPE
Maleated coupling agents are widely used to strengthen composites containing fillers and fibre
reinforcements. Newly developed MaPE couplers for the wood-polyethylene market demonstrate
superior performance compared against other potential polyolefin coupling agents. Results indicate that
the new polyethylene couplers at 3% loading can double the tensile strength and triple the impact
properties compared to non-coupled blend of wood and polyethylene. [18]
8
1.3.3.3. Acetylation
This is the process of adding an acetyl group to a compound by substitution for an active hydrogen
atom. In the case of wood rubber composites, acetylation of the wood fibres produced a composite
which was superior in resistance to biodegrading when submerged in soil when compared to silane and
MA.
1.3.4. Blowing agents

Generally speaking, a blowing agent is mixed with the polymer melt to obtain a plastic article with
reduced density by displacing polymer with gas. Blowing or foaming agents fall into two general
classes – Physical or Chemical.
Chemical foaming agents (CFA’s) can be organic or inorganic compounds that release gasses upon
thermal decomposition. CFA’s are used to obtain low density foams.
Physical blowing agents such as hydrocarbons and liquid CO2 work by expanding to produce cells in
the material when the temperature is increased. This process can be reversible by lowering the
temperature to turn the gas back into a liquid.
CFA’s are categorized as endothermic and exothermic. Endothermic absorb energy to release CO2 and
water whilst exothermic CFA’s release energy and generate nitrogen. Exothermic CFA’s tend to yield
more gas and higher pressures than endothermic. Endothermic CFA’s generally decompose at 130-
230°C whereas exothermic decompose around 200°C.
Depending on cell sizes foams are split into
 Macro cellular – Cell dimension > 100µm

 Micro cellular – Cell dimension 1-100 µm
 Ultra-micro cellular – Cell dimension 0.1-1 µm
 Nano cellular – Cell dimension <0.1 µm
There are also closed and open cells where closed refers to each cell being separate and individual with
walls and open being interconnected cells due to missing walls.
Foaming occurs in three stages
 Formation of polymer/blowing agent solution/mixture

 Cell nucleation
 Cell growth
1.3.4.1 Sodium Bicarbonate (NaHCO3)

Sodium Bicarbonate is a CFA which releases CO2 upon decomposition. It combines with citric acid to
produce a homogenous cellular structure and it has a narrow temperature of decomposition range.
Sodium bicarbonate can be purchased mixed as Hyrocerol which is a mixture of PE, NaHCO3 and citric
acid.
NaHCO3 is not a great foaming agent alone but the presence of citric acid and the PE vehicle massively
increase its effectiveness with a 30% weight reduction at 3wt% and up to 20% weight reduction at
1wt%.
Hydrocerol in terms of morphology produces the most homogenous composite and produces cells
around 50-120 µm. Hydrocerol upon decomposition provides its own nucleation sites during
decomposition.
Hydrocerol decomposes at 170-220°C.
9
1.3.4.2. Azodicarbonamide (AZDC)
AZDC is most commonly used in the production of foams due to its high gas yield and the possibility
of matching its decomposition temperature to the polymer processing temperature through the use of
activating agents such as zinc oxide. AZDC decomposition produces mostly nitrogen and carbon
monoxide gas. AZDC Decomposes at around 225°C. AZDC has the chemical composition shown in the
figure below.
Figure 8 Chemical formula of AZDC
When tested with PP/wood composites AZDC showed good tensile properties even though the density
decreased.
At 1wt% the strength loss, reduction in modulus and elasticity are approximately 10% but at 3wt% the
losses are closer to 50% in all areas apart from elasticity.[14]
1.3.4.3 Expancel
Thermally expandable polymer particles with an encapsulated low-boiling-point hydrocarbon liquid
have been used in the foaming of polypropylene; this allows for the production of foams with up to
30% reduced density whilst maintaining a smooth surface
Expancel is the trademark of a foaming agent constituted by microspheres of polymethymethacrylate

(PMMA) containing an encapsulated liquid hydrocarbon. When the spheres are heated, the
thermoplastic shell softens and the gas increases in pressure, resulting in an expansion of the spheres.
Expancel shows good strength retention but relative to other foaming agents the weight reduction is not
as high.[21]
1.3.4.4. (OBSH) 4, 4 Oxybis (benzenesulfonylhydrazide)

