Electrical and Mechanical Properties of Banana Fiber Reinforced Polyester Composites

ELECTRICAL AND MECHANICAL PROPERTIES OF
BANANA FIBER REINFORCED POLYESTER

COMPOSITES
M. PHIL. THESIS
RANI NASRIN
Roll No. 100714016
Session: October, 2007
BUET
DEPARTMENT OF PHYSICS
BANGLADESH UNIVERSITY OF ENGINEERING & TECHNOLOGY
DHAKA, BANGLADESH
MARCH, 2013
ELECTRICAL AND MECHANICAL PROPERTIES OF
BANANA FIBER REINFORCED POLYESTER
COMPOSITES
A THESIS SUBMITTED TO THE DEPARTMENT OF PHYSICS, BANGLADESH

UNIVERSITY OF ENGINEERING AND TECHNOLOGY (BUET), DHAKA, IN
PARTIAL FULFILLMENT OF THE REQUIREMENT FOR THE DEGREE OF
MASTER OF PHILOSOPHY (M. PHIL.) IN PHYSICS
by
RANI NASRIN
Roll No. 100714016 P
Session: October, 2007
BUET
BANGLADESH UNIVERSITY OF ENGINEERING & TECHNOLOGY
DHAKA, BANGLADESH
MARCH, 2013
BANGLADESH UNIVERSITY OF ENGINEERING & TECHNOLOGY (BUET), DHAKA
Certification of Thesis Work
The thesis titled “ELECTRICAL AND MECHANICAL PROPERTIES OF BANANA

FIBER REINFORCED POLYESTER COMPOSITES” submitted by RANI NASRIN, Roll
No. 100714016 P, Session: October/2007, has been accepted as satisfactory in partial fulfillment
of the requirement for the degree of Master of Philosophy (M. Phil.) in Physics on 23 March,
2013.
BOARD OF EXAMINERS
1. _______________________________
DR. MD. ABU HASHAN BHUIYAN (Supervisor) Chairman
Professor, Department of Physics
BUET, Dhaka
2. _______________________________
DR. MD. ABDUL GAFUR (Co-supervisor) Member
Senior Engineer
BCSIR, Dhaka
3. _______________________________
DR. MD. MOSTAK HOSSAIN (Ex-Officio) Member
Professor and Head, Department of Physics
BUET, Dhaka
4. _______________________________
DR. A. K. M. AKTHER HOSSAIN Member
Professor, Department of Physics
BUET, Dhaka
5. _______________________________
DR. MD. TOFAZZAL HOSSAIN Member (External)
Chief Scientific Officer
BCSIR, Dhaka
BUET
CANDIDATE’S DECLARATION
It is hereby declared that this thesis or any part of it has not been submitted elsewhere for
the award of any degree or diploma.
___________________
(RANI NASRIN)
Roll No. 100714016 P
Session: October/2007
Dedicated
To
My beloved husband
ACKNOWLEDGMENT
I am extremely delighted to express my indebtedness and deepest sense of gratitude to my
reverend teacher Dr. Md. Abu Hashan Bhuiyan, Professor, Department of Physics, BUET,
Dhaka for his supervision, continuous guidance, valuable suggestions, and help that inspired me
to complete this research work.
I express my deepest sense of gratitude and profound respect to my co-supervisor Dr. Md. Abdul
Gafur, Senior Engineer, PP and PDC, BCSIR, Dhaka, for his invaluable time dedication, close
supervision and helpful attitude provided during the work. I like to thank the chairman of BCSIR
for providing their all the facilities of this department unboundedly.
I am grateful to my respected teacher Prof. Dr. Md. Mostak Hossain, Head, Department of
Physics, BUET, for providing necessary facilities to carry out this research work. I am thankful
to my respectable teacher Dr. Md. Forhad Mina, Associate professor, for his valuable
suggestions regarding my thesis.
My deep sense of gratitude is due also to Prof. Dr. Mominul Huq, Prof. Dr. Nazma Zaman, Prof.
Dr. Jiban Podder, Prof. Dr. Md. Feroz Alam Khan, and Prof. Dr. A. K. M. Akther Hossain of the
same department for their encouragement during this work.
I like to thank all teachers of the Department of physics, BUET, Dhaka, for their kind help and
regarding this research work.
I am also grateful to Prof Dr. Syed Jamal, Department of Physics, DUET, Gazipur, for his
valuable comments and keen interest in my work. I would like to express my thanks to Mr. Md.
Rakibul Qadir, Engineer, PP and PDC, BCSIR, Dhaka, for his cordial help during this work.
I also offer my thanks to all the staff members Mr. Md. Idris Munshi, Mr. Md. Liaquat Ali, Mr.
Md. Nurul Haque, Mr. Md. Lutfar Rahman Sarker, Mr. Swapan Kumar Das, Mr. Md.
Muzammel Haque, and Mr. Md. Abu Taher, Department of Physics, BUET, Dhaka, for their
sincere help.
I would like to express my gratitude to my sweet daughter Jarin Roshni and my sweet son Rashik
Rahman for their sacrifice, my beloved husband Prof. Dr. A. T. M. Kaosar Jamil, Department of
Physics, DUET, Gazipur, who inspired me to continue my work. Thanks to my parents and to my
brother and all other family member for being so patient, caring, and keeping my spirits up.
Without them I could not have done this work.
Finally, I am grateful to almighty Allah for giving me strength and opportunity to complete my
thesis work successfully.
ABSTRACT
Banana fiber is a one of the natural fibers with growing interest as a reinforcing agent in
thermosetting polyester resin. Banana fibers were collected from local area and extracted from
banana tree by rotting. Raw banana fibers and fibers treated with 5% NaOH solution were used to
prepare composites as reinforcement in polyester resin matrix with different weight percentage
(wt%) of fiber loading by a simple hand lay-up press molding process. The effects of NaOH
treatment and fiber adhesion in composites on its physical, mechanical, electrical, thermal and
structural properties were investigated. It is found that the bulk density of untreated (raw) banana
fiber-polyester resin composites decreases with the increase of fiber content. The density of treated
samples is higher than that of untreated sample and always improved on treatment of fiber with 5%
NaOH solution at longer times. The water absorption of the composites is increased with the increase
of fiber loading indicating diffusion phenomenon. But the water absorption rate is decreased with the
increase of NaOH treatment time. The treatment of fiber is thought to have changed fiber
morphology and removed hemicellulose and other soluble matters from its surface and might have
increased the crystallinity index percentage of cellulose.
It is observed that the tensile strength of banana fiber-polyester resin composites decreases during the
initial stage of fiber loading which indicates that the load is not properly transmitted to the fibers and
increases with the increase of fiber loading from 5%. The Young’s modulus of composites increases
with the increase of fiber addition. The flexural strength of these composites is decreased with the
increase of fiber addition up to 10% and then increases with composition. At lower addition of fiber,
the interfacial bonding is poor due to presence of lignin, fatty, and waxy materials. In further addition
of fiber (20%), both the fiber and matrix bear the load and make good interfacial bonding between
the fiber and matrix. The tensile strength, Young’s modulus, flexural strength, and flexural modulus
of the composites are improved with the increase of NaOH treatment time. This suggests that due to
treatment of fibers with alkali, the interfacial strength might have slightly increased and aided
mechanical interlocking between the fiber and matrix.
AC conductivity (σac) is increased linearly with the frequency of the applied signal with lower slope
in the low frequency region (up to 105 Hz) and higher slope in the high frequency region (>105 Hz).
The observed frequency dependent of σac indicates that the mechanism of carrier conduction is due to
hopping of charge carriers between the localized states. The dielectric constant (έ) is decreased with
increasing frequency and increased with increasing temperature. This constant is decreased sharply at
low frequency (100 – 900 Hz) region and smoothly decreased at high frequency region. At lower
frequency the value of dielectric constant is much high as compare to higher frequency indicating
ionic effect. All specimens exhibit a normal dielectric behavior of materials, which may be due to the
interfacial polarization. There is a big dip observed in the loss tangent (tanδ) behavior. The dip is
found to maximum at around 100 kHz. The loss tangent gradually decreases with increasing
frequency up to 100 kHz and after that it increases sharply with increasing frequency. The σac, έ, and
tanδ are decreased with the increasing fiber content and NaOH treatment time. It may happen
because of the oxygen vacancy, hydroxyl ion motion or interfaces between the fiber and matrix.
Mass loss profile of TG/DTA/DTG of banana fibers changes considerably when they are treated with
NaOH solution. On treatment with alkali, mass loss (%) in major degradation region is decreased
with an increase in amount (%) of final residual mass (carbonaceous char). Major degradation stage,
maximum degradation rate, and endothermic peak of composites shifts towards higher temperature as
compare to resin sheet and fibers. The banana fibers-polyester resin composites are thermally more
stable than that of fibers and polyester resin.
The observed FTIR spectra of banana fiber and composites are characterized of lignocellulosic fiber,
which consists of the primary components: cellulose, hemicellulose, and lignin. The vibrational
modes after NaOH treatment did not suffer significant changes and the main bands appeared
approximately in the same range of the wave numbers.
Chapter 1: Introduction
1.1 Introduction
1.2 Objective of the Present Study
1.3 Outline of this Thesis
1.4 Summary of this Thesis
References
Chapter 2: Literature Review
2.1 Review of the Earlier Research Works

2.1.1 Study of chemical modification of natural fibers
2.1.2 Study of banana fiber reinforced polymer composites
2.1.3 Study of other natural fiber reinforced polymer composites
References
Chapter 3: Theoretical Background
3.1 Polymer
3.1.1 Classification of polymers
3.1.2 Polymerization
3.1.3 Polymer properties
3.2 Natural Fiber
3.2.1 Structure and occurrence of natural fibers
3.2.2 Classification of fibers
3.2.3 Banana fibers
3.2.4 Chemical composition of natural fibers
3.2.5 Physico-mechanical properties of natural fibers
3.2.6 Chemical properties of natural fibers
3.2.7 Chemical modification of natural fibers
3.3 Polymer Composite
3.3.1 Plastic and composite materials
3.3.2 Classification of composite materials
3.3.3 Principles of fiber reinforcement
3.3.4 Stress-strain relationship
3.3.5 Manufacturing routes for fiber reinforced plastics
3.3.6 Deformation of materials
3.3.6.1 Elastic deformation
3.3.6.2 Plastic deformation
3.3.7 Characteristic parameters of composites materials
3.3.7.1 Critical volume fraction
3.3.7.2 Tensile strength
3.3.7.3 Ultimate tensile strength
3.3.7.4 Elastic modulus
3.3.7.5 Toughness
3.3.8 Application of composite materials based on plastics
3.4 Electrical Properties of Polymer Composites
3.4.1 Conduction mechanism in solid
3.4.2 Theory of Dielectrics
3.4.2.1 Dielectric polarization and its classification
3.4.2.2 Dielectric loss
3.4.2.3 The Debye theory of dielectrics
3.4.2.4 Dielectric nature of the polymer composites
3.5 Theory of Thermal Analysis
3.5.1 Differential thermal analysis
3.5.2 Thermogravimetric analysis
3.5.3 Differential thermogravimetry
3.6 Theory of Infrared Spectroscopy
3.6.1 Infrared frequency range and spectrum presentation
3.6.2 Infrared absorption
References
Chapter 4: Materials and Methods
4.1 Materials
4.1.1 Raw materials
4.2 Methods for Preparation of Banana Fibers
4.2.1 Collection and separation of fiber from their plants
4.2.2 Scouring of the fiber
4.3 Methods for Preparation of Composites
4.3.1 Treatment of fiber with NaoH
4.3.2 Fiber cutting
4.3.3 Hand lay-up
4.3.4 Casting
4.4 Methods for Measuring Physical and Mechanical Properties
4.4.1 Equipments used for the testing of samples (Physical and Mechanical)
4.4.2 Measurement of bulk density
4.4.3 Water absorption/water intake
4.4.4 Tensile properties
4.4.5 Flexural properties
4.5 Methods for Measuring Electrical Properties
4.5.1 Instrument used for electrical measurements
4.5.2 AC electrical measurements for conductivity and dielectrics
4.6 Methods for Measuring Thermal Properties
4.6.1 Procedure of thermal analysis
4.6.2 Thermal analysis of banana fibers and composites
4.7 Methods for Measuring Structural Properties
4.7.1 Fourier transform infrared spectroscopy
References
Chapter 5: Results and Discussion
5.1 Physical Properties of Composites

5.1.1 Bulk density calculation
5.1.2 Water absorption/Water intake
5.2 Mechanical Properties of Composites
5.3 Electrical Measurements
5.3.1 Variation of AC conductivity with frequency
5.3.2 Variation of AC conductivity with temperature
5.3.3 Variation of dielectric constant with frequency
5.3.4 Variation of dielectric loss tangent with frequency
5.4 Thermal Analysis
5.4.1 Thermal analysis of polyester resin sheet
5.4.2 Thermal analysis of untreated banana fiber
5.4.3 Thermal analysis of NaOH treated banana fiber
5.4.4 Thermal analysis of untreated banana fiber-polyester resin composites
5.4.5 Thermal analysis of NaOH treated banana fiber-polyester resin composites
5.5 Structural Analysis
5.5.1 Infrared spectroscopy analysis
5.6 Summary of this Chapter
References
Chapter 6: Conclusions
6.1 Conclusions
6.2 Suggestions for future works
M. Phil. Thesis RANI NASRIN March, 2013
CONTENTS
Page
Chapter 1: Introduction (1–9)
1.1 Introduction 1
1.2 Objective of the Present Study 7
1.3 Outline of this Thesis 7
1.4 Summary of this Thesis 7
References 9
Chapter 2: Literature Survey (10–23)

2.1 Review of the Earlier Research Works 10
2.1.1 Study of chemical modification of fibers 10
2.1.2 Study of banana fibers reinforced polymer composites 12
2.1.3 Study of other fibers reinforced polymer composites 16
References 22
Chapter 3: Theoretical Background (24–79)

3.1 Polymer 24
3.1.1 Classification of polymers 24
3.1.2 Polymerization 27
3.1.2 Polymer properties 29
3.2 Natural Fiber 32
3.2.1 Structure and occurrence of natural fibers 34
3.2.2 Classification of fibers 35
3.2.3 Banana fibers 37
3.2.4 Chemical composition of natural fibers 38
3.2.5 Physico-mechanical properties of natural fibers 43
3.2.6 Chemical properties of natural fibers 44
3.2.7 Chemical modification of natural fibers 45
3.3 Polymer Composite 46
3.3.1 Plastic and composite materials 46
3.3.2 Classification of composite materials 48
3.3.3 Principles of fiber reinforcement 51
3.3.4 Stress-strain relationship 52
3.3.5 Manufacturing routes for fiber reinforced plastics 53
3.3.6 Deformation of materials 55
3.3.6.1 Elastic deformation 55
3.3.6.2 Plastic deformation 55
i
3.3.7 Characteristic parameters of composites materials 57
3.3.7.1 Critical volume fraction 57
3.3.7.2 Tensile strength 58
3.3.7.3 Ultimate tensile strength 58
3.3.7.4 Elastic modulus 58
3.3.7.5 Toughness 59
3.3.8 Application of composite materials based on plastics 60
3.4 Electrical Properties of Polymer Composites 61
3.4.1 Conduction mechanism in solid 61
3.4.2 Theory of Dielectrics 62
3.4.2.1 Dielectric polarization and its classification 63
3.4.2.2 Dielectric loss 65
3.4.2.3 The Debye theory of dielectrics 66
3.4.2.4 Dielectric nature of the polymer composites 68
3.5 Theory of Thermal Analysis 69
3.5.1 Differential thermal analysis 69
3.5.2 Thermogravimetric analysis 71
3.5.3 Differential thermogravimetry 72
3.6 Theory of Infrared Spectroscopy 72
3.6.1 Infrared frequency range and spectrum presentation 73
3.6.2 Infrared absorption 73
References 76
Chapter 4: Materials and Methods (80–99)

4.1 Materials 80
4.1.1 Raw materials 80
4.2 Methods for Preparation of Banana Fibers 81
4.2.1 Collection and separation of fiber from their plants 81
4.2.2 Scouring of the fiber 82
4.3 Methods for Preparation of Composites 82
4.3.1 Treatment of fiber with NaoH 82
4.3.2 Fiber cutting 82
4.3.3 Hand lay-up 82
4.3.4 Casting 83
4.4 Methods for Measuring Physical and Mechanical Properties 84
4.4.1 Equipments used for the testing of samples (Physical and Mechanical) 84
4.4.2 Measurement of bulk density 85
4.4.3 Water absorption/water intake 85
4.4.4 Tensile properties 86
ii
4.4.5 Flexural properties 89
4.5 Methods for Measuring Electrical Properties 92
4.5.1 Instrument used for electrical measurements 92
4.5.2 AC electrical measurements for conductivity and dielectrics 94
4.6 Methods for Measuring Thermal Properties 96
4.6.1 Procedure of thermal analysis 96
4.6.2 Thermal analysis of banana fibers and composites 97
4.7 Methods for Measuring Structural Properties 97
4.7.1 Fourier transform infrared spectroscopy 97
References 99
Chapter 5: Results and discussion (100–137)