OBSH can be used as a blowing agent for both rubbers and plastics. It produces plastics with fine cell
morphology when it is well dispersed into the matrix.
In a study conducted by W. Yamsaengsung and N. Sombatsompop, two types of OBSH were used to
produce samples of wood/natural rubber composites. The two types of OBSH were:
 Plain OBSH
 EPR-b-OBSH (Ethylene-propylene bound OBSH)
It was found that the EPR-b-OBSH gave foam with a greater number of cell structures, higher porosities
and resistances to water penetration on the foam surface. However, the foam with the EPR-b-OBSH
agent had worse elastic recovery as compared to that with plain OBSH due to deformation of cell
structures after prolonged compression loading.
Any of the above foaming agents can be used for HDPE, Natural rubber and Synthetic rubber.
I have chosen to use sodium bicarbonate in the form of Hydrocerol due to the ease of availability and
the homogeneity of the cells in the end product. This will be important in ensuring the mechanical
testing results can be used to predict what would occur in larger samples than the ones I will be
producing. Hydrocerol can be used for the foaming of both the HDPE and the SBR rubber and therefore
will be multifunctional in my tests.
The second foaming agent is Expancel. It was chosen as in previous studies it has been shown to have
good strength retention properties. This could be useful in the construction industry as it provides an
opportunity to produce a composite that retains high strength but is lower in weight.
10
The third foaming agent is AZDC. It was selected due to its extensive use in the foaming industry and
therefore its high availability. AZDC was also selected because the addition of activating agents such as
zinc oxide allows for customisability in terms of the decomposition temperature which means that it can
be used for both the rubber and the HDPE making it multifunctional. AZDC also is not required to be
used in large percentages to have a significant impact in the density of the end product. [49]
1.4. Problem Statement
This Project is linked with the European Project ‘RUBWPC’ aimed at manufacturing a new generation
of wood plastic composites from used tyre rubber, plastic and wood wastes. The aim of this project is to
develop a foaming process which reduces the density of the composite material making it more viable
for use in applications such as insulation.
1.5. Research Methodology
 Mixing of materials in Spain using AZDC and sodium bicarbonate as foaming agents.
 Fabrication of composite samples using the two foaming agents in combination with different
weight fractions of wood, plastic and HDPE.
 Density determination and mechanical testing of the samples.
 Analysis of the surface and cross section using SEM.
1.6. Research Objectives
The main aim of this project is to investigate the effects of foaming the rubber and plastic in the
composite and how the use of different foaming agents can affect this. The aim is to reduce density of
the final product whilst still maintaining relatively high strength. These studies aim to reduce the strain
on the world’s natural resources and reduce the levels of environmental pollution.
11
CHAPTER 2: LITERATURE REVIEW
2.1. Introduction
Wood plastic composites (WPC) have been researched for several decades, however wood rubber
plastic composites (RUBWPC) have not been thoroughly investigated as of yet. As the fibre based
polymer composites are well known for high strength to weight ratio, they are used extensively in
fabricating commercial structures. Manufacturers mostly rely upon some limited laboratory tests whose
methodologies are useful for simulations but not for predicting the products service properties. The
wood plastic composite has been in research attention for decades however minimal research has been
done on wood, rubber plastic composites.
2.2. Foaming of Wood rubber plastic composites
In Brazil, Soares and Nachtigall 2013 studied the effect of chemical and physical foaming additives on
the properties of PP/wood flour composites. In this study, wood flower was mixed with polypropylene.
The foaming agents added are Planagen, ZnO, AZDC, NaHCO3, Expancel and Hydrocerol in varying
quantities between 0.1 and 3 wt.%. They found that AZDC had thermal stability very similar to that of
pp which is slightly undesirable but it can be improved with the addition of zinc oxide at the cost of
some residual mass in the end product. They also found that pure sodium bicarbonate has very low
thermal stability which can be improved with the addition of citric acid. The foaming agents reduced
the density of the product but also introduced significant reductions in mechanical strength. Under SEM
analysis the most homogenous spread of voids comes from the use of a master batch named Hydrocerol
which contains sodium bicarbonate and citric acid along with PP. The AZDC produced a less
homogenous sample compared to Hydrocerol and sodium hydroxide.
In the US, Li and Matuana 2002 examined the influences of the contents, types, and forms of CFAs, as
well as the use of coupling agents, on the density reduction (or void fraction) and average cell size of
extrusion-foamed neat HDPE and HDPE/wood-flour composites. They found that CFA types
(endothermic vs. exothermic) and forms (pure or master batch) did not affect the void fractions
achieved in both neat HDPE and HDPE/wood-flour composite foams. The use of a coupling agent in
the formulation was required to achieve HDPE/wood-flour composite foams with high void fraction.
The optimum active CFA content (to maximize the void fraction) seemed to lie at around 1% for neat
HDPE and 0.5% for HDPE/wood-flour composites, independent of the CFA type.
Zhang et al. 2003 investigated the molecular properties of different HDPEs were first investigated. The
molecular weights of the HDPEs were calculated with rheological methods. Then, the morphology of
the HDPE foams was investigated to determine the effect on _f and morphology. Several conclusions
were obtained by analysis of the data:
1. All HDPE foams with different molecular weights had closed-cell structures.
2. Foaming grade was strongly dependent on ACA concentration and the polymer matrix. The obtained
foaming grades were proportional to ACA concentrations lower than 2.5%. A plateau was observed for
ACA contents higher than 2.5%, except for the highest molecular weight HDPE. Increasing the
molecular weight resulted in a decrease in the foaming grade.
3. Foam cell sizes were also strong functions of the molecular structure and ACA concentration.
For the lowest molecular weight HDPE, the cell size increased as ACA concentration increased.
As molecular weight increased, cell size first increased with ACA content, then reached a maximum,
and decreased. For the highest molecular weight HDPE, cell size only decreased with ACA content
because of high resistance (viscosity).
4. N0 was a strong function of molecular weight and blowing agent concentration. For the lowest
molecular weight structure HDPE, the N0 decreased with ACA concentration. For high-molecular-
weight HDPE, the N0 increased with ACA concentration. Clearly, increasing the molecular weight
resulted in an increase in N0.
12
Kuboki et al. 2009 investigated the mechanical properties and foaming behaviour of cellulose fibre
reinforced HDPE Composites This article investigated the effects of fibre length and maleated polymers
on the mechanical properties and foaming behaviour of cellulose fibre reinforced high density
polyethylene composites. Cellulose fibre lengths used were 60µm and 700µm both at 40 wt%. They
also treated some of the fibres with maleated polymers to test their properties against the untreated
samples. The flexural test results reveal that the long fibre composites had around 50% higher strength
and modulus than the short fibre composites. The higher strength and modulus of the long fibre
composites may be mainly due to the higher aspect ratio of the fibre (the ratio of length to width is 35
for the long fibre and 3 for the short fibre). The higher aspect ratio provided the higher efficiency of
stress transfer from matrix to fibre, thus increasing strength and modulus. All the maleated polymers
increased strength for both short fibre and long fibre composites, and HDPE-MA showed the highest
values for both short and long fibre composites. It is also noted that the addition of the maleated
polymers did not change the order of the composites without maleated polymers, namely, higher
strength of the long fibre composites with the maleated polymers than that of the short fibre
counterparts.
Najib et al. 2011 conducted an experimental investigation on the correlation between the acoustic and
dynamic mechanical properties of natural rubber foam when the foaming temperature is changed. A
higher foaming temperature generated a higher gas pressure, lower viscosity, lower relative density and
lower crosslink density, which increased the average cell size. However the higher foaming temperature
foams suffered greater losses in mechanical strength in exchange for superior sound insulation
properties.
Sombatsompop and Yamsaengsung 2009 found that with increasing quantities of foaming agents the
water uptake increased with increased percentages of blowing agent, the peel strength decreased with an
increase in amount of blowing agent. The thermal conductivity was also shown to decrease with an
increase in the amount of blowing agent used. The study also showed reduced tensile strength at
increased foaming agent levels and lower resistance to prolonged compression with higher permanent
deformations occurring at higher volumes of CFA.
13
CHAPTER 3: EXPERIMENTAL PROCEDURE
3.1. Raw Materials

For the investigation high density polyethylene plastic (HDPE) will be used as the matrix material.
Styrene butadiene rubber (SBR) in powder form will be used as well as the wood which will also be in
powder form. The coupling agent will be either silane and/or maleic anhydride. The foaming agents
used will be sodium bicarbonate and Azodicarbonamide.
3.1.1. Wood Fibre