5.1 Physical Properties of Composites 100
5.1.1 Bulk density calculation 100
5.1.2 Water absorption/Water intake 102
5.2 Mechanical Properties of Composites 104
5.2.1 Tensile properties 105
5.2.2 Flexural properties 109
5.3 Electrical Measurements 111
5.3.1 Variation of AC conductivity with frequency 111
5.3.2 Variation of AC conductivity with temperature 115
5.3.3 Variation of dielectric constant with frequency 117
5.3.4 Variation of dielectric loss tangent with frequency 120
5.4 Thermal Analysis 122
5.4.1 Thermal analysis of polyester resin sheet 123
5.4.2 Thermal analysis of untreated banana fiber 124
5.4.3 Thermal analysis of NaOH treated banana fiber 126
5.4.4 Thermal analysis of untreated banana fiber-polyester resin composites 127
5.4.5 Thermal analysis of NaOH treated banana fiber-polyester resin composites 129
5.5 Structural Analysis 131
5.5.1 Infrared spectroscopy analysis 131
5.6 Summary of this Chapter 133
References 136
Chapter 6: Conclusions (138–139)

6.1 Conclusions 138
6.2 Suggestions for future works 139
iii
LIST OF FIGURES
Fig. 3.1: Classification of natural fibers which can be used as reinforcements or 35
fillers in polymers.
Fig. 3.2: Banana plant. 38
Fig. 3.3: Structure of cellulose. 39
Fig. 3.4: Hydrogen bonding in adjacent chains. 40
Fig. 3.5: The structure of the repeating unit of jute hemicellulose 3-methylxy 41
galactouronic acid linked with xylose units.
Fig. 3.6: Structure of lignin. 42
Fig.3.7: Axial deformation due to the load (p) in a composite reinforced with 52
continuous cylindrical fibers.
Fig. 3.8: Schematic illustration of (a) elastic deformation and (b) plastic deformation. 56
Fig. 3.9: Parallel plate capacitor (AC case). 62
Fig. 3.10: Dispersion of molar polarization in a dielectric (schematic). 64
Fig. 3.11: AC losses in a dielectric: (a) circuit diagram, and (b) simplified diagram of 65
current voltage relationship.
Fig. 3.12: Debye dielectric dispersion curves. 67
Fig. 3.13: Schematic diagrams showing different parts of a DTA apparatus. 70
Fig. 3.14: A pictorial set-up for TGA measurements. 71
Fig. 3.15: Stretching and bending vibrations. 75
Fig. 4.1: Raw banana fiber extracted from banana plants. 81
Fig. 4.2: Photograph of UTM machine. 84
Fig. 4.3: Typical tensile load Vs displacement curve. 88
Fig. 4.4: Typical flexural test set-up for polymer composites. 89
Fig. 4.5: Schematic diagram of specimen chamber. 93
Fig. 4.6: Photographs of the specimen chamber and holder. 94
Fig. 4.7: AC electrical measurement set-up. 95
Fig. 4.8: TG/DTA 6300. 97
Fig. 4.9: Double beam FTIR spectrophotometer. 98
Fig. 5.1: Effect of fiber addition on density for the samples of (a) untreated banana 101
fiber-polyester resin composites and (b) 5% NaOH treated (for different
hours) banana fiber-polyester resin composites.
Fig. 5.2: Effect of soaking time on water absorption of different % of fiber content of 102
(a) untreated banana fiber-polyester resin composites and (b) 5% NaOH
treated (for five hours) banana fiber-polyester resin composites.
iv
Fig. 5.3: Effect of soaking time on water absorption of untreated and treated (for 103
different hours) banana fiber-polyester resin composites of 5% of fiber
content.
Fig. 5.4: Stress-strain curves (before toe correction) of composites as obtained from 104
QMat professional software.
Fig. 5.5: Effect of fiber addition on tensile strength of (a) untreated banana fiber- 105
polyester resin composites and (b) 5% NaOH treated (for different hours)
banana fiber-polyester resin composite.
Fig. 5.6: Effect of fiber addition on Young’s modulus of untreated and NaOH treated 106
(for different hour) banana fiber-polyester resin composites.
Fig. 5.7: Effect of fiber addition on tensile energy of untreated and treated (for 108
different hour) banana fiber-polyester resin composites.
Fig. 5.8: Effect of fiber addition on flexural strength of untreated and treated (for 109
different hour) banana fiber- polyester resin composites.
Fig. 5.9: Effect of fiber addition on flexural modulus of untreated and treated (for 110
different hour) banana fiber- polyester resin composites.
Fig. 5.10: AC conductivity as a function of frequency curves of untreated banana 112
fiber-polyester resin composites of 5% fiber content taken at (a) 300 K in
air and vacuum atmosphere and (b) 300, 323, 348 and 373 K in vacuum
atmosphere.
Fig. 5.10: AC conductivity as a function of frequency curves taken at different 112
temperature of banana fiber-polyester composites of 10% fiber content
treated with NaOH for (c) two hours and (d) five hours.
Fig. 5.10: AC conductivity as a function of frequency curves of treated banana fiber- 113
polyester composites with NaOH for different hours of 5% fiber content
taken at (e) 300 K and (f) 373 K.
Fig. 5.10: AC conductivity as a function of frequency curves of treated banana fiber- 113
polyester composites with NaOH for five hours of 5%, 10% and 20% fiber
content taken at (g) 300 K and (h) 373 K.
Fig. 5.11: AC conductivity as a function of temperature curves taken at different 115
frequency of banana fiber-polyester composites of 5% fiber content treated
with NaOH for (a) one hour and (b) five hours.
Fig. 5.12: Dielectric constant as a function of frequency curves of untreated banana 117
fiber-polyester resin composites of 5% fiber content taken at (a) 300 K in
air and vacuum atmosphere and (b) 300, 323, 348 and 373 K in vacuum
atmosphere.
Fig. 5.12: Dielectric constant as a function of frequency curves taken at different 118
temperatures of treated banana fiber-polyester composites with NaOH for
five hours of (c) 10% fiber content and (d) 20% fiber content.
Fig. 5.12: Dielectric constant as a function frequency curves of treated banana fiber- 119
polyester composites with NaOH for different hours of 5% fiber content
v
taken at (e) 300 K and (f) 373 K.
Fig. 5.12: Dielectric constant as a function frequency curves of treated banana fiber- 119
polyester composites with NaOH for five hours of 5%, 10% and 20% fiber
content taken at (g) 300 K and (h) 373 K.
Fig. 5.13: Dielectric loss tangent as a function of frequency curves of untreated 120
banana fiber-polyester resin composites of (a) 5% fiber content taken at 300
K with air and vacuum atmosphere and (b) 10% fiber content taken at 300,
323, 348 and 373 K with vacuum atmosphere.
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of banana fiber- 121
polyester composites taken at different temperature treated with NaOH for
(c) one hour of 5% fiber content and (d) five hour of 10% fiber content.
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of treated banana 121
fiber-polyester composites with NaOH for different hours of 5% fiber
content taken at (e) 300 K and (f) 373 K.
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of treated banana 122
fiber-polyester composites with NaOH for five hours of 5%, 10% and 20%
fiber content taken at (g) 300 K and (h) 373 K.
Fig. 5.14: TG/DTA/DTG curves of polyester resin sheet. 123
Fig. 5.15: TG/DTA/DTG curves of untreated banana fiber. 125
Fig. 5.16: (a) TG/DTA/DTG curves of NaOH treated (for one hour) banana fiber. 126
Fig. 5.16: (b) TG/DTA/DTG curves of NaOH treated (for five hours) banana fiber. 126
Fig. 5.17: (a) TG/DTA/DTG curves of untreated banana fiber-polyester resin 128
composites of 5% fiber content.
Fig. 5.17: (b) TG/DTA/DTG curves of untreated banana fiber-polyester resin 128
Fig. 5.18: (a) TG/DTA/DTG curves of NaOH treated (for one hour) banana fiber- 129
polyester resin composites of 5% fiber content.
Fig. 5.18: (b) TG/DTA/DTG curves of NaOH treated (for five hours) banana fiber- 129
polyester resin composites of 5% fiber content.
Fig. 19: FTIR spectra of (a) untreated banana fiber (UBF), (b) untreated banana 131
fiber-polyester resin composite (UBF-PR), (c) treated banana fiber (TBF)
for 1 h and treated banana fiber-polyester resin composite (TBF-PR) for 5 h.
vi
LIST OF TABLES
Table 3.1: Properties of select natural fibers. 33

Table-3.2: Average chemical amounts of some natural fiber. 39
Table 3.3: Three smaller areas in IR region. 73
Table 4.1: The NaOH treatment steps followed for the samples. 83
Table 5.1: Average chemical compositions of banana fibers. 100
Table 5.2: Effect of fiber treatment with 5% NaOH solution (for different hours) on 107
tensile properties of composites.
Table 5.3: Effect of fiber treatment with 5% NaOH solution (for different hour) on 110
the flexural properties of composites.
Table 5.4: Values of n in σac(ω) = Aωn of untreated and treated banana fiber 114
composites.
Table 5.5: Activation energies of untreated and treated banana fiber composites. 116
Table 5.6: Effect of heating on mass loss (%) events at different temperature 130
intervals, onset of major degradation, and maximum slop of degradation
observed on TG curve.
Table 5.7: Effect of heating on the peak positions and rates observed on DTA and 130
DTG curves.
Table 5.8: Assignments of FTIR absorption bands for banana fiber and banana fiber- 132
polyester resin composites.
vii
Chapter 1 Introduction

INTRODUCTION
1.1 Introduction
It is known that technological development depends on the advancement in the field of materials.
Many of our modern technologies require materials with unusual combinations of properties that
cannot be meet by conventional metal alloys, ceramics, and polymeric materials. This is
especially true for materials that as needed for aerospace, underwater, and transportation
applications. For examples aircraft engineers are increasingly searching for structural materials
that have low densities, are strong, and abrasion and impact resistant, and are not easily
corroded. Frequently, strong materials are relatively dense; also increasing the strength or
stiffness generally results in a decrease in impact strength [1].
Materials property combinations and ranges have been, and are being, extended by the
development of composite materials. Composite materials represent nothing but a giant step in
the ever constant endeavor of optimization in materials. Strictly speaking, the idea of the
composite is not a new or recent one. Nature is full of example wherein the idea of composite is
used. The coconut, plum leaf is nothing but a cantilever using the concept of fiber reinforcement.
Woods is fibrous composite; cellulose fiber in lignin matrix. The cellulose fibers have high
tensile strength but are very flexible. While the lignin matrix joins the fiber furnishes the
stiffness [2].
The use of composites in all products - from sporting goods to bridges to satellites is increasing.
Outside of the profession, though, many people would be hard pressed to identify a composite.
This article presents a simple definition of composite materials. Although it is primarily written
for people new to the materials, composite professionals may also find a few things of interest.
Most of the products are made from monolithic materials. That means the individual components
consist of a single material (an unreinforced plastic), or a combination of materials that are
combined in such a way that the individual components are indistinguishable (a metal alloy).
Composite materials, on the other hand, consist of two or more materials combined in such a
way that the individual materials are easily distinguishable. A common example of a composite
1


is concrete. It consists of a binder and reinforcement. Adding another reinforcement transforms

concrete into a three-phase composite.
The individual materials that make up composites are called constituents. Most composites have
two constituent materials: a binder or matrix, and a dispersed phase for reinforcement [3]. The
reinforcement is usually much stronger and stiffer than the matrix, and gives the composite its
good properties. The matrix holds the reinforcements in an orderly pattern. Because the
reinforcements are usually discontinuous, the matrix also helps to transfer load among the
reinforcements. Reinforcements basically come in three forms: particulate, discontinuous fiber,
and continuous fiber.
A classification scheme for various composite types based on reinforcement is given below [3]:
Composites
Particle-reinforced Fiber-reinforced Structural
Large- Dispersion- Continuous Discontinuous Laminates Sandwich

particle strengthened (Short) panels
Aligned Randomly oriented
A particle has roughly equal dimensions in all directions, though it doesn't have to be spherical.
Gravel, micro balloons, and resin powder are examples of particulate reinforcements.
Reinforcements become fibers when one dimension becomes long compared to others.
Discontinuous reinforcements (chopped fibers, milled fibers, or whiskers) vary in length from a
2


few millimeters to a few centimeters. Most fibers are only a few microns in diameter, so it
doesn't take much length to make the transition from particle to fiber.
With either particles or short fibers, the matrix must transfer the load at very short intervals.
Thus, the composite properties cannot come close to the reinforcement properties. With
continuous fibers, however, there are few if any breaks in the reinforcements. Composite
properties are much higher, and continuous fibers are therefore used in most high performance
components, be they aerospace structures or sporting goods.
Composite materials are available as plies or lamina. A single ply consists of fibers oriented in a
single direction (unidirectional) or in two directions (bidirectional; for example a woven fabric).
There are other forms, but these are the most important for this discussion.
Composite properties are best in the direction of the fibers. Perpendicular, or transverse to the
fibers, the matrix properties dominate because load must be transferred by the matrix every fiber
diameter. Because most structures are not loaded in a single direction, even though one direction
may dominate, it is necessary to orient fibers in multiple directions. This is accomplished by
stacking multiple plies together. Such a stack is called a laminate.
The most efficient composites have most of their fibers oriented in the primary load direction,
and just enough fibers oriented in the other directions to carry secondary loads and hold the
structure together. Efficiency means both low weight and low cost, because any fibers, which
don’t carry much load, could probably be removed.
Polymer science and technology is one of the most active and promising fields in science,
embracing a multitude of topics natural polymers such as cellulose, wool, silk, jute, banana, coir
fiber etc. which are of outmost importance for living system, to the synthetic high polymers.
Development of polymer is a continuous process for achieving polymer in a specific application
under certain environmental condition [4]. The bombardment of the invention of different
polymer field is increased day by day. The natural polymer is biodegradable, abundantly
available, and easily decomposable in the environment and co-friendly [5]. The polymer
materials that are biodegradable are now enjoying considerable popularity, especially from the
standpoint of environmental protection [6].
3


Natural fiber is completely biodegradable on the other hand synthetic fibers are imparting bad
effect on the environment. So, we have to increase the use of natural fiber to reduce the
environmental problem. There are about two thousands species from which natural fibers can be
extracted, but few of them have economical value. So, we must find out alternative resources for
the natural fiber extraction, which may be economical. Jute fiber was extensively used from the
past day in our country. But it has high production cost with large land area and low quality. On
the other hand some natural fibers like banana, palm, pulque, coir, etc. fibers are high quality
fiber and can be produced without any sufficient care and cost [4].
The most important properties of some natural fibers are given below [6]:
1) Very good strength properties, especially tensile strength. In relation to its weight the
best bast fibers attain strength similar to that of Kevlar.
2) Very good heat, sound and electrical insulating properties.
3) Combustibility. From a waste point of view, combustibility is an advantage. Products can
be disposed of through burning at the end of their useful service lives and energy can
simultaneously be generated.
4) Biodegradability. As a result of their tendency to absorb water, fibers will biodegrade
under certain circumstances through the actions of fungi and/or bacteria.
5) Dimensional stability. As a consequence of the hygroscopicity of the fibers, products and
materials based on plant fibers are not dimensionally stable under changing moisture
conditions. This is the greatest disadvantage in relation to industrial use of plant fibers.
However, if necessary, this may be controlled at an extra cost by a number of known
treatments (e.g., heat treatments or chemical modification procedures such as
acetylation).
6) Reactivity. The hydroxyl groups present in the cell wall constituents not only provide
sites for water absorption but are also available for chemical modification (e.g., to
introduce dimensional stability, durability, or improved oil/heavy metal absorption
properties).
Now a days the composites of engineering polymers combined with natural components like
wood, flax, hemp, jute, palm, sisal, banana, etc. are intensively studied from ecology point of
view and for their interesting physical properties. Natural fibers have several advantages
4


compared with their inorganic counterparts [7, 8]. They are low-cost fibers, highly available and
renewable, with low density and high specific properties as well as they are biodegradable and
less abrasive to expensive molds and mixing equipment. The main problem of these natural
fibers of their potential use as reinforcement is greatly reduced because of their incompatibility
with the hydrophobic polymer matrix, their poor resistance to moisture, and their tendency to
form aggregates during processing [7–12]. Therefore, the constituents need to be chemically
modified to enhancing adhesion between fiber and polymer matrix. It was reported that
enhancing the mechanical properties of these composites are dependent on the amount and kind
of chemical treatment [8, 9]. Jute/Glass fiber-reinforce unsaturated polyester hybrid composites
having 25% jute show improved mechanical properties as tensile strength 125%, tensile modulus
49%, bending strength 162%, and bending modulus 235% better than untreated jute composites
[10]. It was also reported that the mechanical response, water uptake and dielectric properties of
jute fiber reinforced polypropylene composites are dependent on the fiber volume fraction [11].
The tensile Young’s modulus and tensile strength monotonically increase with increasing the
fiber volume fraction, whereas the impact resistance increases up to a critical value of the fiber
volume fraction. A change in the dependence of water uptake and dielectric properties with fiber
loading at a critical fiber content is noticed. On the other hand, a study of the effect of
alkalization using 3% NaOH solution was carried out on flax, kenaf, abaca, and sisal to observe
impact that this common fiber pre-treatment process on fiber mechanical properties [12]. The
result of the investigation indicated that over treatment of natural fibers using NaOH could have
a negative effect on the base fiber properties.
With composites, the properties of the final product are determined by a number of plant fiber
characteristics. These include surface chemistry (e.g., waxes and inorganics such as silica) and
fiber aspect ratio in particular. In addition, other factors such as thickness, fiber percentage, and
amount and type of bonding agent (if any) will be important. The existing wood composites
industry (e.g., MDF manufacturing) already produces a very wide variety of product lines as a
function of product density, thickness, and other characteristics. New composites can similarly
be designed to have the required stiffness and strength and other properties depending upon
application. The importance of the role of final product design and the involvement of designers
with a good understanding of plant fiber-based materials in new product development cannot be
overstated [13].
5