Struktol supplied the rettenmaier wood floor. The wood flour has an approximate heat capacity of
2KJ/Kg-K.
Figure 9 Wood flour
3.1.2. Rubber
The waste tyre rubber was provided by Crumbrubber. Code CS0420-0000.
Figure 10 Rubber powder
14
3.1.3 HDPE
In this project, high density polyethylene plastic will be used, this material is readily available and low
in cost with a relatively low melting temperature of approximately 200°c. HDPE was chosen as the low
melting point enables the heat pressing to occur at lower temperatures without risking the burning of the
wood fibres or the thermal degradation of the rubber.
3.1.4. Coupling Agent

Maleic anhydride and silane are the two coupling agents used to improve the interfacial adhesion
between the three constituent materials in the composite. These two coupling agents are most effective
when heated to approximately 200°C which aligns them with the melting point of the HDPE matrix.
3.1.5 Foaming Agent

Commercially available Azodicarbonamide (AZDC) and sodium bicarbonate will be used as foaming
agents in this project. They were chosen as they are readily available and have activation temperatures
around the 200°C point which brings them in line with the coupling agents and the melting point of the
HDPE.
15
3.2. Equipment
Hot pressing machine– 150 Tonne, Single Ram Upstroke, Window Frame type, Single Daylight, Hot
Platen Hydraulic Press with Water cooling.
Figure 11 Heat press machine
Hot Press mould- A hot press mould with an internal volume measuring (100x100x100) mm custom
built for this experiment.
High temperature release wax and aluminium foil- Aluminium foil used to cover the top surface of the
mix which is in direct contact with the hot plate. Maximum Mould Release Wax was used to coat the
internal surface area of the mould allowing for the easy release of the heat pressed sample.
Figure 12 High temperature release wax
[www.smitsgroup.co.nz]
16
Mixer- A specialised hot mixer in Spain was required as the equipment was not available at Brunel
University. This mixer has the capacity to mix the ingredients at temperatures up to 300 degrees Celsius
enabling increased homogeneity of the mixture.
Figure 13 Barbender high temperature mixing machine
17
3.3. Initial Experimental Design
Below is a table summarising the initial experimental design for the samples which will be mixed and
heat pressed. All samples also included 1.5% MAPE, 1.5% Silane, 3.5% 12HSA, 4% ZnO and 3.5%
TPW709. Control sample had no ZnO.
Table 2 Initial experimental design
Sample Wood Wood HDPE PE size Rubber CFA CFA

(%) size (%) (micron) (%) 1 2
(micron) (%) (%)
3-1 50 Original 40 Original 0 8 0

3-4 30 125-250 40 Original 20 8 0
3-5 30 Original 40 <500 20 8 0
3-6 30 125-250 40 <500 20 8 0
3-10 30 125-250 40 Original 20 0 8
3-11 30 Original 40 <500 20 0 8
3-12 30 125-250 40 <500 20 0 8
Control 30 Original 40 Original 20 0 0
CFA 1: azodicarbonamide, CFA 2: Sodium Bicarbonate
The table below shows a summary of the analysis techniques used in 40 papers written on the foaming
of HDPE and rubber and the frequency of the occurrence of each technique.
Table 3 Analysis techniques used in 40 previous papers
No. of
Analysis technique papers
SEM 24
Density and swelling 15
DSC 12
Mechanical testing eg tensile, compressive, torsional 12
XRD analysis 5
Infrared spectroscopy 4
porosity 4
Quantitative image analysis 3
thermal conductivity 3
peel strength 2
TGA 2
AFM 1
Small Amplitude Oscillatory Shear (SAOS) tests 1
Surface roughness by eye and touch 1
18
3.4. Methodology
The required amounts of wood flour, rubber powder, polyethylene and all additives were packaged in
plastic bags and flown to Spain for mixing. They were mixed at 200 degrees Celsius. The different
mixtures were then put into 40g bags for transport back to Brunel University. High temperature release
film was cut into squares the same size as the base of the mould. And the inner face of the release film
was coated in a layer of high temperature release wax. 28g of each sample was weighed and put into the
mould. A layer of release film was placed on top and then the top piece of steel was placed to enclose
the mould.
The mould was then placed into the hot press and left to preheat to a temperature of 190 degrees Celsius
for 30 minutes. The mould was then pressed at a pressure of ten tonnes for 10 minutes. The final
thickness of the samples was determined by the materials resistance to flowing out of the mould.
Samples were then left to cool down for to room temperature prior to being taken out of the mould. The
samples were then cut into 5 strips 5-7mm wide and 100mm long. The remainder of each sample was
cut into three pieces with right angle corners for swelling and density testing. The strips were cut using
a table top ban saw accurate to 1mm and the material was conditioned at 20 degrees Celsius with 50%
humidity.
Figure 14 Samples 1-7
19
Figure 15 Samples 7-12
Figure 16 Samples 1-12 cut and prepared for the tensile tests
20
3.5. Testing Procedure
The tests done to the produced samples are according to European standards guidelines. The samples
are cut to the required size as specified by BS EN 326-1 using a ban saw accurate to 1mm. The samples
are then conditioned at 20 degrees with a variation of up to 3 degrees Celsius. And at 50% humidity for
24 hours prior to testing. [17]
3.5.1. Density
3.5.1.1. Scope
The testing of the samples is to be done under laboratory conditions according to BS EN 323-1993,
Wood based panels: Determination of density.
As defined in BS EN 323-1993 Density is;

‘The ratio of mass for each test piece to its volume both measured at the same moisture content and the
use of these results to estimate the density of the whole boards’.[17]
3.5.1.2. Apparatus
Length and width measurement -

Vernier calliper with capacity to measure lengths above 5mm and a reading accuracy to 0.01mm
Thickness measurement –
Use of a micrometer or equivalent measuring instrument, comprising of a flat and parallel circular
measuring surface of 16 mm diameter. It provides an operational force of 4N with a reading accuracy to
0.01mm. [17]
Balance-
Scientific balance to be used with accuracy of 0.01g
Dimensions-
Individual test pieces are required to maintain a square shape of length 50mm.
3.5.1.3. Procedure
Firstly each test piece must be weighed to within 0.01g. This value will be represented as (m) in the
formulaic calculations.
Measurement of the dimensions of the sample pieces is done according to BS EN 325-1993. The
thickness, t is measured at the centre of the sample to an accuracy of give or take 0.005 mm.
Measurements must then be taken of lengths along the x and y axis as shown in the figure below.[18]
Figure 17 Axes layout of the samples
21
3.5.1.4. Results
The density of the test samples is determined using the following equation:
Equation 1 Density of samples
𝒎
𝝆= × 𝟏𝟎𝟔 (1)
𝒙×𝒚×𝒕
Results will be produced in kgm-3 when measurements for ‘m’ are done in grams and measurements for
x, y and t are done in mm. If multiple tests are done for samples cut from the same piece of board, the
average density is to be taken.
3.5.2. Tensile Strength
3.5.2.1. Scope
This test procedure will be used to determine the resistance of the composite material under tensile
loading perpendicular to the plane of the board.
3.5.2.2. Principle
As determined by BS EN 319:1993 the tensile strength is:
‘Determination of resistance to tension perpendicular to the surface of the test piece by submitting the
latter to a uniformly distributed tensile force until rupture occurs. Tensile strength perpendicular to the
plane of the board is determined by the maximum load in relation to the surface area of the test piece.
[16]
3.5.2.3. Apparatus
An INSTRON testing machine will be used to carry out the tensile tests. A sliding calliper according to
BS EN 325 will be used. Hardwood test blocks will be used to sandwich the sample and provide a
gripping area for the metal clamps on the INSTRON. An illustration of the apparatus set up is provided
on the following page.
22
Figure 18 Tensile testing diagram
Figure 19 Instron testing machine
23
3.5.2.4. Sampling
‘Sampling and cutting of the test pieces shall be carried out according to EN 326-1. The test pieces shall
be rectangular with length (100 ± 1) mm and width (6± 1) mm. The test pieces shall be cut with
precision, the angles shall be 90° and the edges shall be straight and clean. The test pieces and the
hardwood, or hardwood plywood, testing blocks shall be conditioned to constant mass in an atmosphere
with a mean relative humidity of (65 ± 5) % and a temperature of (20 ± 2) °C. Constant mass is
considered to be reached when the results of two successive weighing operations, carried out at an
interval of 24 h, do not differ by more than 0,1 % of the mass of the test piece.’ [19] The test pieces are
then glued to the hardwood gripping pieces using epoxy 106 resin and excess glue pressed out from the
glue line is removed.
3.5.2.5. Procedure
Each sample is then gripped to the clamp via the hardwood pieces and a tensile force is applied until
failure occurs. ‘The load shall be applied at a constant rate of crosshead-movement throughout the test.
The rate of loading shall be adjusted so that the maximum load is reached within (60 ± 30) s.’ [19].
3.5.2.6 Results
Equation 2 Tensile strength
(2)
Where Fmax is the breaking load in Newtons and a, b is the length and width of the test piece, in
millimetres.
3.5.3 Scanning Electron Microscopy

A SIGMA series field emission scanning electron microscope was used to study the surface of the
samples split during tensile tests. The samples were coated in a thin layer of gold using a sputter coater
to increase the conductivity. Below is an image of gold coated samples prepared for the SEM.
Figure 20 Gold coated samples prepared for SEM
Figure 21 Gold coating machine
24
3.5.4. Thickness Swelling and Moisture Absorption
3.5.4.1. Scope
Testing is to be done according to BS EN 317:1993[15]. ‘This European Standard specifies a method of
determining the swelling in thickness of flat-pressed or drum-pressed particleboards, fibreboards, and
cement-bonded particleboards.’ [15].
3.5.4.2. Principle
Swelling in thickness is determined by measuring the increase in thickness of the test piece after
complete immersion in water. [15].
3.5.4.3. Apparatus
Micrometer
Micrometer, according to EN 325.
Water bath
‘A thermostatically controlled water bath, capable of maintaining a temperature of (20 ± 1) °C. Immerse
the test pieces with their faces vertical in clean, still water, having a pH of 7 ± 1 and a temperature of
(20 ± 1) °C. This temperature shall be maintained throughout the test period. During the test, the test
pieces shall be separated from each other and from the bottom and the sides of the water bath. The
upper edges of the test pieces shall be covered by (25 ± 5) mm of water throughout the test. The water
shall be changed after each test.’ [15].
3.5.4.4. Test piece preparation
Dimensions
Test pieces cut into squares of varying sizes determined by the amount of materials remaining.
3.5.4.5. Procedure
The thickness of each test piece will be measured using callipers to an accuracy of ± 0.01mm in
accordance with BS EN 325. The weight of the samples will also be taken before submersion and then
again after. After submersion, the dimensions will also be re-measured.
3.5.4.6. Results
The swelling in thickness of each sample Gt shall be calculated using the following formula.
Equation 3 Swelling
𝑡2−𝑡1
𝐺𝑡 = 𝑡1
× 100 (3)
Where t1 is the thickness of the sample in mm before immersion and t2 is the thickness of the sample
after immersion in mm. Gt will be calculated as a percentage and expressed to the nearest 1 decimal
place.
The change in mass shall be expressed as a percentage using the following formula.
Equation 4 Moisture absorption

𝑚2−𝑚1
𝑊𝑡 = 𝑚1
× 100 (4)
Where m1 is the weight of the test pieces before submersion in milligrams and m2 is the weight of the
test pieces after immersion in milligrams
25
CHAPTER 4: RESULTS AND DISCUSSION
4.1 Tensile Tests
Sample Tensile stress Tensile extension Strain at

at Maximum at Maximum load Maximum
Load (MPa) (mm) load (%)
1 6.175666667 0.110343333 0.22
2 3.9772 1.715518 3.43
3 4.82025 0.366025 0.73
4 7.614333333 0.531967 1.06
5 6.60475 0.50265 1.01
6 5.9434 0.1708 0.34
7 8.27375 0.15205 0.30
8 5.024 1.49475 2.99
9 3.56875 0.2331 0.47
10 5.0925 0.24565 0.49
11 4.8866 0.35034 0.70
12 6.4726 0.41428 0.83
Control 8.3444 1.37044 2.74088

sample
Table 4 Tensile test results
The control sample’s tensile results can be compared with those of samples 3 and 9 if the intent is to
find the impact on tensile strength of the foaming agents. Sample 3 shows that the tensile strength is
significantly reduced by the addition of the
26
Figure 22 Graph of tensile strength against tensile extension for samples 1-6
Figure 21 shows a graph of the tensile results for samples 1-6. These curves were calculated as the
average curve of the five pieces for each sample. The results show that sample 4 had the highest overall
tensile strength followed by sample 5 and then sample 1. This suggests that reducing the particle size of
the wood flour alone is most effective in increasing the tensile strength of the material. Sample 3
consists of the same mass fractions as samples 4, 5 and 6 and has a lower tensile strength than all 3.
This means that reducing the particle sizes of the constituent materials increases the tensile strength.
The sample with the lowest tensile strength is sample 2 at 3.9 MPa, this is likely due to the lack of wood
fibres which have high strength and the presence of higher rubber content which is weak in tension.
Sample 2 however did display the largest tensile extension which may be desirable in some
applications.
Comparing sample 3 to sample 8 it can clearly be seen that the tensile strength has been significantly
reduced by the addition of AZDC from 8.34 MPa to 4.82 MPa. The tensile strength of sample 4 would
suggest that the results for sample 3 may be outliers as some of the samples had wrinkling all over the
sample which could be weak points during the tensile tests and some of the test pieces for sample 3 split
at the point where the wrinkling occurred.
Some of the samples showed clumping of the particles