Banana fiber is obtained from the edible-fruit-bearing plant, species Musa cavendishi and Musa
sapientum. The fibers are obtained mainly from the stem of the plant [4]. About 37 kg (average
weight) of stem yields about 1 kg of good quality fiber; the yield is 1–1.5% of dry fiber. The
fiber obtained from the central core is of lower quality. The fiber has not been exploited much
commercially hitherto, as it was considered inferior to abaca and other available hard fibers. It
can be extracted by hand scraping, by retting, or by using raspador machines; it can also be
extracted chemically, for example by boiling in NaOH solution. Extraction of the fiber for local
use (in cordage) or for cottage industries in due to its high cellulose and low lignin content, its
use in the paper industry (tissue, filters, specialty nonwoven, document, printing, surgical and
hygienic applications, coffee bags, meat casings, etc.) have been reported. Over the years, there
has been considerable interest in exploiting it for a variety of household and industrial uses on a
commercial scale. For instance, the use of banana fiber as reinforcement with autoclaved cement
mortar, with air-cured cement, or with air-cured plaster is being investigated. Therefore, the
development of mechanical decorticating methods is reported to be in progress. The potential
yield of the fiber in India is estimated to be 1102 tons annually. Unfortunately there is no work
or utilization of banana plant or fiber so far in our country. So, immediate attention must be
given for proper utilization of this high cellulose and low lignin content fiber.
For the manufacturing of reinforced composite materials, factors such as fiber content, fiber
diameter, fiber length, void content matrix properties, fiber-matrix bonding, fiber orientation and
fiber properties are very important as they determine the final properties of the natural fiber
reinforced composite components [14]. The banana fiber can be considered as important
potential reinforcing agent in thermosetting polyester resin. The use of banana fiber and their
effects on properties are not well documented. So in this project, an attempt will be made to
fabricate banana fiber-polyester resin and the effect of banana fiber addition on the properties of
banana-polyester resin composites. A study on jute-polyester reveals that properties markedly
affected by different process variables [15]. The knowledge will help better design composite
process and estimate the influence on composite properties by convenient and relevance analysis
and investigation of banana fibers.
6


1.2 Objective of the Present Study
The work is aimed at preparing and characterizing banana fiber reinforced polyester resin
composites. Structural, thermal, mechanical, and electrical characteristics of the banana fiber-
polyester resin composites of various compositions with different content of banana fiber will be
investigated. The effect of chemical treatment of banana fiber on the different proportion of
composites will also be investigated. The electrical and mechanical properties of the composites
as function of banana fiber content and the effect of thermal behavior will be discussed.
Mechanical and electrical properties of different composites will be analyzed to correlate these
properties with composition of the composites. These findings may indicate the suitability of
these composites for some application in different industries.
1.3 Outline of this Thesis
Polyester resin will be collected from local market. Banana fiber will be extracted from banana
tree. Raw and treated fibers (alkalization/acetylation) will be used as reinforcement. Banana
fiber-polyester resin composites with different fiber loading (as much as possible) will be
prepared by compression molding process. Banana fiber content, filler content, etc. will be
varied in the composites. Bulk density and water absorption of the different composites will be
measured. Structural and thermal analysis of composites will be performed by IR and
DTA/TGA, respectively at BCSIR. Mechanical properties (tensile and flexural strength) will be
measured by using a Universal Testing Machine (UTM) at BCSIR. AC-electrical and dielectric
parameter will be measured for all the samples at different frequencies and temperatures using a
LF Impedance Analyzer Agilent 4192.
1.4 Summary of this Thesis
To make this research work reader friendly this dissertation has been configured into six chapters
which are as follows:
7


Chapter 1: Introduction
In this chapter, a general introduction is presented where an idea about the natural fiber,
composite, fabricated composite are summarized. The purpose and outline of thesis are
described.
Chapter 2: Literature Survey

In this chapter, some earlier and resent works of a number of literatures are reviewed to
understand the scientific importance of those studies needs for the present investigation and the
objectives of the study.
Chapter 3: Theoretical background

In this chapter, the details about polymer, natural fiber and composites are described.
Deformation, stress, strain, dielectric, thermal analysis and infrared spectroscopy (IR) are
focused at the end of this chapter.
Chapter 4: Materials and methods

The experimental procedures are briefly explained in this chapter along with description of the
sample preparation, raw materials. The fundamentals and working principles of measurement
setup are discussed.
Chapter 5: Results and discussion

In this chapter, results and discussion are thoroughly explained. Bulk density, mechanical
properties (tensile and flexural), AC electrical measurements are discussed. Thermal analysis and
IR analysis are discussed at the end of this chapter.
Chapter 6: Conclusions
The results obtained in this study are summarized. Suggestions for future research on these
studies are included.
References are added at the end of each chapter.
8


References
[1] Joseph S., Sreekala M. S., Oommen Z., Koshy P., and Thomas S., “A comparison of the
mechanical properties of phenol formaldehyde composites reinforced with banana fibers
and glass fibers”, Compos. Sci. Technol., 62, 1857–1868, 2002.
[2] Kalaprasad G., Francis Bejoy and et.al., Polym. Int., 53, 1624–1638, 2004.
[3] William D. Callister, Jr., “Materials science and engineering an introduction” John Wiley
& Sons, Inc., New York, 473–547, 2000.
[4] Albert F., “Hill Economic Botany”, TMH edition, 9th Reprint-1990, 18–51, 1972.
[5] Lawrence E. N. and Robert F. L., “Mechanical properties of polymer and composite”, 2nd
edition, 5–35, 1994.
[6] Eichhorn S. J. et. al., J. Mater. Sci., 36, 2107–2131, 2001.
[7] Rozman H. D., Peng G. B., and Mohd Ishak Z. A., “The effect of compounding techniques
on the mechanical properties of oil palm empty fruit bunch-polypropylene composites”, J.
Appl. Polym. Sci., 70, 2647–2655, 1998.
[8] Erasmus E. and Anandjiwala R., “Enhancement of mechanical properties and interfacial
adhesion by chemical modification of natural fiber reinforced polypropylene composites”,
CSIR Fiber and Textile, Gomery Ave, Summerstrand, Port Elizabeth, 6001, 2008.
[9] Graupner Nina, “Improvement of the mechanical properties of biodegradable helm fiber
reinforced Poly(lactic acid) (PLA) composites by the admixture of man-made cellulose
fibers”, J. Compos. Mater., 43, 689–702, 2009.
[10] Kafi A., Abedin M. Z., Beg M. D. H., Pickering K. L., and Khan M., “Study on the
Mechanical Properties of Jute/Glass Fiber Reinforced Unsaturated Polyester Hybrid
Composites: Effect of Surface Modification by Ultraviolet Radiation”, Plast. Comp., 25,
575–588, 2006.
[11] Cabral H., Ciseros M., Kenny J. M., Vazquez A., and Bernal C. R., “Structure–Properties
Relationship of Short Jute Fiber-Reinforced Polypropylene Composites”, J. Comp.
Materials, 00, 2004
[12] Symington M.C., Banks W. M., West O. D., and Pethrick R. A., “ Tensile Testing of
Cellulose Based Natural Fibers for Structural Composite Applications”, J. Compos. Mater.,
43, 1083–1108, 2009.
[13] http://www.ienica.net/fibersseminar/olesen
[14] George Jayamol, Sreekala M. S., and Thomas Sabu, Polym. Eng. Sci., 41(9), 1471–1485,
2004.
[15] Salma Begom, “Study of the electrical and mechanical properties of jute mat-polyester
resin composites”, M. Phil. Thesis, Department of Physics, BUET, June, 2008.
9

Chapter 2 Literature Review
LITERATURE REVIEW
2.1 Review of the Earlier Research Works
New technology demand new materials. Polymer composites with their wide range of possible
fillers (biomaterials) and polymers open the way to an enormous range of material differing with
physical, mechanical, electrical, structural, optical and thermal properties. The complexity of
biomaterials available today is a result of the continual demand to improve the quality of
biomaterials needed for technological advancement. The new era of science and technology
know how in research development is a foundation for every other procedure. Different chemical
modifications of natural fibers have also been carried out to enhance fiber-matrix interfacial
strength in composites. Here is a survey on the reported works on fibers, polyester resin
composites and other polymer composites.
2.1.1 Study of chemical modification of natural fibers
Alkali treatment of natural fibers, also called mercerization is the common method to produce
high quality fibers [1]. Jute fibers were treated with 5% alkali solution for 0, 2, 4, 6 and 8 h at 30
o
C. The fibers were then dried at room temperature for 48 h followed by oven drying at 100 oC
for 6 h. Sreekala et al. [2] indicated that a 10–30% sodium hydroxide solution produced the best
defects on natural fiber properties. Flax fibers were soaked into 2.5, 5, 10, 15, 18, 20, 25 or 30%
NaOH solutions and it was found that 5 or 10 or 18% of sodium hydroxide solution were the
appropriate concentrations for mercerization. It has been reported by Garcia et al. [3] that 2%
alkali solution at 200 oC and 1.5 MPa pressure for 90 s was suitable for degumming and
defibrillation to individual fibers.
Several workers have performed works on alkali treatment [4, 5] and reported that mercerization
leads to an increase in the amount of amorphous cellulose at the cost of crystalline cellulose and
the removal of hydrogen bonding in the network structure. The jute fibers were washed with
detergent (2 vol% in aqueous solution, 15% active matter) and then immersed in beakers with a
solution of 5 wt% NaOH for 24 h at room temperature. After that, the fibers were washed
thoroughly with distilled water to remove the excess of NaOH and dried at 70 oC for 24 h under
10

vacuum [6]. The alkali treatment of jute fibers produced a drop in both tensile strength and
Yong’s modulus of the fibers. This result was attributed to the damage induced in the cell wall
and the excessive extraction of lignin and hemicelluloses, which play a cementing role in the
structure to the fibers. The banana fibers were cleaned and refluxed in 0.25% solution of NaOH
for 1 h and then washed in very dilute acid to remove the non-reacted alkali. Washing was
continued until the fibers were alkali free. The washed fibers were then dried in an oven at 70o C
for 3 h [7].
Acetylation is beneficial in reducing the moisture absorption of natural fibers. Reduction of

about 50% moisture uptake for acetylated jute fibers and of up to 65% for acetylated pine fibers
has been reported by A. K. Bledzki and J. Gassan [8]. Mishra et al. [5] investigated the
acetylation of sisal fibers. Dewaxed sisal fiber was immersed in 5 and 10% NaOH solution for 1
h at 30 oC; the alkaline-treated fiber was soaked in glacial acetic acid for 1hr at 30 oC; it was
decanted and soaked in acetic anhydride containing one drop of concentrated H2SO4 for 5 min.
Effect of different chemical treatments (as treatment methods: (i) untreated, (ii) benzol/ alcohol,
(iii) acetic, acid-alkali, (iv) alkali, (v) acetylated, (vi) thermal, (vii) alkali-thermal and (viii)
thermal-alkali) on the tensile properties of sisal fiber was studied by Yang et al. [9]. Except for
the treatment methods of (iii), (vii) and (viii), the tensile strength was found to be increased in
comparison to that of untreated fibers. The reinforcing ability of the fibers depends upon the
various factors such as mechanical strength of fiber, polarity of the fiber, surface characteristics
and presence of reactive centres. All these factors control interfacial interaction between fibers
and matrix. The improve stiffness of the fiber was attributed to the crystalline region of the fiber.
The fibers also showed very good elongation properties, with values increasing upon
modifications. Lower elongation properties of the untreated fibers may be due to the three
dimensionally cross-linked networks of cellulose and lignin. Pretreatments broke this network
structure giving the fiber higher elongation and lower strength properties.
Joseph et al. [10] reported the effect of chemical treatment on the tensile properties of short sisal-
fiber-reinforced polyethylene (PE) composites (both randomly & unidirectional oriented) and
analyzed the mechanisms of different treatment methods. Their treatment methods and results
are:
11

a) Alkali treatment: Alkali treatment can remove natural and artificial impurities and produce a
rough surface topography. In addition, alkali treatment leads to fiber fabrilation, i.e. breaking
down the fiber bundle into smaller fibers. This increases the effective surface area available for
wetting by the matrix resin. Hence increasing the fiber aspect ratio caused better fiber/matrix
interface adhesion and increase in mechanical properties.
b) Isocyanate treatment: The hydrophilic nature of sisal fibers can be reduced by treating the
fibers surface with urethane derivative of cardanol (CTDI), because of the linkage of the long
chain structure of CTDIC to the cellulosic fibers. This makes sisal fibers compatible with PE
matrix, thus resulting in a strong interfacial bond between these two constituents with improved
mechanical properties.
c) Peroxide treatment: The function of peroxide treatment is that it can graft PE on to the
cellulosic surface. The grafting reaction is a result of the peroxide initiated free radical reaction
between the PE matrix and cellulose fibers. The tensile strength of the composite increases with
peroxide concentration up to a critical level depending on the fiber content and then remains
constant.
2.1.2 Study of banana fiber reinforced polymer composites
Joseph et al. [11] carried out research on a comparison of the mechanical properties of phenol
formaldehyde composites reinforced with banana fibers and glass fibers. They fabricated
composites using banana fiber and glass fiber with varying fiber length and fiber loading. The
analysis of tensile, flexural and impact properties of these composites revealed that the optimum
length of fiber required for banana fiber and glass fiber were different in phenol formaldehyde
resin matrix. Both banana fiber and glass fiber reinforced composites showed a regular trend of
increase in properties with fiber loading. Interfacial shear strength values obtained from single
fiber pull out test revealed that the interlocking between banana fiber and phenol formaldehyde
resin was much higher than that between glass and phenol formaldehyde resin. SEM studies
were carried out to evaluate fiber/matrix interactions. Finally, the experimental tensile strengths
were compared with the theoretical predictions.
12

Joseph et al. [12] studied the electrical properties of banana fiber-reinforced phenol
formaldehyde composites with special reference to fiber loading, fiber treatments, and
hybridization with glass fibers. The dielectric constant decreased with frequency and fiber
loading. Treatments with silanes, NaOH and acetylation, latex treatment, heat treatment, and
cyanoethylation decreased the dielectric constant value. The dielectric constant was higher for
banana/PF composites than that of glass/PF composites. In hybrid composites, the dielectric
constant decreased with increase in glass fiber concentration. The volume resistivity of banana
fiber-reinforced phenol formaldehyde composites decreased with frequency and fiber loading.
Chemical modifications in the fiber increased the volume resistivity of the composites. Volume
resistivity of banana/glass hybrid composites increased with increase in glass fiber content.
Layered composites with glass fiber at periphery were found to have higher volume resistivity
than other layering patterns. The loss factor decreased by the chemical treatments and in hybrid
composites it decreased with increase in volume fraction of glass fibers.
Barreto et al. [13] carried out the structural characterization of the banana fibers modified by
alkali treatment. It was observed by XRD that chemical treatment with NaOH increased the
crystalline fraction of the banana fiber, due to partial removal of the lignin (amorphous phase).
The vibrational modes obtained by IR spectroscopy did not suffer significant changes after this
alkaline process and the main bands appeared approximately in the same range wave number.
The dielectric permittivity and the loss factor are dependent on the alkaline solution
concentration. It was obtained 12.59 for dielectric permittivity at 10 Hz with the major
concentration. The values for the dielectric loss were approximately between 10-1 and 10-2
depending on the sample. These values are reasonable and could also be utilized as an electronic
device in conjunction with other materials to do a composite phase.The dielectric relaxation
processes observed by the electrical modulus were dependent on the temperature measurements
and related to water molecules present in hydrophilic groups of the anhydroglucose. The
chemical treatment employed in this work contributed to increase the metal removal, and the
values were governed by solution pH. The results showed that treated banana fiber is a low cost
alternative for metal removal in aqueous industry effluents. Thus, for regions with low resources,
the biosorbents are an alternative to diminish the impact of the pollution caused by local
industries, besides being a biodegradable product.
13