Figure 23 Sample 3 wrinkling
Figure 24 sample 9 showing the collecting of the larger wood particles
27
Figure 25 Graph of tensile strength against tensile extension for samples 7-12
Figure 22 shows the tensile test results for samples 7-12 which were foamed using sodium bicarbonate.
The sample with the highest tensile strength is sample 8 with tensile strength 8.27 MPa. Comparing this
to the result for sample 1 which has a tensile strength of 6.18 MPa. This result is due to the more
uniform foaming of the polyethylene which is shown in the SEM analysis.
Sample 9 had a tensile strength of 3.5 MPa which is lower than sample 3 with a tensile strength of 4.82
MPa. This result may be due to the fact that sodium bicarbonate is used for foaming of rubber which
means that both the polyethylene and the rubber may have foamed in sample 8 which would reduce its
tensile strength.
Comparing sample 9 to the control sample shows that sodium bicarbonate has significantly reduced the
tensile strength of the material. The addition of the zinc oxide will have made the foaming more violent
and could have been responsible for the large voids which are clearly visible in the SEM analysis. As
with samples 1-6, samples 7-12 also had wrinkling which was more common in the samples which were
allowed to cool slowly to room temperature overnight. The samples left to cool overnight were samples
3, 6, 9 and 12.
Comparing samples 9-12, the results show that reducing the size of the wood flour particles increases
the tensile strength by approximately the same amount as reducing the size of the polyethylene pellets.
Reducing the size of both the polyethylene pellets and the wood flour shows the biggest improvement
in tensile strength. It should be noted that samples 10-12 were sieved to remove large clumps which are
larger than 500 microns in order to prevent the larger particles of wood from collecting together as
shown in figure 22.
28
4.2. Density
Table 5 Table of density and swelling results
mass change % Thickness swelling %

Sample Density
no. (Kg/m3) 24h 48h 7 Days 24h 48h 7 Days
1 915.97 3.89 4.33 7.68 -3.67 1.56 5.05
2 1005.69 0.24 0.32 1.61 -0.83 0.08 -1.29
3 996.02 1.34 1.24 2.11 -1.75 -1.37 2.29
4 1038.91 0.99 1.01 1.71 -1.43 -2.62 1.27
5 1000.81 1.74 1.73 3.16 0.94 0.71 3.76
6 983.61 2.23 1.25 2.44 0.62 0.54 3.92
7 1016.27 16.17 17.70 17.93 10.02 11.41 14.67

0.17 2.97
8 978.25 3.98 6.36 8.11 2.97
7.81 14.00
9 967.60 25.27 26.25 29.96 14.00
10 939.93 10.18 31.00 40.23 4.62 4.69 8.35
11 975.53 8.79 11.03 18.10 -0.07 4.56 11.38
12 1052.10 7.28 9.09 13.98 4.04 5.09 10.82
PE 926.02 0.31 0.03 0.78 -2.36 -1.77 0.34
Control 1006.77 1.79 1.05 1.52 0.48 0.08 3.42
29
Samples 1-6
1060
1040
1020
1000
980 Sample 1
Sample 2
Density Kg/m3
960 Sample 3
940 Sample 4
Sample 5
920 Sample 6
900
880
860
840
Figure 26 Density bar chart for samples 1-6
The above chart shows the densities of samples 1-6 which all contained 8% AZDC. Sample 1 and 2 are
control samples where sample 1 consists of 50% wood, 40% PE and no rubber and sample 2 consists of
no wood, 40% PE and 50% rubber with all other compositions being the same between the two
samples. The wood plastic composite had a density of 915.97 Kg/m3 and the rubber plastic composite
has a density of 1005.69 Kg/m3. This shows that increased rubber content in the sample will increase
the density of the composite.
Samples 3, 4, 5 and 6 have the same percentage mass compositions of all ingredients at 30% wood,
40% HDPE and 20% rubber content. Sample 3 has both the wood flour and the PE powder at its
original un-sieved size, sample 4 has sieved wood flour which has been sieved so that only particles of
wood in the size range 125-250 microns. Sample 5 has the original size wood flour but the polyethylene
pellets have been sieved so that only pellets smaller than 500 microns were used. Sample 6 has both the
sieved wood flour and the sieved HDPE.
The density of sample 3 is 996.02 Kg/m3 and the density of sample 4 is 1038.91 Kg/m3 this suggests
that reducing the size of the wood flour increases the density of the composite. The density of sample 5
is 1000.81 Kg/m3 which suggests that reducing the size of the PE flour will result in increased density
of the sample.
Sample 6 has a density of 983.61 Kg/m3 which is lower than that of sample 3, this suggests that when
the particle sizes of both the wood flour and the PE is reduced, the density of the Composite is slightly
reduced.
30
Samples 7-12
1080
1060
1040
1020 Sample 7
Sample 8
1000
Sample 9
Density Kg/m3
980 Sample 10
960 Sample 11
Sample 12
940
Control Sample
920 PE Sample
900
880
860
Figure 27 Density bar chart for samples 7-12 including control and PE sample
The chart above shows the density results for samples 7-12 which have 8% Sodium Bicarbonate and
also for a pure polyethylene sample and the control sample which has the same mass fractions as
samples 3-6 and 9-12.
Sample 7 has a density of 1016.27 Kg/m3 and sample 8 has a density of 978.25 Kg/m3 this suggests that
in the case of using sodium bicarbonate as a foaming agent, an increased quantity of rubber as a
substitute for wood flour will result in reduced density. Comparing sample 1 to sample 7 shows that the
density was higher for sample 7 which suggests that AZDC has a greater foaming effect on
polyethylene than the Sodium Bicarbonate. Comparing sample 2 to sample 8 shows that sample 2 had
higher density than sample 8 which suggests that Sodium Bicarbonate is a better foaming agent on
rubber. These results are in line with what is expected as AZDC not often used for the foaming of
rubber whereas the use of Sodium bicarbonate as a foaming agent is more common practice.
Samples 9, 10, 11 and 12 have the same percentage mass compositions of all ingredients at 30% wood,
40% HDPE and 20% rubber content. Sample 9 has both the wood flour and the PE powder at its
original un-sieved size, sample 10 has sieved wood flour which has been sieved so that only particles of
wood in the size range 125-250 microns. Sample 11 has the original size wood flour but the
polyethylene pellets have been sieved so that only pellets smaller than 500 microns were used. Sample
12 has both the sieved wood flour and the sieved HDPE.
Sample 9 has a density of 967.60 Kg/m3 and sample 10 has a density of 939.93 Kg/m3 this suggests that
the reduced size of wood flour particles will reduce the density of the resulting composite when sodium
bicarbonate is used as a foaming agent. Sample 11 has a density of 975.53 Kg/m3 meaning that in this
case there was little change in the density when reducing the size of the polyethylene particles. Sample
12 has a density of 1052.10 Kg/m3 meaning that reducing the size of both wood flour particles and PE
particles results in increased density. The density of the control sample was 1006.77 Kg/m3. Samples 9
and 3 had the same mass fraction distribution and particle size range as the control sample and both
showed a lower density than the un-foamed control sample. Sample 3 being 1.07% lighter and sample 9
being 3.89% lighter.
31
4.3 Mass change Figure 28 Graphs of mass change over time for samples 1-8
1 2
10 3.5
3
8
Mass change (%)
Mass change (%)