Ghosh et al. [14] studied on the effect of fiber volume fraction on the tensile strength of banana
fiber reinforced vinyl ester resin composites. They found an improvement in the tensile
properties of these composites. At 35% of fiber volume fraction the tensile strength is increased
by 38.6% and 65% increased in tensile modulus. At lower volume fraction of banana fiber, the
strength of composite specimen is reduced when compared with the virgin resin. Banana fiber
having high specific strength makes a light weight composite material and can be used to make
light weight automobile interior parts.
Sathasivam et al. [15] reported that the thermal properties of modified banana trunk fibers (BTF).
Dynamic TG analysis was employed to investigate the thermal decomposition of five treated
BTF. The treatments are mercerization, acetylation, peroxide treatment, esterification, and
sulphonation. The common iso-conventional methods (Kissinger, Friedman, and Flynn–Wall–
Ozawa) were employed to determine the apparent activation energy of these fibers. A similar
degradation pattern was observed for all the treated BTF (except for BTF-5), as the base material
is cellulosic fibers. The obtained curves had distinct peak and a high temperature tail which is
attributed to cellulose and lignin, respectively. Decomposition temperature of the treated fibers
increased in the order of esterification > untreated > mercerization > peroxide treated >
acetylation. The apparent activation energy of the treated fibers is within the polymer processing
temperature range, indicating that the modification is suitable for polymer composite processing.
Silviya et al. [16] prepared and characterized of composite films based on poly(ethyleneco-vinyl
acetate) (EVA) and cellulose derived from banana plant waste. The composite films were
subsequently examined by scanning electron microscopy, thermogravimetry, differential
scanning calorimetry (DSC), and FTIR spectroscopy. It was found that the EVA/cellulose
composites were more thermally stable than EVA or cellulose alone. In the DSC results, a shift
in softening temperature of vinyl acetate in EVA was observed, indicating the development of a
favorable interaction between cellulose and vinyl acetate regions of EVA copolymer. The
mechanical testing of the samples revealed that 7.5 wt % cellulose loaded EVA offered the
highest tensile strength. The elastic modulus was found to increase with the cellulose content
whereas percentage strain at break decreased, within the loading range of 0–10 wt %. X-ray
diffraction studies showed that EVA/cellulose composites were more crystalline than EVA.
14

Nayak et al. [17] fabricated the hybrid composites of polypropylene (PP), reinforced with sort
banana and glass fibers using Haake torque rheocord followed by compression molding with and
without the presence of maleic anhydride grafted polypropylene (MAPP) as a coupling agent.
Incorporation of both fibers into PP matrix resulted in increase of tensile strength, flexural
strength, and impact strength upto 30 wt% with an optimum strength observed at 2 wt% MAPP
treated 15 wt% banana and 15 wt% glass fiber. The rate of water absorption for the hybrid
composites was decreased due to the presence of glass fiber and coupling agent. The effect of
fiber loading in prence of coupling agent on the dynamic mechanical properties was analyzed to
investigate the interfacial properties. An increase of storage modulus of the treated composites
indicated higher stiffness. The loss tangent spectra confirms a strong influence of fiber loading
and coupling agent concentration on the α and β relaxation process of PP. The nature of fiber
matrix adhesion was examined through scanning electron microscope (SEM) of the tensile
fractured specimen. Thermal were carried out through differential scanning calorimetry (DSC)
and the thermogravimetric analysis (TGA), indicated an increase in the crystallization
temperature and thermal stability of PP with the incorporation of MAPP-treated banana and glass
fiber.
Jandas et al. [18] fabricated poly lactic acid (PLA)/banana fiber (BF) biocomposites employing
melt blending technique followed by compression molding. BF were surface treated by NaOH
and various silanes viz. 3-aminopropyltriethoxysilane (APS) and bis-(3-triethoxy silyl propyl)
tetrasulfane (Si69) to improve the compatibility of the fibers within the matrix polymer.
Mechanical tests revealed an increase of tensile strength to the tune 136% and impact strength to
49% as compared with the untreated biocomposite. Thermal properties of the composites were
evaluated using DSC and TGA. DSC thermograms revealed an increase in the melting transitions
thus revealing effective fiber/matrix interface. The thermal stability in the biocomposites also
increased in case of banana fiber treated with Si69. Viscoelastic measurements using DMA
confirmed an increase of storage modulus and low damping values in the silane treated
biocomposites. Biodegradation studies in the biocomposites were investigated in B. cepacia
medium through morphological and weight loss studies.
Pothan et al. [19] reported that the hybrid composites of glass and banana fiber in polyester
matrix were subjected to dynamic mechanical analysis over a range of temperature and three
15

different frequencies. The effect of temperature on the storage modulus (E'), loss modulus (E"),
and loss factor or damping efficiency (tanδ) is determined. All the properties were compared
with those of the neat polyester samples and the un-hybridized composites. The effects of the
layering pattern of the two fibers on the ultimate viscoelastic behavior of the composites were
investigated. Composites were prepared with banana as the surface layer and glass as the surface
layer and also as an intimate mixture of glass and banana. At temperatures above Tg,, the storage
modulus values were found to decrease even with the addition of glass fiber for the geometry
where glass is the core material. The value of the storage modulus of the composites with the
above mentioned geometry was found to be different, above and below Tg, the value above Tg
being lower than that below Tg unlike in unhybridized composite. The loss modulus curves and
the damping peaks were found to be flattened by the addition of glass. Layering pattern or the
geometry of the composites was found to have a profound effect on the dynamic properties of the
composite. An intimately mixed composite was found to have the highest storage modulus
values in all compositions. The values were consistent with the results of tensile strength. The
tanδ curve was found to be affected by the layering pattern followed and gave insight into the
interaction in the material. The dielectric behavior of the composites was also found to be
dependent on the glass fiber volume fraction as well as the layering pattern employed.
2.1.3 Study of other natural fibers reinforced polymer composites
For the interface between sisal fibers and epoxy, Bisanda and Ansell [20] adopted silane
treatment methods to improve the adhesion and moisture resistance properties. They treated sisal
fibers in silne preceded by mercerization that produced very little change in the mechanical
properties of dry composites, mechanical performance of wet composites and hence water
resistance could improved. The treatment in 100% silane produced fibers that were almost
hydrophobic. This might be a result of improved interfacial bonding arising room the use of
silane. Water molecules at the interface tend to replace the resin-fiber covalent bond by water
hydrogen bonds. Hence, silane plays an important role in reducing water absorption in cellulose
fiber-reinforced composites.
16

Islam et al. [21] worked out research on development structure and strength properties of PP
(polypropylene)/jute blends. The composites of biodegradable PP reinforced with short jute
natural fiber was prepared by melt mixing followed by hot press molding. The mechanical
properties, thermal properties, microstructure analysis and morphologies of the composites were
studied via universal testing machine (UTM), thermo-gravimetric analysis (TGA), infrared (IR)
spectroscopy and scanning electron microscope (SEM) techniques respectively. The mechanical
properties like tensile and flexural strength were measured for both treated and untreated
specimens and compared. The result shows that alkali treated jute reinforced composites have
much better properties than the untreated jute reinforced composites. Both tensile and flexural
strengths and modulus have been decreased with increasing untreated fiber and increased with
increasing treated fiber in PP-jute composites (PPJC). The changes in the mechanical properties
were broadly related to the accompanying modification and interfacial bonding of PPJC. SEM
observations indicated good interfacial contact between the short fiber and PP matrix. TG/DTG
revealed that the introduction of short jute fiber led to a slightly improved thermo-oxidative
stability of PP-jute composites.
Beckermann et al. [22] studied on the processing production and improvement of hemp-fiber
reinforced polypropylene composite materials. The purpose of the research was to produce an
improved hemp-fiber reinforced polypropylene composite by optimizing the fiber strength, fiber
processing, composite processing and fiber-matrix interfacial bonding. An investigation was
performed on a crop of New Zealand grown hemp to determine the effect of point growth
duration on fiber strength. By conducting single fiber tensile tests on the hemp fiber, it was
discovered that the optimum growing periods was 114 days, producing fibers with an average
tensile strength of 857 MPa. An investigation was then conducted to determine suitable fiber
treatment methods to separate the fibers from their fiber bundles and to remove lignin and pectin,
whilst remaining the fiber strength. An alkali treatment consisting of digesting the fibers in a
10% NaOH solution at a maximum temperature of 160 oC and a hold time of 45 min was found
to produce strong fibers with low lignin content and good fiber separation. Finally, the alkali
treated fibers polypropylne and a maleated polypropylene (MAPP) coupling agent was
compounded in a twin-screw extruder, and injection molded into composite tensile test
specimens. The strongest composite produced consisted of polypropylene with 40 wt% fiber and
17

2wt% MAPP, and had a tensile strength of 38 MPa and a stiffness of 4 GPa. The addition of
MAPP improved the fiber-matrix interfacial bonding.
Khondker et al. [23] studied on the processing and mechanical properties of jute thermosetting
composites with woven and flat braided fabrics. Composites were manufactured by hand
lamination methods. Tensile and flexural properties were investigated to study their dependence
upon the surface modifications due to bleaching and coating treatments (coating agents: poly
vinyl alcohol and polypropylene) on the fiber materials. Test samples were polished and pre and
post failure examinations were carried out using optical and scanning electron microscopy in
order to analyze the test results and their relationships to the state of resin impregnation into the
fiber bundles, fiber/matrix interfacial interactions and the fracture and failure mechanisms. Full
bleaching treatment on the oven jute fabrics clearly improved mechanical performance of the
resultant composites by removing surface impurities and enhancing hydrophobicity of the
cellulose fiber surface, as compared to natural and half bleached specimens. While tensile
properties of flat-braided jute composites slightly degraded due to coating treatments, flexural
properties showed clear improvements. The changes in the mechanical properties were broadly
related to the accompanying modifications and to the state of microstructure imperfections, viz.
fiber/matrix interfacial adhesion, severity of resin matrix shrinkage during curing process,
fiber/matrix debonding and distribution of disbands within the matrix region, and also to the
relative fiber filament density along the loading axis, in the cured composite structure.
Monterio et al. [24] worked out research on mechanical performance of coir fiber/polyester
composites. The structural characteristics and mechanical properties of coir fiber polyester
composites were evaluated. The coir fibers were obtained from disregarded coconut shells that if
not properly processed constitute an environmental hazard. The as-received coir fiber was
characterized by scanning electron microscopy coupled with X-ray dispersion analysis.
Composites with two molding pressures and with amounts of coir fiber up to 80% were
fabricated. Up to 50% of fiber, rigid composites were obtained. For amounts of fiber higher than
this figure, the composites performed like more flexible agglomerates. The results obtained for
flexural strength allowed comparison of the technical performance of the composites with other
conventional materials.
18

Yang et al. [25] studied PVC composites with respect to the effects of fiber and matrix
modification, processing parameters on the mechanical and water resistance properties. Their
main objectives were to obtain the best processing parameters and interface modification to
make novel sisal/PVC composites. To make good use of sisal fiber and PVC it is important to
improve the interface so that better mechanical properties of the composites can be obtained. But
unfortunately, their results showed that thermal treatment, acetylating and coupling agent
improved neither the interface nor the mechanical properties. On the contrary, the untreated
sisal-fiber-reinforced PVC composites possessed better mechanical properties. These results
were explained by the small fiber volume fraction (18.5%) of the composites and the melting
process method that led to the poor immersion of fiber in the PVC matrix. However both treated
and untreated sisal/PVC composites had quite good moisture resistance.
Manikandan et al. [26] studied the tensile properties of short fiber-reinforced polystyrene
composites. Untreated and benzoylated sisal fibers were used to produce the composite and the
influences of fiber length, fiber content, fiber orientation and fiber benzoylation were
investigated. Variation in fiber length produced no considerable change in the modulus of the
composites but gave maximum tensile strength (25 MPa) at a fiber length of about 10 mm.
Alvarez et al. [27] carried out research on the effect of microstructure on the tensile and fracture
properties of sisal fiber/starch-based composites. The effect of microstructure on the tensile and
fracture properties of injection molded biocomposites consisting of starch-based matrix and short
sisal fibers were investigated. Tensile tests were carried out on samples cut in longitudinal (L)
and transverse (T) directions with respect to the melt flow direction. An increasing trend in
Young’s modulus and tensile strength with fiber content was found, irrespective of the sample
orientation. In addition, this reinforcing effect was more pronounced for L samples with many
fibers mainly oriented longitudinally to the loading direction. Quasistatic fracture tests were also
performed on SENB specimens with cracks propagating both parallel and perpendicular to the
melt flow direction. The stress intensity factor was found to increase with fiber content, and it
also depended on fiber orientation. The observed trend in fracture toughness with fiber content
and microstructure was explained in terms of the fiber pullout mechanism. Puncture tests were
carried out for all compositions. Injection molded composites exhibited higher values of total
fracture energy than neat matrix. Furthermore, fiber orientation induced different patterns in the
19

damage zone. Finally, several theoretical models were used in this study to predict the elastic
properties of these composites.
Singh et al. [28] worked out research on sisal polyester composites. They concluded that the
properties of sisal-fiber-reinforced polyester composites can be improved when sisal fibers were
suitably modified with surface treatment. They carried out surface modification of sisal fiber
using coupling agents which were – a) N-substituted methacrylamide (coupling agent-1), b)
Gamma-methacryloxypropyl trimethoxy silane (coupling agent-2), c) Neopentyl (diallyl)oxy,
tri(dioctyl)pyrophosphato titanate (coupling agent-3) and d) Neopentyl (diallyl)oxy, triacryl
zirconate (coupling agent-4). They explained that the modified ‘interphase’ is much less stiff
than the resin matrix and it may prevent fiber/fiber contacts, hence removing the surface of high
stress concentrations in the final composites. Their experiment showed that by improving
interfacial adhesion the moisture induced degradation of composites can be reduced. Treated
fiber composites absorb moisture at a slower rate than the untreated counterparts, probably
because of the formation of a relatively more hydrophobic matrix interface region by co-reacting
organo-functionality of the coupling agents with the resin matrix. They also concluded that N-
substituted methacrylamide treated sisal-fiber-reinforced polyester composite generally exhibit
better mechanical properties under dry & wet condition. Because it has relatively void contents
compared to other fiber treated composites.
Ray et al. [29] worked out research on impact fatigue behavior of untreated and alkali treated
jute fiber reinforced vinyl ester composites. Jute fiber was kept immersed in the alkali solution
for 4 and 8 h. They reported that longer alkali treatment removed the hemicelluloses and
improved the crystallinity and gave better fiber dispersion. 35% jute/vinyl ester composites
containing both untreared and alkali treated fibers. The flexural strength of the composite made
from treated fibers was superior. 4 h alkali treated jute fibers gave the optimum combination of
improved interfacial bonding and fiber strength properties. On the contrary, the composites
reinforced with 8 h alkali treated fibers displayed superior impact fatigue properties.
Ray et al. [30] reported that vinyl ester-resin-matrix composites reinforced with untreated and
5% NaOH treated jute fibers for 4 and 8 h with different fiber loading were subjected to dynamic
mechanical and thermal analysis to determine their dynamic properties as a function of
temperature. For all the composites the storage modulus (E`) decrease with increase in
20

temperature, with a significant fall in the temperature range 110-170 oC. For the treated
composites the rate of fall dE`/dt, had an inverse relationship with the defect concentrations in
the 4 h treated composites corresponded to the highest rate of fall. The glass transition
temperature Tg of the unreinforced resin corresponding to the loss modulus peak was 101.2 oC
whereas that of the composites increased by nearly 28 oC on account of the restricted mobility of
the resin molecules in the presence of the fibers. In the case of treated composites, the Tg value
showed a decreasing trend (128-125 oC) unlike the plain resin a tiny hump was observed in the
loss modulus (E``) curves of all the composites around 166 oC which became broader and more
prominent with increase in the jute fiber content. The very high loss tangent (tanδ) value of the
resin decreased in the composites indicating that the addition of the fiber lowered the damping
capacity of the composites.
21

References
[1] Ray D., Sarkar B. K., Rana A. K., and Bose N. R., Bull. Mater. Sci., 24, 129, 2001.
[2] Sreekala M. S., Kumaran M. G., Joseph S., Jacob M., and Thomas S., Appl. Compos.
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[8] Bledzki A. K., and Gassan J., “Composites reinforced with cellulose based fibers”, J. Prog.
Polym. Sci., 24, 221, 1999.
[9] Yang G. C., Zeng H. M., Li J. J., Jian N. B., and Zhang W. B., Acta Scien.-tiarum
Naturalium, Universitatis Sunyatseni, 35, 53, 1996.
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[11] Joseph S., Sreekala M. S., Oommen Z., Koshy P., and Thomas S., “A comparison of the
mechanical properties of phenol formaldehyde composites reinforced with banana fibers
and glass fibers”, Compos. Sci. Technol., 62, 1857–1868, 2002.
[12] Joseph S. and Thomas S., “Electrical properties of banana fiber-reinforced phenol
formaldehyde composites”, J. Appl. Polym. Sci., 109, 256–263, 2008.
[13] Barreto A. C. H., Costa M. M., Sombra A. S. B., Rosa D. S., Nascimento R. F., Mazzetto
S. E., and Fechine P. B. A., “Chemically modified banana fiber: structure, dielectrical
properties and biodegradability”, J. Polym. Environ., 18, 523–531, 2010.
[14] Ghosh R., Krishna A. R., Reena G., and Raju Bh. L., “Effect of fiber volume fraction on
the tensile strength of banana fiber reinforced vinyl ester resin composites”, Int. J. Adv.
Eng. Sci. Technol., 4, 89–91, 2011.
[15] Sathasivam K. and Haris M. R. H. M., “Thermal properties of modified banana trunk
fibers”, J. Therm. Anal. Calorim. DOI 10.1007/s10973-011-1793-1, 2011.
[16] Silviya E. K., Unnikrishnan G., Varghese S., and Guthrie J. T., “Thermal and mechanical
characterization of EVA/banana fiber-derived cellulose composites”, J. Appl. Polym. Sci.,
DOI 10.1002/app.35140, 2011.
22

[17] Nayak S. K., Mohanty S., and Samal S. K., “Influence of interfacial adhesion on the
structural and mechanical behavior of PP-banana/glass hybrid composites”, Polym.
Compos., 31, 1247–1257, 2010.
[18] Jandas P. J., Mohanty S., Nayak S. K., Srivastava H., “Effect of surface treatments of
banana fiber on mechanical, thermal, and biodegradability properties of PLA/banana fiber
biocomposites”, Polym. Compos., 32, 1689–1700, 2011.
[19] Pothan, L. A., George C. N., John M. J., and Thomas, S., “Dynamic Mechanical and
Dielectric Behavior of Banana–Glass Hybrid Fiber Reinforced Polyester Composites”, J.
Reinf. Plast. Compos., 00, 1–15, 2009.
[20] Bisanda E. T. N. and Ansell M. P., “The effect of silane treatment on the mechanical and
physical properties of sisal epoxy composites”, Compos. Sci. Technol., 41, 165–178, 1991.
[21] Islam M. N., Bagom J., Gafur M. A., and Khan A. H., “Development, structure and
strength properties of PP/jute blends”, Jahangirnagar University J. Sci., 30, 89–106, 2007.
[22] Beckermann G. W., Pickering K. L., and Foreman N. J., “The processing, production and
improvement of helm-fiber reinforced polypropylene composite materials”, The 2nd
International Conference on Structure, Processing and Properties of Materials, Dhaka,
Bangladesh, SPPM2004, 257–265, February 2004.
[23] Khondker O. A., Ishaiku U. S., Nakai A., and Hamadu H., “Processing and mechanical
properties of jute thermosetting composites reinforced with woven flat-braided fabrics”,
The 2nd International Conference on Structure, Processing and Properties of Materials,
Dhaka, Bangladesh, SPPM2004, 224–231, February 2004.
[24] Monteiro S. N., Terrones L. A. H., and D’Almeida J. R. M., “Mechanical performance of
coir fiber/polyester composites”, Polymer Testing, 27, 591–595, 2008.
[25] Yang G. C., Zeng H. M., and Li J. J., “The study of technology and properties of composites
for sisal fiber reinforced PVC”, Fiber Reinforced Plastics/Composites, 6, 22–26, 1995.
[26] Manikandan K. C., Nair S. M. D., Thomas S., “Tensile properties of short sisal fiber
reinforced polystyrene composites”, J. Appl. Polym. Sci., 60, 1483–1497, 1996.
[27] Alvarez V., Vazquez A., and Bernal C., J. Compos. Mater., 40, 2–35, 2006.
[28] Singh B. and Gupta M. V., “Influence of fiber surface treatment on the properties of sisal-
polyester composites”, Polym. Compos., 17, 910–918, 1996.
[29] Ray D., Sarkar B. K., and Bose N. R., “Impact fatigue behavior of vinyl ester resin matrix
composites reinforced with alkali treated jute fiber”, Composite, 33, 233–241, 2002.
[30] Ray D., Sarkar B. K., Das S., and Rana A. K., “Dynamic mechanical and thermal analysis
of vinyl ester-resin-matrix composites reinforced with untreated and alkali treated jute
fiber”, Compos. Sci. Technol. 62, 911–917, 2002.
23

Chapter 3 Theoretical Background
THEORETICAL BACKGROUND
3.1 Polymer
A molecule has a group of atoms, which have strong bonds among themselves but relatively
weak bonds to adjacent molecules. Examples of small molecules are water (H2O), Methanol
(CH3OH), carbon dioxide, and so on. Polymers contain thousands to millions of atoms in a
molecule which is large; they are also called macromolecules; polymers are prepared by joining
a large number of small molecules called monomers. Polymers can be thought of as big buildings
and monomers as the bricks that go into them. Monomers are generally simple organic molecules
containing a double bond or a minimum of two active functional groups [1].
Polymers are structurally much more complex than metals or ceramics. They are cheap and
easily processable. On the other hand, polymers have lower strength and modulus and lower
temperature use limits. Prolonged exposure to ultraviolet light and some solvents can cause the
degradation of polymer properties. Because of predominantly covalent bonding, polymers are
generally poor conductor of heat and electricity. Polymers, however, are generally more resistant
to chemical than other metals. Structurally, polymers are giant chain like molecules (hence the
name macro molecules is also used) with covalently bonded carbon atom forming the backbone
of the chain. The process of forming large molecules form small one’s is called polymerization;
that is polymerization is the process of joining many monomers the basic building blocks,
together to form polymers.
3.1.1 Classification of polymers

Polymers are classified in many points of view to such as:
• Source
• Nature of the backbone chain of polymers
• Characteristic towards heat
• Ultimate nature
• Chemical structure
• Method of synthesis
24
• Composition and
• Polarity
According to the mechanical response at elevated temperatures, polymers can be classified in the
following classes:
i) Thermoplastic polymer (or thermoplasts)
ii) Thermosetting polymer (or thermosets)
i) Thermoplastic polymer: This type of polymer consists of linear molecular chains which are
not cross-linked. Instead, the attractive forces between the chains are the weaker secondary
bonding forces, i.e., Vander Walls forces. Thus, they are not-as rigid as the thermo sets, and
exhibit softening upon heating. These polymers soften when heated (and eventually liquefy) and
harden when cooled. The process of heating, reshaping and retaining the same on cooling can be
repeated several times. These materials are normally fabricated by the simultaneous application
of heat and pressure. The thermoplastics commonly used as matrix materials for fiber-reinforced
plastics include polycarbonates, polyamide (nylon 66), polystyrene, polyethylene, and
polypropylene. In general, the polymeric materials display low tensile strengths compared to
metals and ceramics. However, as a group they also exhibit relatively low specific growth which
makes them attractive candidates for lightweight matrix applications.
ii) Thermosetting polymer: These polymers undergo some chemical change on heating and
convert themselves into an infusible mass. They are like the yolk of the egg, which on heating
sets into a mass, and once set, cannot be reshaped such polymer, that became an infusible and is
soluble mass on heating are called thermosetting polymers (e.g. phenolics, polyurethane,
polyester, epoxy resin). These polymers become soft during their first heating and become
permanently hard when cooled. They do not soften upon subsequently heating. This group of
polymers is characterized by three-dimensional networks. Such non-linearity occurs when these
are more than two reactive sites per monomer and cross-linking takes place between linear
chains. Indeed, this type of polymer is initially cured or hardened by the application of heat,
hence the term thermosets. Thermosetting polymers are generally harder, stronger and more
brittle than thermoplastic polymers and have better dimensional stability. They are more usable
in process requiring high temperatures. These matrix materials are generally used in liquid
formulations, so they can be cast into any desired shape. In addition to cast ability, the initial
25
liquid form facilitates infiltration of the reinforcing phase and enhances setting of the fibers. The
thermosetting resin commonly used as matrix materials include epoxies, polyesters, phonetics,
and melamine.
In terms of molecular structure, there are several types of polymers such as linear, branched,
cross-linked and network polymers:
Linear polymer: Linear polymers are those in which mer units are joined together end to end in
single chains. (Mer: The group of atoms that constitutes a polymer chain repeat unit). These long
chains are flexible and may be thought of as a mass spaghetti. For linear polymers, there may be
extensive Van der Waals bonding between the chains. Some of the common polymers that form
with linear structures are polyethylene, polyvinyl chloride, polystyrene, polymethyl
methacrylate, nylon and the fluorocarbons.
Branched polymer: Polymer may be synthesized in which side-branch chains are connected to
the man ones; these are fittingly called branched polymers. The branches, considered to be part
of the main-chain molecule, result from side reactions that occur during the synthesis of the
polymer. The chain packing efficiency is reduced with the formation of side branches, which
results in a lowering of the polymer density.
Cross-linked polymer: In cross-linked polymers, adjacent linear chains are joined one to
another at various positions by covalent bonds. The process of cross-linked in achieved either
during synthesis or by a nonreversible chemical reaction that is usually carried out at an elevated
temperature. Often, this cross-linking is accomplished by additive atoms or molecules that are
covalently bonded to the chains. Many of the rubber elastic materials are cross-linked; in
rubbers, this is called vulcanization.
Network polymer: Tri-functional mer units, having three active covalent bonds, form three-
dimensional networks instead of the linear chain framework assumed by bi-functional mers.
Polymers composed of tri-functional units are termed network polymers. Actually, a polymer
that is highly cross-linked may be classified as a network polymer. These materials have
distinctive mechanical and thermal properties; the epoxies and phenol-formaldehyde belong to
this group.
26
It should be pointed out that polymers are not usually of only one distinctive structural type. For
example, a predominantly linear polymer might have some limited branching and cross-linking.
Depending on their origin, polymers can be grouped as natural polymers and synthetic polymers.
Natural polymer: Those isolated from natural materials are called natural polymers. Typical
examples are: cotton, silk, wool and rubber, cellophane, cellulose rayon and so on are in fact
chemical modification of natural polymer.
Synthetic polymer: Polymers synthesized from low molecular weight compound are called
synthetic polymer. Typical example: polyethylene, polyvinyl chloride (PVC), nylon, terylene etc.
Polymers are also classified as organic and inorganic polymers:
Organic polymer: A polymer whose backbone chain is essentially made of carbon atom is
termed an organic polymer. The atoms attached to the side valences of the backbone carbon atom
are, however, usually those of hydrogen, oxygen, nitrogen etc. The majority of synthetic
polymers are organic and they are very extensively studied. In fact, the number and variety of
organic polymers are so large that when we refer to "polymers", we normally mean organic
polymers.
Inorganic polymer: The molecules of inorganic polymers on the other hand, generally contain
no carbon atom in their chain backbone. Glass and Silicone rubber are example of inorganic
polymers.
3.1.2 Polymerization
In polymer chemistry, polymerization is a process of reacting monomer molecules together in a

chemical reaction to form three dimensional networks or polymer chains [2–4]. There are many
forms of polymerization and different systems exist of categorize them. The main categories are
chain-growth polymerization and step-growth polymerization.
Chain-growth polymerization: Chain growth polymerization (or addition polymerization)

involves the linking together of molecules incorporating double or triple chemical bonds. These
27
unsaturated monomers (the identical molecules that make up the polymers) have extra internal
bonds that are able to break and link up with other monomers to form the repeating chain. Chain-
growth polymerization is involved in the manufacture of polymers such as polyethylene,
polypropylene and PVC. A special case of chain-growth polymerization leads to living
polymerization.
In the radical polymerization of ethylene, its π bond is broken, and the two electrons rearrange to
create a new propagating center like the one that attacked it. The form this propagating center
takes depends on the specific type of addition mechanism. The free radical mechanism was one
of the first methods to be used. Free radicals are very reactive atoms or molecules that have
unpaired electrons. Taking the polymerization of ethylene as an example, the free radical
mechanism can be divided into three stages: chain initiation, chain propagation and chain
termination.
Heat, light
n (CH2 = CH2) → (– CH2 – CH2 –)n
Pressure or catalyst Polyethylene
Free radical addition polymerization of ethylene must take place at high temperatures and
pressures, approximately 300 oC and 2000 atms. While most other free radical polymerizations
do not require such extreme temperatures and pressures, they do tend to lack control. One effect
of this lack of control is a high degree of branching. Also, as termination occurs randomly, when
two chains collide, it is impossible to control the length of individual chains. A newer method of
polymerization similar to free radical, but allowing more control involves the Ziegler-Natta
catalyst, specially with respect to polymer branching.
Other forms of chain-growth polymerization include cationic addition polymerization and

anionic addition polymerization.
Step-growth polymerization: Step-growth polymers are defined as polymers formed by the

stepwise reaction between functional groups of monomer. Most step-growth polymers are also
classified as condensation polymers, but not all step-growth polymers (like polyurethanes formed
from isocyanate and alcohol bi-functional monomers) release condensates, in this case we talk
about addition polymers. Step-growth polymer increase in molecular weight at a very slow rate
28
at lower conversions and reach moderately high molecular weights only at very high conversion
(i.e., >95%)
Copolymerization: The process of polymerizing a single monomer or a single monomer pair is

termed as homopolymerization and the polymer thus obtained as homopolymer. On the other
hand, in copolymerization two or more monomers/monomer pairs are polymerized
simultaneously and hence, the polymer is composed of more than one repeat unit, In a word,
copolymerization is the addition polymerization of two or more different monomers.
Homopolymerization: A +A + A… → AAA… (homopolymer)