2.5
6 2
4 1.5
1
2
0.5
0 0
0 50 100 150 200 0 50 100 150 200
Time (hours) Time (hours)
3 4
2.5 2.5
Mass change (%)
2 2
1.5 Mass change (%) 1.5
1
1
0.5
0.5
0
0 50 100 150 200 0
Time (hours) 0 50 100 150 200
Time (hours)
5 6
4 3
Mass change (%)
Mass change (%)
2.5
3
2
2 1.5
1
1
0.5
0 0
0 50 100 150 200 0 50 100 150 200
7 Chart 8
20 20
Mass change (%)
15 15
10
10
5
5
0
0 50 100 150 0
Time (hours) 0 50 100 150 200
-5
32
Figure 29 Graphs of mass change over time for samples 9-12, the control sample and PE sample
Chart 9 10
50 80
Mass change (%)

40 60
30 40
20 20
10 0
0 50 100 150 200
0 -20
0 50 100 150 200 Time (hours)
11 12
25 20
Mass change (%)
Mass change (%)

20 15
15
10
10
5 5
0 0
0 50 100 150 200 0 50 100 150 200
PE Sample Control Sample

2 3
Mass change (%)
2.5
Mass change (%)
1.5
2
1 1.5
1
0.5
0.5
0 0
0 50 100 150 200 0 50 100 150 200
-0.5
The graphs above show the mass change results for 3 test pieces for each of the 14 samples. These are
significant as they show where results are consistent and therefore more likely to be reliable or
inconsistent and therefore unreliable. Samples 1, 2, 3, 4, 5, 7, 10, 11 and 12 are reliable as they follow
the expected curve for mass change due to moisture absorption but samples 6, 8, 9, PE and the control
sample are not reliable as they have negative values which should not occur. Some of the graphs
showed reductions in mass because it was very difficult to dry the samples to the same degree each time
when they were removed from the water bath. This meant that sometime the samples had more or less
water on the surface which introduced the inconsistency in the mass measurements.
33
The density results ranged from 915.97 Kg/m3 to 1052.10 Kg/m3, The composites made using Sodium
bicarbonate as a foaming agent tended to have lower density than those made using AZDC as a foaming
agent. This is due to the fact that sodium bicarbonate can be used for foaming of both polyethylene as
well as rubber. The samples with the larger wood fractions tended to have the lowest density as wood is
the lowest density constituent material used in the composite. According to Anatole 2007, the higher
plastic content composites will have a lower density, this cannot be put to the test in this case as all
samples had the same HDPE content, however the density of the pure polyethylene sample (926.02
Kg/m3) shows that it has a lower density than all of the combined samples excluding sample 1.
The moisture absorption in composites should increase with the increase in wood content and samples 1
and 7 which both consist of 50% wood flour both showed large mass changes with sample 1 having the
largest mass change for samples 1-6 at 24 hours, 48 hours and 7 days and sample 7 showing the second
largest mass change after 24 hours. However Samples 9, 10 and 11 displayed the largest mass changes
overall after 7 days at 21.47%, 40.3% and 18.1% respectively.
According to Stokke 2003, the moisture absorption in the composites is mainly due to the presence of
lumens, fine pores and hydrogen bonding sites in the wood flour, the gaps and flaws in the interfaces
and the micro-cracks in the matric formed during the compounding process. This would explain the
smallest moisture absorption being displayed by the pure polyethylene sample. The number of water
residence sites increases with an increased wood content therefore more water is absorbed.
Santiago et al 2011 explains that natural fibres are highly hydrophilic due to the hydroxyl group of
polysaccharides found in the cellulose, which are able to form hydrogen bonds between water and the
fibre. This is supported by Razavi et al 2006 who sates that, as the filler content in a composite
increased, the number of OH groups on the lignocellulose fibres increases. Through hydrogen bonding,
free OH groups come in contact with water which results in water uptake and weight gain in the
composites.
The same trend was followed by the thickness swelling results whereby the samples with the highest
wood content displayed the largest swelling. With sample 1 which has 50% wood content displayed a
swelling of 5.05% at 7 days which is the highest for samples 1-6 and sample 7 which also has a 50%
wood content showing a swelling of 14.67% at 7 days which is the highest overall swelling of all the
samples. However this swelling occurred more slowly than in some of the other samples with sample 9
having a higher thickness swelling value than sample 7 after 48 hours.
Zhang et al 2008, states that the thickness swelling is an indicator of the internal bond strength of the
composite. This would indicate that sample 2, 3, 4 and 5 have the highest internal bond strength.
Rebollar et al 2005, suggests that in order to increase the performance of the composite in thickness
swelling tests, the addition of water repellent or an increase in the resin content would be good options.
Comparing the thickness swelling results from the control sample and those from samples 3 and 9
which have the same composition, the control sample shows a swelling of 3.42% where sample 9 has a
swelling of 14% and sample 3 has a swelling of 2.29%. This means that the addition of the AZDC has
actually increased the strength of the internal bonding in the material. The Sodium bicarbonate
however has decreased the strength of the internal bonding causing an increase in swelling from 3.42%
to 14%.
34
4.4 SEM Results
Figure 30 Sample 1 SEM images
The above images show the SEM micrograph images taken of sample 1 which has 50% wood flour
content, 40% HDPE content and is using AZDC as the foaming agent. The dispersion of the materials is
good with little clustering of the wood flour particles. Some small voids approximately 50microns in
diameter are visible in the sample possibly caused by trapped air when the sample is pressed. The
surface of the Polyethylene in the sample is packed with small bubbles approximately 4 microns in
diameter which are a result of the foaming agent. The interface between the wood and the polyethylene
has got some gaps which indicates that the interfacial adhesion is weak.
35
The above images show the SEM analysis images for sample 2 which contained 50% rubber and 40%
HDPE with AZDC as the foaming agent. This sample has three clearly visible large voids with a width
of between 200 and 400 microns and length of 400-800 microns. There are no visible voids on the
interface between the rubber and HDPE meaning that interfacial bonding was good. There are also no
visible bubbles on the rubber but there are bubbles on the HDPE which are unevenly spread and vary in
size. The presence of large voids means we would expect a large mass increase when submerged in
water but these voids are so large that the absorbed water will seep out when the sample is removed
from the water meaning that the increased mass won’t be reflected in the results shown previously.
36
The above image shows the SEM images for sample 3. Sample 3 consisted of 30% wood flour, 40%
HDPE powder and 20 % rubber powder and AZDC as the foaming agent. The particle distribution in
this sample is uneven with areas with clusters of rubber and wood. This sample has many uneven voids
of varying sizes. The polyethylene has large amounts of bubbling with bubbles ranging in size from 2-8
microns. The interface between the plastic and rubber has gaps in some areas meaning that the
interfacial adhesion is not good.
37
HDPE powder and 20 % rubber powder and AZDC as the foaming agent. This sample was made using
sieved wood flour particles between 125 and 500 microns. This sample has many voids in the size range
50-200 microns. The bubbling of the HDPE is very uneven and the size of the foamed bubbles is
ranging from 2 microns to 20 microns. The particle dispersion is quite uneven with clusters of wood
and rubber particles and areas where there is just polyethylene.
38
sieved powder of polyethylene where the powder particles are all smaller than 500 microns. The finer
polyethylene particles have produced a more even void distribution than sample 3 and 4 and the voids
are smaller at between 1 and 5 microns. The surface adhesion is also good as there doesn’t appear to be
a gap between the polyethylene and the rubber or wood particles.
39
Figure 35 Samples 6 SEM images
the wood flour particles in the size range 125-500 microns and the polyethylene particles smaller than
500 microns. The particle dispersion is very uneven in this sample with large clusters of wood fibres.
The surface of the polyethylene is quite evenly foamed and the bubbles are approximately in the range
from 1 to 8 microns.
40
HDPE powder and sodium bicarbonate as the foaming agent. This sample has many clearly visible
large voids which appear to be interconnected. This explains that it has the largest moisture absorption
of all the samples after 7 days of submersion. The dispersion of the wood fibres is uneven but the
foaming of the HDPE is more even than in sample 1 and the bubbles are also smaller ranging between 1
and 5 microns. The interfacial bonding is good for this sample as there doesn’t appear to be a gap
between the weed fibres and the HDPE.
41
The above image shows the SEM images for sample 8. Sample 8 consisted of 40% HDPE powder and
50 % rubber powder and sodium bicarbonate as the foaming agent. This sample doesn’t have the very
large voids that sample 2 does. The particle size distribution is even and the foaming of the HDPE is
also even. The interfacial adhesion is not very good as there are clearly visible gaps between the two
samples.
42
HDPE powder and 20 % rubber powder and sodium bicarbonate as the foaming agent. Sample 9 has a
very large void almost the same size as the thickness of the sample. This void was caused by bad
particle distribution and a lot of wood particles being clustered together there are several areas where
pieces of wood and rubber have clustered together with little to no polyethylene between them
explaining why sample 9 has 29% mass change after 7 days of submersion.
43
HDPE powder and 20 % rubber powder and sodium bicarbonate as the foaming agent. Sample 10 was
made using the wood flour that was sized between 125 and 500 microns. And the result is a more even
distribution of the particles and a reduction in the number of large voids. Some voids are still present
and visible and the interface has gaps between the rubber and the HDPE.
44
HDPE powder and 20 % rubber powder and sodium bicarbonate as the foaming agent. This sample was
made with the rubber particles smaller than 500 microns. Sample 11 has many very large voids clearly
visible. The particle size distribution is uneven but the foaming of the HDPE is even and the bubbles are
very fine at between 1 and 5 microns.
45
HDPE powder and 20 % rubber powder and sodium bicarbonate as the foaming agent. Sample 12 was
made with the wood flour with particle size between 125 and 500 microns and HDPE with particle size
less than 500 microns. This sample showed some large voids but had better particle distribution. This
sample was sieved meaning that the particle sizes are more even. When compared to sample 6, sample
12 has more large voids but more even foaming on the HDPE.
46
Figure 42 Pure Polyethylene SEM images
She above image shows the SEM images for the pure polyethylene sample. This sample is very flat
with no voids. The surface structure is very different to the polyethylene in the foamed samples in that it
is not jutting out perpendicular to the surface. It is also evident that the microstructure of the
polyethylene is changed by the foaming agent as in the pure polyethylene sample a webbing can be seen
which is not present in the foamed samples.
47
Figure 43 Control Sample SEM images
She above image shows the SEM images for the control sample. This sample consists of 30% wood
flour, 40% HDPE powder and 20 % rubber powder but has no foaming agent. The surface of this
sample has much less large voids than the foamed samples and when looking at the higher zoom
images, it can be seen that the polyethylene has not formed bubbles but rather it has just surrounded the
small rubber and wood particles. This sample is likely to have better interfacial adhesion as there is
more surface area to make contact with the materials due to the lack of bubbles.
48
CHAPTER 5 CONCLUSION AND RECCOMENDATIONS
5.1. Limitations and recommendations