Copolymerization: A + B + A… → ABA… (copolymer)
Copolymerization thus can make materials with different properties than those of both
homopolymer and thus another dimension is added to the technology.
3.1.3 Polymer properties
Polymer properties are broadly divided into several classes based on the scale at which the
property is defined as well as upon its physical basis [5]. The basic structural properties of a
polymer are the identity of its constituent monomers and microstructure that play a major role in
determining bulk physical properties of the polymer, which describe how the polymer behaves as
a continuous macroscopic material. Chemical properties, at the nano-scale, describe how the
chains interact through various physical forces. At the macro-scale, they describe how the bulk
polymer interacts with other chemicals and solvents.
Microstructure
The microstructure of polymer (sometimes called configuration) relates to the physical
arrangement of monomer residues along the backbone of the chain [6]. These are the elements of
polymer structure that require the breaking of a covalent bond in order to change. Structure has a
strong influence on the other properties of a polymer. For example, two samples of natural
rubber may exhibit different durability, even though their molecules comprise the same
monomers.
29
Branching of polymer chains affects the ability of chains to slide past one another by altering
intermolecular forces, in turn affecting bulk physical polymer properties. A good example of this
effect is related to the range of physical attributes of polyethylene. High density polyethylene
(HDPE) has a very low degree of branching, is quite stiff and is used in applications such as milk
jugs. Low density polyethylene (LDPE), on the other hand, has significant numbers of both long
and short branches, is quite flexible and is used in applications such as plastic films.
The physical properties of a polymer are strongly dependent on the size or length of the polymer
chain. For example, as chain length is increased, melting and boiling temperatures increase
quickly [7]. Impact resistance also tends to increase with chain length, as does the viscosity, or
resistance to flow, of the polymer in its melt state [8]. Chain length is related to melt viscosity
roughly as 1:10, so that a tenfold increase in polymer chain length results in a viscosity increase
of over 1000 times [9, 10]. Increasing chain length furthermore tends to decrease chain mobility,
increase strength and toughness and increase the glass transition temperature (Tg). This is a result
of the increase in chain interactions such as Van der Waals attractions and entanglements that
come with increased chain length. These interactions tend to fix the individual chains more
strongly in position and resist deformation and matrix breakup, both at higher stresses and higher
temperatures.
Polymer Morphology
Polymer morphology generally describes the arrangement and micro scale ordering of polymer
chain in space.
Crystallinity: When applied to polymers, the term crystalline has a somewhat ambiguous usage.
In some cases, the term crystalline finds identical usage to that used in conventional
crystallography. For example, the structure of a crystalline protein or polynucleotide, such as a
sample prepared for X-ray crystallography, may be defined in terms of a conventional unit cell
composed of one or more polymer molecules with cell dimensions of hundreds of angstroms or
more. A synthetic polymer may be loosely described as crystalline if it contains regions of three-
dimensional ordering on atomic (rather than macromolecular) length scales, usually arising from
intermolecular folding and/or stacking of adjacent chains. Synthetic polymers may consist of
both crystalline and amorphous regions; the degree of crystallinity may be expressed in terms of
a weight fraction or volume fraction of crystalline material. Few synthetic polymers are entirely
30
crystalline [11]. The crystallinity of polymers is characterized by their degree of crystallinity,

ranging from zero for a completely non-crystalline polymer to one for a theoretical completely
crystalline polymer. Polymers with microcrystalline regions are generally tougher (can be bent
more without breaking) and more impact-resistant than totally amorphous polymers [12].
Polymers with a degree of crystallinity approaching zero or one will tend to be transparent, while
polymers with intermediate degree of crystallinity will tend to be opaque due to light scattering
by crystalline or glassy regions. Thus for many polymers, reduced crystallinity may also be
associated with increased transparency.
Mechanical properties
Mechanical properties of polymers are manifested by tensile strength, Young’s modulus of
elasticity, flexural strength and flexural modulus.
Transport properties
Transport properties such as diffusivity relate to how rapidly molecules move through the
polymer matrix. These are very important in many applications of polymers for films and
membranes.
Phase behavior
Melting point: The term melting point, when applied to polymers, suggests not a solid-liquid
phase transition but a transition from a crystalline or semi-crystalline phase to a solid amorphous
phase. Though abbreviated as simply ‘Tm’, the property in question is more properly called the
crystalline melting temperature. Among synthetic polymers, crystalline melting is only discussed
with regards to thermoplastics, as thermosetting polymers will decompose at high temperatures
rather than melt.
Glass transition temperature: A parameter of particular interest in synthetic polymer

manufacturing is the glass transition temperature (Tg), which describes the temperature at which
amorphous polymers undergo a transition from a rubbery, viscous amorphous liquid, to a brittle,
glassy amorphous solid. The glass transition temperature may be engineered by altering the
degree of branching or cross-linking in the polymer or by the addition of plasticizer [13].
31
Chemical properties
The attractive forces between polymer chains play a large part in determining a polymer’s
properties. Because polymer chains are so long, these interchain forces are amplified far beyond
the attractions between conventional molecules. Different side groups on the polymer can lend
the polymer to ionic bonding or hydrogen bonding between its own chains. These stronger forces
typically result in higher tensile strength and higher crystalline melting points.
The intermolecular forces in polymers can be affected by dipoles in the monomer units.
Polymers containing amide or carbonyl groups can form hydrogen bonds between adjacent
chains; the partially positively charged hydrogen atoms in =N–H groups of one chain are
strongly attracted to the partially negatively charged oxygen atoms in =C=O groups on another.
These strong hydrogen bonds, for example, result in the high tensile strength and melting point
of polymers containing urethane or urea linkages. Polyesters have dipole-dipole bonding
between the oxygen atoms in =C=O groups and the hydrogen atoms in H–C≡ groups. Dipole
bonding is not as strong as hydrogen bonding, so polyester’s melting point and strength are lower
than Kevlar’s (Twaron), but polyesters have greater flexibility.
Ethene, however, has no permanent dipole. The attractive forces between polyethylene chains
arise from weak Van der Waals forces. Molecules can be thought of as being surrounded by a
cloud of negative electrons. As two polymer chains approach, their electron clouds repel one
another. This has the effect of lowering the electron density on one side of a polymer chain,
creating a slight positive dipole on this side. This charge is enough to attract the second polymer
chain. Van der walls forces are quite weak, however, so polyethylene can have a lower melting
temperature compared to other polymers.
3.2 Natural Fiber
Jute, sisal, banana, palm and coir, the major source of natural fibers, are grown in many parts of
Bangladesh. Some of them have aspect ratios (ratio of length to diameter) > 1000 and can be
woven easily. Sisal and banana fibers are cellulose-rich (> 65%) and show tensile strength,
modulus and failure strain comparable with other cellulose-rich fibers like jute and flax whereas
32
the lignin-rich (> 40%) coir, palm fiber is relatively weak and possess high failure strain. These
fibers are extensively used for cordage, sacks, fishnets, matting and rope, and as filling for
mattresses and cushions (e.g. rubberized coir). Cellulosic fibers are obtained from different parts
of plants, e.g. jute and ramie are obtained from the stem; sisal, banana and pineapple, palm from
the leaf; cotton from the seed; coir from the fruit, and so on [14].
Recent reports indicate that plant-based natural fibers can very well be used as reinforcement in
polymer composites, replacing to some extent more expensive and non-renewable synthetic
fibers such as glass. The maximum tensile, impact and flexural strengths for natural fiber
reinforced plastic (NFRP) composites reported so far are 104.0 MN/m2 (jute-epoxy), 22.0 kJ/ m2
(jute-polyester) and 64.0 MN/m2 (banana-polyester), respectively [15]. The properties of some of
the natural fibers are compared in Table 3.1.
There are many examples of the use of cellulosic fibers in their native condition like sisal, coir,
jute, banana, palm, flax, cotton, and paper for reinforcement of different thermoplastic and
thermosetting materials like phenol formaldehyde, unsaturated polyester, epoxy, polyethylene,
cement, natural rubber etc. Different geometries of these fibers, both singly and in combination
with glass, have been employed for fabrication of uni-axial, bi-axial and randomly oriented
composites. Amongst these ligno-cellulosic fibers, jute contains a fairly high proportion of stiff
natural cellulose.
Table 3.1: Properties of select natural fibers [15].
Property Jute Banana Sisal Pineapple Coir

Width or diameter (mm) - 80-250 50-200 20-80 100-450
Density (gm/cc) 1.3 1.35 1.45 1.44 1.15
Volume Resistivity at 100 volts - 6.5-7 0.4-0.5 0.7-0.8 9-14
5
(W cm x 10 )
Micro-fibril angle (degree) 8.1 11 10-22 14-18 30-49
Cellulose/lignin Content (%) 61 /12 65 /5 67 /12 81 /12 43 /45
Elastic modulus (GN/m2) - 8-20 9-16 34-82 4-6
Tenacity (MN/m2) 440-533 529-754 568-640 413-1627 131-175
Elongation (%) 1-1.2 1.0-3.5 3-7 0.8-1.6 1.5-4.0
33
Advantages and disadvantages of natural fibers: Natural fibers have so many advantages such
as abundantly available, low weight, biodegradable, cheaper, renewable, low abrasive nature,
interesting specific properties, as these are waste biomass and exhibit good mechanical
properties. Natural fibers also have some disadvantages such as moisture absorption, quality
variations, low thermal stability and poor compatibility with the hydrophobic polymer matrix.
3.2.1 Structure and occurrence of natural fibers
All plant species are built up of cells. When a cell is very long in relation to its width it is called
a fiber. For example, wood fibers are mostly 50–100 times as long as they are wide. The fiber is
like a microscopic tube (i.e., a wall surrounding a central void referred to as the lumen).
Moreover, when the cell wall is made up mainly (85% or more) of cellulose, hemicellulose and
lignin, we talk about lingo-cellulosed fibers, and this includes woody species, scrubs and most
agricultural crops. Typical lingo-cellulosed fibers from agriculture are found, for example, in
straws, flax, hemp, jute and sisal. Non-ligno-cellulosed fibers are those that do not contain lignin
and are found in potatoes, beets and cotton amongst other crops. Furthermore, the various types
of raw material are separated using processes to generate fibers suitable for specific end
products, e.g., bast or stem fibers are mainly used in the textile or rope industries because both
require fibers that are as long as possible. Bast straw, for example, is not separated into single
fibers but into fiber bundles, which may contain thousands of single fibers; in contrast, wood is
usually separated into single fibers or very small fiber bundles suiting the particular needs of the
pulp, paper or board industries. Thus, in selecting fibers for new materials, there are a great
number of opportunities for selecting fibers of different dimensions.
Although put to so many different uses, and perhaps differing in texture, strength, chemical
composition, and place of origin, with few exceptions fibers are alike in that they are
sclerenchyma cells and serves as the part of the plant skeleton. For the most they are long cell
with thick walls, correspondingly small cavities, and usually pointed ends. The walls often
contain lignin as well as cellulose. Fibers may occur singly or in small groups, but more likely to
form sheets of tissue with the individual cells overlapping and interlocking [14].
34
Fibers may be found in almost any part of the plant–– stems, leaves, roots, fruits, and even seeds.
The four chief types, classified according to their origin, include bast fibers; wood fibers;
sclerenchyma cells associated with the vascular-bundle strands in leaves; and surface fibers,
which are hair like outgrowths on the seeds of various plants. The use of the “bast fibers” is often
to criticism on the ground that it gives no indication as to the particular tissue or origin in which
the fibers occur. From a morphological viewpoint it would be preferable to designate those fibers
which occur in the outer parts of a steam as cortical fibers, pericyclic fibers, or phloem fibers.
3.2.2 Classification of fibers
Natural fiber can be classified according to their origin and grouped into:
Grasses and reeds: These fibers come from the stems of monocotyledonous plant such as
bamboo, alfa and sugarcane (bagasse). Both types of fibers can be used to reinforce plastics.
Reinforcing natural fibers/ fillers
Non-wood natural fibers Wood fibers
Soft and hard woods
Straw Bast Leaf Seed/ fruit Grass
Examples: Example: Examples: Examples: Examples:

Corn, wheat flax, jute, henequen, cotton, coir bamboo, switch
rice straws hemp sisal, leaf grass
Fig. 3.1: Classification of natural fibers which can be used as reinforcements or fillers in
polymers [16].
35
Leaf fibers: Leaf fibers are those that run lengthwise through the leaves of most
monocotyledonous plants such as sisal, banana, henequen, abaca, cantala, curaua, date palm,
pineapple, and esparto. These fibers are also referred to as hard fibers.
Bast fibers: These fibers (bundles) come from the inner bark (Phloem or bast) of the stems of
dicotyledonous plants. Common examples are jute, flax, hemp, kenaf, ramie etc. The bast and
leaf (the hard fibers) types are the most commonly used in composite applications.
Seed and fruit fibers: These are fibers that come from seed-hairs and flosses, which are
primarily represented by cotton (seed fiber) and coir (fruit fiber). Amongst other fruit fibers are
kapok and oil palm.
Wood fibers: These are come from the xylem of angiosperm (hardwood) and gymnosperm
(softwood) trees. Examples include maple, yellow poplar, pine and spruce. Wood fibers are the
most abundantly used cellulosic fibers due to their extensive use in pulp and paper industries.
It is possible to classify fibers in six groups based on their utilization, as follows [14]:
Textile fibers: The most important use of fibers at the present time is in connection with the
textile industry, which is concerned with the manufacture of fabrics, netting, and cordage. In
making fabrics and netting, flexible fibers are twisted together into thread or yarn and then oven,
spun, knitted, or otherwise utilized. Fabrics include cloth for wearing apparel, domestic use,
awnings, sails, etc., and also coarser materials such as gunny and burlap. The fabric fibers are all
of commercial importance. Netting fibers, which are used for lace, hammocks, and forms of net,
include many of the commercial fabric fibers and a host of native fibers as well. Both
commercial and native fibers used for cordage. For this purpose of the individual fibers are
twisted together rather than woven. Twine, binder twine, fish lines, rope, hawsers, and cables are
among the many kind of cordage.
Brush fibers: These are tough and stiff fibers, or even twigs and small stems, which are utilized
in the manufacture of brushes and brooms.
Plaiting and rough weaving fibers: Plates are flat, pliable, fibrous strands which are interlaced
to make straw hats, sandals, basket, chair seats and the like. More elastic strands are roughly
36
woven together of nettings and thatched roofs of houses, while supple twigs or woody fibers are
used for basket, chairs, and other forms of wickerwork.
Filling fibers: These fiber are used in upholstery and for stuffing mattresses, cushions, etc.; for
culking the seams vessels and in casks and barrels; and stiffening in plaster; and as packing
materials.
Natural fibers: These are usually tree basts, which are extracted from the bark in layers or
sheets and pounded in to rough substitutes for cloth or lace.
Paper making fibers: Paper making fibers include wood fibers, textile fiber utilized in either
the raw or manufactured state, or many other kinds.
It is obvious that any one plant cannot be restricted absolutely to any single group in this
economic classification, since the same fiber may be used for a different purpose and since the
plant may yield more than one kind of fiber [17].
3.2.3 Banana fibers
Chemically speaking, banana fiber is a composite leaf fiber extracted from the banana plant by
retting in water. Banana fiber is a complex mixture of chemical compound, which a no built up
by natural process during the growth of banana fiber in the plant stem. The composition of
banana fiber is not uniform. The condition of soil, climate maturity of the plant, retting etc.
makes considerable variation in the constituents of the fiber.
Figure 3.2 shows the banana plant of edible-fruit-bearing species Musacavendishi. The fibers are
obtained mainly from the stem of the plant [14]. About 37 kg (average weight) of stem yields
about 1 kg of good quality fiber; the yield is 1–1.5% of dry fiber. The fiber obtained from the
central core is of lower quality. The fiber has not been exploited much commercially hitherto, as
it was considered inferior to abaca and other available hard fibers. It can be extracted by hand
scraping, by retting, or by using raspador machines; it can also be extracted chemically, for
example by boiling in NaOH solution. Extraction of the fiber for local use (in cordage) or for
cottage industries in due to its high cellulose and low lignin content, its use in the paper industry
37
(tissue, filters, specialty nonwoven, document, printing, surgical and hygienic applications,
coffee bags, meat casings, etc.) have been reported. Over the years, there has been considerable
interest in exploiting it for a variety of household and industrial uses on a commercial scale. For
instance, the use of banana fiber as reinforcement with autoclaved cement mortar, with air-cured
cement, or with air-cured plaster is being investigated. Therefore, the development of mechanical
decorticating methods is reported to be in progress. The potential yield of the fiber in India is
estimated to be 1102 tons annually. Unfortunately there is no work or utilization of banana plant
or fiber so far in our country. So, immediate attention must be given for proper utilization of this
high cellulose and low lignin content fiber.