One major limitation is the unavailability of a cooling system on the hot press machine. This causes the
a pressure build-up during pressing. Vapour from the sample builds up on the surface of the sample and
becomes superheated. When the pressure is released the superheated moisture releases suddenly which
will affect the molten components of the composite. This can be resolved by the use of a heat press
machine which cools the sample prior to pressure release.
The use of a steel mould created some limitations during post processing curing of the sample as the
heat stored in the base, side walls and top plate created an uneven cooling process for the sample. The
top and bottom surfaces cooled faster than the sides prior to removal from the mould. This increased the
period of thermal action on the middle section of the sample and may have pre-stressed the sample
which would affect its behaviour in mechanical tests.
The rate of cooling will have also been influenced by the room temperature at the time as the samples
were made during a period of 5 days and on colder days the sample will have cooled faster than on hot
days. The differential cooling also meant that the high temperature release film on the top and bottom of
the sample would have cooled in different parts at different times, this causes the film to contract in
some areas and remain expanded due to residual heat in others, this is responsible for the wrinkling
effect caused on some of the samples as shown in figure 23. This issue could also have been resolved
by the use of a hot press machine with a built in cooling system.
Another limitation is the fact that the samples had to be pre mixed in spain due to the unavailability of
the barbender high temperature mixing machine on campus. This meant that only enough mixture for
one sample of each composition could be produced for testing. Making more samples of the same
composition would have made results more reliable and enabled the removal of outliers in the sample
making process.
The unavailability of an extrusion process in the Civil Laboratory of Brunel University meant that the
samples could not be produced using the method which is most likely to be used in mass manufacturing
of the end product.
The duration of the making process for the samples was a limitation as each sample required 30 min of
preheating, followed by 10 min of pressing and then finally 30 min of cooling. This coupled with the
fact that the hot press machine takes 35-45 min to get to the correct temperature meant that only 2-3
samples could be produced in a single day.
Pressing the sample only once meant that it was less likely that the sample was of uniform density and
thickness. Pre-pressing the sample during the mixing stage would have enabled an even density
distribution prior to the hot press stage which would have increased the consistency of the samples.
The unavailability of some foaming agents such as expancell meant that others which may not have
been as effective had to be used as a replacement. This could be rectified if there was more time
available to wait until the desired foaming agents became available.
49
5.2. Conclusions
The following conclusions can be drawn from the experiments conducted to investigate the foaming of
wood, rubber, plastic composites:
 The density of the samples foamed using azodicarbonamide ranged from 915.97 to 1038.91.
The density of the samples foamed using sodium Bicarbonate ranged from 939.93 to 1052.10.
The density of the control sample made using no foaming agent was 1006.77. This shows that
both foaming agents produced samples with lower density than the control sample however
they also produced samples which were shown to have higher density than the control sample
which is likely to be due to inconsistency in the manufacturing process. This also shows that the
azodicarbonamide was more effective in reducing the density of the samples than the sodium
bicarbonate.
 The tensile testing of the samples showed that samples foamed using azodicarbonamide had a
range of tensile strength from 3.98 MPa to 7.61 MPa and the samples foamed using sodium
bicarbonate had tensile strength ranging from 3.57 MPa to 8.27 Mpa. Which shows that
azodicarbonamide produced samples with tensile strength which is more consistent however it
also shows that samples foamed with sodium bicarbonate could produce samples of greater
tensile strength.
 The control sample had a tensile strength of 8.34MPa which means that both foaming agents
significantly reduced the tensile strength with samples made using azodicarbonamide as the
foaming agent showing the larger tensile strength reduction.
 SEM analysis of the samples showed that both azodicarbonamide and sodium bicarbonate
increased the number of voids in the samples in comparison with the control sample however,
the samples made using the sodium bicarbonate had higher uniformity in the foaming of the
polyethylene whilst simultaneously having a higher likelihood of producing samples which
have large voids.
50
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FOAMING OF RUBBER WOOD PLASTIC COMPOSITES (RUBWPC)

Elton Qafaliaj [1213525]

Supervisor: Professor Mizi Fan

Individual Dissertation submitted to the Department of Civil Engineering

School of Engineering and Design, Brunel University

Table 1 Composition of a tyre (WRAP) .................................................................................................... 6

Figure 1 Chemical structure of cellulose. .................................................................................................. 3

HDPE High Density Polyethylene

1.1. Composite Material History

Figure 1 Chemical structure of cellulose.

Figure 3 Chemical structure of a small piece of lignin polymer

1.3.1.4. Other extractives.

Figure 4 Cross-section of modern car tyre

Brief descriptions of the parts of a tyre:

Textile cord ply-

Controls internal pressure and maintains the tyres shape. [31]

Enhances directional stability and gives steering precision [31]

Steel cord for belt plies-

Table 1 Composition of a tyre (WRAP)

1.3.2.1.1. Synthetic rubber

1.3.3. Coupling agents

Figure 5 General formula for a silane coupling agent

 By improving the wettability of resins

1.3.3.2. Maleic Anhydride

Figure 7 Chemical formula of MaPE

1.3.4. Blowing agents

Depending on cell sizes foams are split into

 Macro cellular – Cell dimension > 100µm

Foaming occurs in three stages

 Formation of polymer/blowing agent solution/mixture

1.3.4.1 Sodium Bicarbonate (NaHCO3)

Hydrocerol decomposes at 170-220°C.

Figure 8 Chemical formula of AZDC

Expancel is the trademark of a foaming agent constituted by microspheres of polymethymethacrylate

1.3.4.4. (OBSH) 4, 4 Oxybis (benzenesulfonylhydrazide)

1.4. Problem Statement

1.5. Research Methodology

1.6. Research Objectives

2.2. Foaming of Wood rubber plastic composites

3.1. Raw Materials

3.1.1. Wood Fibre

Figure 9 Wood flour

Figure 10 Rubber powder

3.1.4. Coupling Agent

3.1.5 Foaming Agent

Figure 11 Heat press machine

Figure 12 High temperature release wax

Figure 13 Barbender high temperature mixing machine

Table 2 Initial experimental design

Sample Wood Wood HDPE PE size Rubber CFA CFA

3-1 50 Original 40 Original 0 8 0

CFA 1: azodicarbonamide, CFA 2: Sodium Bicarbonate

Table 3 Analysis techniques used in 40 previous papers

Figure 14 Samples 1-7

As defined in BS EN 323-1993 Density is;

Length and width measurement -

Figure 17 Axes layout of the samples

3.5.2. Tensile Strength

Figure 19 Instron testing machine

Equation 2 Tensile strength

3.5.3 Scanning Electron Microscopy

Figure 21 Gold coating machine

3.5.4.4. Test piece preparation