Fig. 3.2: Banana plant.
3.2.4 Chemical composition of natural fibers
The properties of natural fiber largely depend on the chemical composition of the fiber and the
properties of composites made from natural fibers are strongly influenced by these fiber
properties. Chemical constituents of natural fibers are cellulose, hemicellulose, lignin, water
soluble matters, fatty and waxy matters, pectin, moisture, ash etc. The chemical compositions of
some natural fiber are shown below:
38
Table 3.2: Average chemical amounts of some natural fiber.
Constituents Amounts (percentage dry basis)

Palm fiber [18] Banana fiber [15] Pulque fiber [18] Jute fiber [19]
α-Cellulose 38.4 63-64 66 60
Hemicellulose 30.9 19 12 22
Lignin 27.3 5 7 12
Others 3-5 10-11 - -
It is evident from the composition of natural fibers that the main constituents are α-cellulose,
hemicellulose, and lignin and the rest are very little influence to the structure of natural fiber.
Cellulose: Cellulose pertains to the class of carbohydrates. It contains 44.4 percent of carbon, 6.2
percent of hydrogen and 49.4 percent of oxygen [20]. Cellulose is the principal constituent of all
plant life. It is a linear polymer of anhydroglucose units linked in 1 and 4 position by a β-glucoside
links. The empirical formula of cellulose (C6H10O5)n corresponds to a polyanhydride of glucose.
The two terminal glucose residues of a cellulose molecule contain two different end groups; one
contains a reducing hemiacetal group in the position C1, and is therefore, known as the reducing end
group, where as the other contains an extra secondary hydroxyl group in the position C4 and is
known as the non-reducing end group. The structure of cellulose is written as follows:
The structure of cellulose :
CH2OH H OH CH2OH
H OH
H O O H H O O
H H H
OH H OH H OH H
H OH H
OH H H O O H H
H O OH
H OH CH2OH H OH
n CH2OH
Cellobiose residue = repeating unit of cellulose
Fig. 3.3: Structure of cellulose.
There are two secondary and one primary alcoholic hydroxyl groups in each basic anhydro-D-
glucose unit (C6H10O5)n, which are arranged in positions 2, 3 and 6 respectively, on the basic
unit. The reactivity of the hydroxyl groups varies in different reactions. In many reactions
39
(mainly esterification) the primary hydroxyl groups have a greater reactivity. The two secondary
hydroxyls, at the second and third carbon atoms, differ somewhat in their reactivity. The primary
hydroxyls of cellulose elementary units are responsible for the storability and dye ability of
cellulose materials. Cellulose is highly stereo specific. The high hydroxyl content of cellulose
might suggest high water solubility. This is because of stiffness of the chains and hydrogen
bonding between hydroxyl groups of adjacent chain [21] as shown in the following figure.
OH OH
OH OH OH
Fig. 3.4: Hydrogen bonding in adjacent chains.
Besides hydrogen bonding, another type of linkages called “Semiacetal linkages” are present
between the adjacent chain molecules of cellulose [22].
From X-ray diffraction diagram, it has been concluded that cellulose has two regions: crystalline
and amorphous. In the amorphous region the polymer chains end to be folded, and consequently,
they will have rather different properties the crystalline region. It is in disordered regions that the
most of the chemical reactions take place with cellulose. Again, polymeric fibers are never
completely crystalline. This interconnection of crystalline and amorphous regions enhances the
strength of the polymer [21]. As early as 1920, Herzog and Janeke [23] recognized that cellulose
from such widely different sources as cotton, ramie, wood, jute and flax gave identical X-ray
diagram and concluded that the these fibers had identical crystalline structures.
Hemicellulose: Hemicellulose is a group of cell wall polysaccharides. The isolated hemicellulose

is amorphous substances. The cellulose and lignin of plant cell walls closely interpenetrated by a
mixture of polysaccharides called hemicellulose. It is soluble in dilute alkali and they are readily
hydrolysed to pentose and hexose with some uronic acids.
Sarker [24] and others showed xylose linked with methyluronic acid formed the basic building units
of hemicellulose in jute. It appeared that six xylose units were linked with 1-methyl glucuronic acid
units [25]. The structure of the repeating unit of jute hemicellulose 3-methylxy galactouronic acid
40
linked with xylose units. The hemicellulose is relatively short chain compounds and, therefore,
occupies longitudinally the same space as the anhydroglucose unit in cellulose chain. The short
chain polysaccharides would, therefore, pack rigidly into the oriented cellulose structure between
which some cross-bridging or looping may also occur.
T h e s t r u c t u r e o f h e m i c e llu lo s e
H OH H H OH
O
H H H
O H O OH H
OH H
H H H
O O
H H H
O O
H H OH H n
CO OH
H O O
H
O CH H
3
OH H
H H
Fig. 3.5: The structure of the repeating unit of jute hemicellulose 3-methylxy galactouronic acid
linked with xylose units.
Lignin: Most plant tissues contain, in addition to carbohydrate and extractives, an amorphous
polymeric gummy material is called lignin [26–27]. The nature of lignin and its relationship to
cellulose and other constituents of fiber are still uncertain. Unlike cellulose and hemicellulose,
lignin gives a series of colour reactions [28] that indicate the presence of compounds for which
these reactions are typical. Isolated lignin is generally an amorphous material having average high
molecular weight.
Lignin is an insoluble, resin like substance of phenolic character. It is built up to a large extent, of
phenyl propane building stones, often having a hydroxyl group in the para position and methoxyl
group/groups in meta position/positions to the side chain [29]. Besides, there may be carbon to
carbon or carbon to oxygen bonds joining the aromatic ring to the portions of structure. The lignin
molecule, thus being polyfunctional due to the presence of alcoholic and phenolic hydroxyl groups,
may exist in combination with two or more neighboring chain molecules, cellulose or
41
hemicellulose, serving the function of a cross-linking agent. Postulated monomer in lignin [30] is
shown below.
S tru ctu ra l u n it of lig n in :
HO CH 2 CH 2 CH 3
C H 3O
4 -h y d roxy-3 -m eth o xy p h en y l p ro p a n e.
Over all structure of lignin:
C
OCH3 OCH3
OH O
O C CH2 O C CH2
HO
CH2
CH2
O
O
OCH3 OCH3
Fig. 3.6: Structure of lignin.
The alkali sensitive linkage is an ester type of combination existing between hydroxyl groups of
lignin and carboxyl groups of ironic acids of hemicelluloses. The other one is being lived to be of
ether or similar types occur through the hydroxyl grouped of lignin. The lignin molecule thus
being polyfunctional due to the presence of alcoholic and phonetic hydroxyl groups may exist in
combination with two more neighboring chain molecules cellules or hemicelluloses serving the
function of a cross linking agent.
Lignin which is a short chain isotropic and non-crystalline (DP60) made up of units derived from
phenylpropane, lignin to found in the middle lamella of the fiber bundle as well as in the woody
core and the epidermal and cortical cells of the plant stem. It is also found in the walls of the
ultimate cells of the fibers the nature of lignin in different parts of the plant can be different. To
42
determine the lignin content the fiber sample from which waxes water soluble pectin matter and
hemicelluloses have been detracted, may be first chlorinated and then extracted with sodium
sulfite solution what remains is cellulose. The lignin can also be dissolved in sodium chlorite. In
the klason method, the cellulose is dissolved in 72% H2SO4 and the remaining lignin is weighed.
Association of cellulose, hemicellulose and lignin: There is no conclusive proof with regard to
the chemical union of hemicellulose with cellulose in the fiber. The opinion is that
hemicellulose, except xylan, cannot enter into cellulose crystallites due to spacing difficulty. The
cellulosans, mainly xylan, associated with the true cellulose in the cellulose structure, are
relatively short chain compounds, and occupy longitudinally the same space as the glucose units
in the cellulose chains. Xylan and cellulose are laid as a mixed crystallite structure probably with
incrusting cement consisting of lignin and hemicellulose [30].
Regarding the possibility of cellulose lignin combination, the view is that the lignin cannot enter
the cellulose crystallite due to the same spacing difficulties, but a small amount of lignin is
intimately associated at the cell wall boundaries of cellulose. Chemical union exists between
lignin and hemicellulose and it is the ester type linkage between the alcoholic hydroxyl group of
lignin and the carboxyl group of polyuronic acid of hemicellulose, and the ether type linkage
between phenolic hydroxyl group of lignin and hydroxyl group of hemicellulose [31].
3.2.5 Physico-mechanical properties of natural fibers
Physical properties of fiber such as breaking strength, extensibility, flexibility and moisture
absorption etc. all depend on a number of factors of which the length of the fiber molecules, the
mode of alignment amongst them and the nature and intensity of inter chain cohesive forces are
important. In pure cellulose fiber the lateral cohesive forces including hydrogen bonds have
maximum intensity in the crystalline regions, where the chain molecules are arranged in a more
organized manner. The crystalline portions contribute in the strength and rigidity of fibers, while
amorphous portions, which allow a better freedom of movement of the chain molecule account
for extensibility, flexibility and moisture affinity. The non-crystalline region of cotton tree is
contributed to a considerable extent to its strength by the cross-linkages of incrustants which are
43
distributed entirely in the amorphous regions. If these cross-linkages are ruptured, appreciable
loss of wet strength of the fiber results [31].
Like tensile strength, the other properties of fibers such as extensibility and flexibility are also
influenced to a great extent by the cross-linkages in the amorphous regions usually, the low inter
cohesion in the amorphous region permits a better freedom of movement to the chain molecules
as a result of which these regions impart the above useful qualities to the fiber. In natural fiber,
however, due to the presence of cross-linkages the relative movement of the carbohydrate chains
in much restricted, which ultimately affects both flexibility and extensibility [31].
3.2.6 Chemical properties of natural fibers
Natural plant fibers like jute, sisal, banana, palm fibers are a lingo-cellulose or leaf fibers which
properly speaking, compounds of cellulose with lignin. Unlike pure cellulose fiber, it is highly
reactive towards various chemical reagents such as acids alkalies and oxidizing reagents and the
higher reactivity arises mainly from the non-cellulosic constituents of the fiber, namely
hemicellulose and lignin. Lignin is unhydrolysable by acids readily oxidizable and soluble in hot
alkali while carbohydrates are easily hydrolysed by strong mineral acids to water soluble sugars
are relatively resistant to oxidizing agents [32].
The lingo-cellulose fiber is highly susceptible to the action of light. The main features of the
photo-chemical changes are the loss of tensile strength and development of a yellow or brown
color. The degradation caused by light to this fiber has been found to the greatest amongst all
natural cellulose fibers. The reactions involved in photo-chemical degradation of textiles are
mainly oxidative in nature and on prolongs exposure to light, the constituent chain molecules are
gradually oxidized in all possible manners and ultimately broken down to smaller fragments as a
result in the tensile strength of the fiber is adversely affected. It has been observed that all the
main fiber components including cellulose superior degradation and the components lignin and
hemicellulose are much reactive to light. Due to the influence of light ligneous residues
(phenolic group) are into color quinoid derivatives resulting in yellow or brown color. It is
established that lignin is responsible for yellowing of fibers. It is claimed that this photo-
chemical action of light on fiber is minimum in absence of moisture or atmospheric oxygen.
44
3.2.7 Chemical modification of natural fibers
The major drawback of cellulosed fibers as reinforcing agent is the high moisture absorption of
the fibers due to hydrogen bonding of water molecules to the hydroxyl groups within the fiber
cell wall. This leads to a moisture build-up in the fiber cell wall (swelling) and in the fiber matrix
interface. This is responsible for changes in the dimension of cellulose-based composites,
particularly in the thickness and the linear expansion due to reversible and irreversible swelling
of the composites. Consequently, the fiber matrix adhesion becomes weak and the dimensional
stability of cellulose based composites particularly for outdoor applications will be greatly
affected. Researchers investigated the effect of weathering on jute-polyester reinforced
composites and found decrease in composite properties because of weathering [33, 34].
Absorption and desorption of moisture by the composites during the study produced high
shrinkage stresses which caused surface crazing and deboning of matrix and banana, choir fibers.
This led to a reduction in mechanical properties of the composites studied [33]. The pretreatment
of natural fibers are aimed at improving the adhesion between fibers and matrix. In
pretreatments, either hydroxyl groups get activated or new moieties are added that can
effectively interlock with the matrix [35]. The chemical modification of natural fibers can be
done through several approaches including bleaching, alkalization, acetylation, etherification,
benzoylation, plasma activation, graft copolymerization [35].
Alkalization
Alkali treatment of natural fibers, also called mercerization, is the common methods to produce
high quality fibers [36]. Mercerization leads to fibrillation which causes the breaking down of
the composite fiber bundle into smaller fibers. Mercerization reduces fiber diameter, thereby
increases the aspect ratio which leads to the development of a rough surface topography that
results in better fiber-matrix interface adhesion and an increase in mechanical properties [37].
Moreover, mercerization increases the number of possible active sites and allows better wetting.
Mercerization has an effect on the chemical composition of the flax fibers, degree of
polymerization and molecular orientation of the cellulose crystallites due to cementing
substances like lignin and hemicellulose which were removed during the mercerization process.
As a result, mercerization had a long-lasting effect on the mechanical properties of flax fibers,
mainly on fiber strength and stiffness [38]. Several workers have performed work on alkali
45
treatment [37–40] and reported that mercerization leads to an increase in the amount of
amorphous cellulose at the cost of crystalline cellulose and the removal of hydrogen bonding in
the network structure.
3.3 Polymer Composite
Composite materials are produced by combining two or more dissimilar materials into a new
material that may be better suited for a particular application than either of the original materials
alone. Overall, the properties exhibited by a composite material are strongly influenced by the
properties of the individual constituents, their respective amounts (percentage), shape,
orientation and distribution plus any synergistic interaction between these constituents when they
are combined in composite formation. The most common example of a composite material is the
fiber-glass-reinforced plastic commonly used in household goods and in many industrial
applications. The plastic alone is relatively weak and has a low elastic modulus, that is, it bends
and stretches easily. However, it is very stable chemically and constitutes an excellent matrix for
the composite. The glass fibers provide the strength and stiffness; their modulus of elasticity may
be 50 times greater than that to the plastic [41]. Since the glass fibers can withstand a much
higher tensile stress before strain or yielding occurs, they take most of the load when the
composite is stressed. Many composite materials are composed of just two phases; one is termed
the matrix, which is continuous and surrounds the other phase, often called the dispersed phase.
3.3.1 Plastic and composite materials
Plastic materials
Plastics are indispensable to our modern way of life. Many people sleep on pillows and
mattresses filled with a type of plastic- either cellular polyurethane or polyester. At night, people
sleep under blankets and bedspreads made of acrylic plastics, and in the morning, they step out
of bed onto polyester and nylon carpets. The cars we drive, the computers we use, the utensils we
cook with, the recreational equipment we play with, and the house and buildings we live and
work in all include important plastic components. The average 1998-model car contains nearly
46
12 percent of the vehicle’s overall weight. Telephones, textiles, compact discs, paints, plumbing
fixtures, boats, and furniture are other domestic products made of plastics. In 1979 the volume of
plastics produced in the United States surpassed the volume of domestically produced steel [42].
Plastic materials made up of large, organic (carbon-containing) molecules that can be formed
into a variety of products. The molecules that compose plastics are long carbon chains that give
plastics many of their useful properties. In general, materials that are made up of long, chainlike
molecules are called polymers. The word plastic is derived from the word plasticus (Latin for
“capable of molding”) and plastikos (Greek “to mold” or “fit for molding”). Plastics can be made
hard as stone, strong as steel, transparent as glass, light as wood, and elastic as rubber. Plastics
are also lightweight, waterproof, chemical resistant, and produced in almost any color. More than
50 families of plastics have been produced, and new types are currently under development [42].
Composite materials
Composite materials have been classified in many ways depending on the ideas and concepts that
need to be identified. A useful and all embracing classification is set out with some examples.
Most naturally occurring materials derive their superb properties from a combination of two or
more components, which can be distinguished readily when examined in optical or electron
microscopes. Thus, for example, many tissues in the body, which have high strength combined
with enormous, flexibility, are made up of stiff fibers such as collagen embedded in a lower
stiffness matrix. The fibers are aligned in such a way as to provide maximum stiffness in the
direction of high loads and are also able to slide past each other, so that the tissue is very
flexible. Similarly, a microscopic examination of wood and bamboo reveals a pronounced fibril
structure, which is very apparent in bamboo when it is fractured. It is not surprising that bamboo
has been called natural fiberglass [43].
Practically, everything is a composite material in this world. Thus a common piece of metal is a
composite (polycrystal) of many grains (or single crystals). Such a definition would make thing
quite unwieldy. Therefore, it must be agreed on an operational definition of composite materials
for our purposes in this text. We shall call a material that satisfies the following conditions a
composite material.
i) It is manufactured (naturally occurring composite, such as wood are excluded).
47
ii) It consists of two or more physically and/or chemically distinct, suitably arranged or
distributed phases with an interface separating them.
iii) It has characteristics that are not depicted by any of the components in isolation.
3.3.2 Classification of composite materials
Generally, there are two kinds of composite materials [44]:
i) Natural composite materials

ii) Synthetic composite materials
Again, Broad classification of composite materials:
i) Natural composite materials: Wood, Bone, Bamboo, Muscle and other tissue
ii) Micro composite materials: Metallic alloys, e.g. steels, Toughened thermoplastics,
e.g., impact polystyrene, ABS, sheet-molding compounds, reinforced thermoplastics.
iii) Macro composite materials (Engineering products): Galvanized steel, reinforced
concrete beams and Helicopter blade skis.
One simple scheme for the classification of composite materials consists of three main divisions
[41]:
1. Particle-reinforced: i. Large particle

ii. Dispersion-strengthened
2. Fiber-reinforced: i. Continuous (aligned)
ii. Discontinuous (short) a) Aligned
b) Randomly oriented
3. Structural: i. Laminates
ii. Sandwich panels
Particle-reinforced composites
The dispersed phase (i.e., reinforcement) for particle reinforced composites is equiaxed (i.e.,
particle dimensions are approximately the same in all directions). The distinction between large
48
particle and dispersion strengthened composites is based upon reinforcement or strengthening

mechanism.
Large-particle composites: The term ‘large’ is used to indicate that particle-matrix interactions
cannot be treated on the atomic or molecular level; rather continuum mechanics is used. For most
of these composites, the particulate phase is harder and stiffer than the matrix. These reinforcing
particles tend to restrain movement of the matrix phase in the vicinity of each particle. In
essence, the matrix reinforces some of the applied stress to the particles, which bear a fraction of
load. The degree of reinforcement or improvement of mechanical behavior depends on strong
bonding at the matrix-particle interface. For effective reinforcement, the particles should be
small and evenly distributed throughout the matrix. Some polymeric materials to which fillers
have been added are really large-particle composites. Another familiar large- particle composite
is concrete, being composed of cement (the matrix) and sand and gravel (the particulates). Large-
particle composites are utilized which all three material types (metals, polymers and ceramics).
The cermets are examples of ceramic-metal composites.
Dispersion-strengthened composites: Metals and metal alloys may be strengthened and

hardened by the uniform dispersion of several volume per cent of fine particles of a very hard
and inert material (i.e., the dispersed particles are chosen to be unreactive with the matrix phase).
The dispersed phase may be metallic or non metallic; oxide materials are often used. The high-
temperature strength of nickel alloys may be enhanced significantly by the addition of about 3
vol. % of thoria (ThO2) as finely dispersed particles; this material is known as thoria-dispersed
(or TD) nickel. The same effect is produced in the aluminium-aluminium oxide system. A very
thin and adherent alumina coating is caused to form on the surface of extremely small (0.1 to 0.2
µm thick) flakes of aluminium, which are dispersed within an aluminium metal matrix; this
material is termed as sintered aluminium powder (SAP).
Fiber-reinforced composites
Technologically, the most important composites are those in which the dispersed phase is in the
form of a fiber. The fiber phase may be a polymer, metal or ceramic that has been drawn into a
long and thin filament. Design goals of fiber-reinforced composites often include high-strength
and/or stiffness on a weight basis. Those characteristics are expressed in terms of specific
49
strength and specific modulus parameters, which correspond, respectively, to the ratios of tensile
strength to specific gravity and modulus of elasticity to specific gravity.
Structural composites
A structural composite is normally composed of both homogeneous and composite materials, the
properties of which depend not only on the properties of the constituent materials but also on the
geometrical design of the various structural elements. Two most common structural composites
are laminar composites and sandwich panels.
Laminar composites: A laminar composite is composed of two-dimensional sheets (or panels)

that have a preferred high-strength direction such as is found in wood and continuous and
aligned fiber-reinforced plastics. The layers are stacked and subsequently cemented together
such that the orientation of the high-strength direction varies with each successive layer.
Laminations may also be constructed using fabric material such as cotton, paper or woven glass
fibers embedded in a plastic matrix. Thus, a laminar composite has relatively high strength in a
number of directions in the two-dimensional plane; however, the strength in any given direction
is, of course, lower than it would be if all the fibers were oriented in that direction. An example
of a relatively complex laminated structure is the modern ski.
Sandwich panels: Sandwich panels consist of two strong outer sheets or faces, separated by a
layer of less-dense material (or core), which has lower stiffness and low strength. The faces bear
most of the in-plane loading, and also any transverse bending stresses. Typical face material
include aluminum alloys fiber-reinforced plastics, titanium, steel and plywood. Structurally, the
core serves two functions:
a. It separates the faces and resists deformations perpendicular to the face plane.
b. It provides a certain degree of shear rigidity along planes which are perpendicular
to the faces.
Various materials and structures are utilized for cores, including foamed polymers, synthetic
rubbers, inorganic cements, as well as balsa wood. Another popular core consists of a
honeycomb structure–– thin foils that have been formed into interlocking hexagonal cells, with
axes oriented perpendicular to the face planes. Sandwich planes find a wide variety of
50
applications such as roofs, floors and walls of buildings; and, in aircraft, for wings fuselage and
tailplane skins.
Based on the matrix, composites are categorized into three classes:

1. Metal matrix composites (MMC)
2. Ceramic matrix composites (CMC)
3. Polymer matrix composites (PMC)
3.3.3 Principles of fiber reinforcement
The mechanical properties of a composite can depend on many factors, as alluded to in the
introduction basically; these factors include the specific properties of the matrix and the
reinforcing agent, their respective volume fractions, the shape, size distribution, and orientation
of the reinforcing phase and the bond between the reinforcement and its matrix [45]. Fiber
reinforced composites with exceptionally high specific strengths and moduli have been produced
that utilize low density fiber and matrix materials. The arrangement or orientation of the fibers
relative to one another, the fiber concentration and the distribution all have a significant
influence on the strength and other properties of fiber reinforced composites.
Some critical fiber length is necessary for effective strengthening and stiffening of the composite
material. The critical length ‘1c’ is dependent on the fiber diameter ‘d’ and its ultimate (or
tensile) strength ‘σf’ and on the fiber-matrix bond strength (or the shear yield strength of the
matrix) ‘τc’ according to:
.
lc = (3.1)
For a number of glass and carbon fiber-matrix combinations, this critical length is on the order of
1 mm, which ranges between 20 and 150 times the fiber diameter. Fibers for which l >> 1c
(normally 1 > 151c) are termed continuous; discontinuous or short fibers have lengths shorter
than this [41].
51
3.4.4 Stress-strain relationship
In order to analyze the stress strain behavior of a composite we will consider a simple situation
where a matrix containing continuous cylindrical fibers is deformed in direction parallel to the
long axis of the fibers, as illustrated in the following figure. If we can assume that no slippage
occurs at the interface between the fibers and matrix, the elongation is the same in both phases.
Therefore, the engineering strain in the composite may be expressed as:
<l
ec = e f = e m = (3.2)
lo
Where, ef = strain in fibers and em = strain in matrix.
lo
∆l
Fig.3.7: Axial deformation due to the load (p) in a composite reinforced with continuous
cylindrical fibers.
Furthermore, when these strains are elastic the engineering stress in the respective composite can
be determined by applying Hooke’s law as follows:
σf = Ef ef and σm = Em.em (3.3)

Where, σf = stress in fiber
σm = stress in matrix
Ef = elastic modulus of fiber
Em = elastic modulus of matrix
In most cases, the modulus of the fiber is greater than that of the matrix, for a given strain the
stress in the fiber is greater than the matrix stress. Although this is a bray simplified analysis it
52
serves to illustrate the extremely important concept fiber reinforcement. Generally, the fibers are
more highly stressed than the matrix when a load is applied to the composite. The mechanism
permits transfer of the stresses from the matrix to the reinforcing phase. As a result, the
composite can sustain greater stresses than the unreinforced matrix material. This concept of
utilizing the advantages of one material such as high modulus or high strength, in conjunction
with the advantages of another, such as low density or corrosion resistance, is the very essence of
composite materials.
3.3.5 Manufacturing routes for fiber reinforced plastics
Manufacturing routes : Outline of fabrication and processing methods.

Open mold processes
1. Hand lay-up : Chopped stand mats, woven roving and other fabrics made
from the fibers are plagued on the mold and impregnated
with fusion by painting and rolling. Layers are built up until
design thickness is achieved. Molding cures without heat or
pressure.
2. Spray up : Chopped fiber roving and resin sprayed simultaneously into
prepared mold and rolled before the resin cures.
3. Vacuum bag : Layers of fiber usually unidirectional sheets are pre-
Pressure bag impregnated with resin and partially cured (β-staged) to form
Autoclave a pre-peg. The pre-peg sheets are stacked on the mold
surfaces in predetermine orientations, covered with a flexible
bag, and consolidated using a vacuum or pressure bag in an
autoclave at the required using temperature.
4. Filament winding : Continuous roving or stands of fibers are filled over rollers
and guides through a bath of resin and then forward, using a
program controlled machine, onto a mandrel at
predetermined angles. The resin in partially or completely
cures before removing the component, usually a tube from
53
the mandrel.
5. Centrifugal castings : Mixtures of fibers and resin are introduced into a rotating
mold and allowed to cure in a site.
Closed mold processes

6. Hot press molding : Heated matched dies or tools are loaded with raw material
Compression molding (Sheet molding compound (SMC), dough molding
compound (DMC), cloth or unidirectional pre-peg.) pressed
to the shape of the cavity and cured.
7. Injection molding : Molten or plasticized polymer mixed with short fibers is
Transfer molding injected, usually at high pressure, into the cavity of a split
and allowed to solidify on curing.
8. Pultrusion : A continuous feed of fibers, in pre-selected orientations is
impregnated with resin and poured through a heated die to
give the shape of the final section (e.g., tubes or I-beam).
Partial or complete cure occurs during passage through the
die.
9. Cold press molding : A low pressure, low temperature process in which fibers are
impregnated with resin and then pressed between matched
dies. Heat is generated during the cure.
10. Resin injection : Fibers in cloth form are placed in the tool, which is then
closed. The resin is injected at low pressure into the cavity
flows through the fibers to fill the mould space.
11. Reinforced reaction : Involving compounds which are mixed immediately before
injection molding injection is used. Fibers are either placed in the closed mold
(RRIM) before resin is injected or added as short fibers to one of the
resin components to form slurry before injection.
54
3.3.6 Deformation of material
When an engineering material (as composite) is subjected to forces, such as those typically
imposed by service loads, its atoms may be displaced from their equilibrium positions. Any
displacement from the position or separation results in an energy increase. This requires work,
which is supplied by the forces creating the displacement. Thus it is clear that this premise holds
whether the material is stretched, causing the atoms to separate, thus bringing attractive forces
into play, or compressed, bringing the atoms closer together and causing repulsion [28].
3.3.6.1 Elastic deformation
The displacement of atoms from their equilibrium positions constitutes deformation. Such
deformation is termed elastic if the atoms can resume their equilibrium positions when the
imposed forces are released. Elastic deformation then is recoverable and indicates the relative
resilience of a material. For example, a rubber band can be stretched quite far yet snap back to its
original dimensions upon being released. A slightly different manner of stating this concept of
elasticity is that it is the property of a material to return to its initial form and dimension after the
deforming force is removed. The process of elastic deformation is presented schematically in the
Fig. 3.8. Here the atoms are represented as “hard” spheres on a lattice, when no forces are
applied, the assume equilibrium separation (a). A relatively small tensile force tends to pull the
atoms apart producing elastic deformation (σE). Their separation is now slightly larger than ao.
However, when the force is released, the atoms resume their equilibrium positions and no
deformation or displacement remains. The material is restored to its initial condition.
3.3.6.2 Plastic deformation
On the other hand, if the engineering material undergoes deformation which exceeds the elastic
capability (elastic limit) to restore the atoms to their equilibrium positions, the deformation is
permanent and termed plastic. Plastic deformation is non-recoverable and leaves the atoms
permanently displaced from their original positions where the forces are released. Deformation
of materials may be entirely elastic, or elastic plus plastic. The total deformation may then
55
Schematic illustration of deformation figures are shown in below:
Fig. 3.8: Schematic illustration of (a) elastic deformation and (b) plastic deformation.
56
consist of the combined elastic and plastic portion. In this case, removal of the load or forces
producing the deformation results in recovery of the elastic portion, while the plastic portion
remains. This process is illustrated in Fig. 3.8.
Plastic deformation of engineering materials is permanent in that work or energy must be

supplied to restore the atoms to their original equilibrium positions. For instance, the effect of
this type of deformation can be alleviated by thermal treatments, when necessary [28].
3.3.7 Characteristic parameters of composite materials
Mechanical properties of an engineering material are manifested by average strain (i. e.,
engineering strain), true strain, average stress (i.e., engineering stress), true stress, shear strain,
Poison’s ratio, elastic modulus, tensile strength and toughness [41].
The engineering strain (ε) is related to the true strain (εtr) as follows:
ε ln ε 1 (3.5)
And the engineering stress (σ) is related to the stress (σtr) as:
σ σ ε 1 (3.6)
3.3.7.1 Critical volume fraction
The critical volume fraction is defined as the volume fraction of fibers above which the fibers
being to strengthen rather than weaken the matrix. The critical volume fraction may be
calculated using the following equation.
v (3.7)
Here σm and σf are the ultimate tensile strength (UTM) of the matrix and fiber respectively and
σm* is the stress on the matrix from the stress-strain curve at a strain value where the ultimate
57
tensile strength of the fiber is reached. The critical volume fraction, vcrit, for composite decreases
with fibers of increasing strength with the other factors remaining the same.
3.3.7.2 Tensile strength
For all values of strain
σ σ́ V σ́ V (3.8)
Where σ represents the stress value at a particular strain value and V represents the volume
fraction of the components in the composite. The subscripts c, f and m represent the composite,
fiber and matrix respectively.
For Vf < Vcrit, σc = σmVm
For Vf > V crit , σm = σm Vf + σm*Vm (3.9)
3.3.7.3 Ultimate tensile strength
Using the equation (3.8) and the terms for stress specified in critical volume fraction, the
ultimate tensile strength (UTS) of the composite can be calculated as:
σc = σm Vf + σm*Vm (3.10)
Here, σm* represents the stress on the matrix from the stress-strain curve at a strain value where
the ultimate tensile strength is reached. This equation is based on the assumption that the
composite fractures when the fibers fail.
3.3.7.4 Elastic modulus
The elastic modulus (E) is a measure of the stiffness of an engineering material. Examination
reveals that for a given stress, greater values of E result in smaller elastic strains, meaning that
the higher the elastic modulus, the smaller the elastic strains. That is, the higher the elastic
58
modulus, the smaller the response of the structure to a particular stress. This parameter is
important for design and analysis purposes, especially in computing the allowable displacements
and deflections of engineering components or structure.
Although the modulus of elasticity is a structure insensitive property, it is affected by

temperature. As temperature is increased, E decreases, thereby reducing the stiffness of a
material. This reduction in elastic behavior is due to an inverse relationship between the modulus
and the inter-atomic or inter-ionic distance in metals and ceramics respectively.
Case I: Within the strain limits where the fiber and the matrix are in elastic deformation, the
modulus for the composite can be calculated using the rule of mixture equation.
Ec = Ef Vf + EmVm (3.11)
Where, Ec, Ef and Em are the modulus of elasticity of the composite, fiber and matrix
respectively, and Vf and Vm are the volume fraction of the fiber and the matrix respectively.
Case II: Within the strain limits where the fiber is in elastic whereas the matrix is in plastic
deformation, the equation is
Ec = Ef Vf + σmVm (3.12)
Where, σm is the slop of the stress-strain curve of the matrix at a given strain beyond the
proportional limit of the matrix.
3.3.7.5 Toughness
Toughness is a mechanical term that is used to several contexts; loosely speaking, it is a measure
of the ability of a material to absorb energy up to fracture. Specimen geometry as well as the
manner of loading application is important in toughness determinations. For dynamic loading
condition and when a notch is present, notch toughness is assessed by using an impact test.
Fracture toughness is a property indicative of a material’s resilience to facture when crack is
present.
59
For the static (low strain rate) situation, toughness may be ascertained from the result of a tensile
stress-strain test. It is the area under the σ–ε cure up to the point of fracture. For a material to be
tough it must display both strength and ductility; often, ductile materials are tougher than brittle
ones. Brittle materials have higher yield tensile strength; but lower toughness than ductile ones.
3.3.8 Application of composite materials based on plastics
Some applications of polymer matrix composites have been listed below.
Application area Examples

Aerospace Space structures, satellite antenna, rocket motor cases, high pressure
fuel tanks, nose cones, launch tubes etc
Aircraft Fairings, access doors, stiffeners, floor beams, entire wings, wing
skins, wing spars, fuselages, vertical and horizontal stabilizers,
landing gears, helicopter blades etc.
Automobile Body panels, dashboards, frames, cabs, spoilers, lamp-housings,
front-end panels, bumpers, leaf springs, seat housings, drive shafts
etc.
Chemical Pipes, tanks, pressure vessels, hoppers, valves, pumps, impellers,
gaskets etc.
Domestic Interior and exterior panels, chair , tables, ladders, handle of brush,
baths, shower units etc
Electrical Panels, housings , switchgears, insulators, connectors etc.
Leisure Tennis racquets, ski poles, skis, golf clubs, swimming pools, canoes,
protective helmets, fishing rods, playground equipment, bicycle
frames etc
Marine Hulls, decks, masts, engine shrouds, interior panels etc.
Medical Prosthesis, wheel chairs, orthofies, medical equipment etc
60
3.4 Electrical Properties of Polymer Composite
3.4.1 Conduction mechanism in solid
The electrical conduction may occur through the movement of either electrons or ions in
insulation solids. It may be contribution to the conductivity from several different types of
carries that is electrons and holes in electronic conduction and cation and anion pairs in ion
conduction. The most of the insulating materials, it is very difficult to observe any electronic
conductivity and whatever conductivity there is, it usually depends on the movement of
adventitious ions [46]. Therefore (a) Ionic conductivity and (b) Electronic conductivity are all
improvement in their own way insulation solids. Again the electronic conductivity may be (i)
Band conduction and (ii) Hopping (Tunneling) conduction.
(a) Ionic conduction
The ionic conduction in bulk material occurs due to the drift of defect under the influence of an
applied electric field. The degrees of ionic impurities which may be totally ignored in the context
of other properties may have a significant effect on conductivity. A theoretical expression may
be derived, for the current density, following through a sample, on the basis of simple model and
is given by
eaE
J ∝ sinh (3.13)
2kT
Where, E is the electric field and a is the distance between neighboring potential wells.
(b) Electric conduction
(i) Band conduction: In insulating solids electronic conduction may differ in several important
ways from the more familiar kind in metals and inorganic semiconductors. That is not to say that
they are separate subjects.
(ii) Hopping conduction: Both energetic and spatial distributions of electronic states are
affected by the property of disorder in a lattice. For a random distribution of atoms, the density
of electronic energy states tails into what is normally forbidden zone electron in this tails are
localized, when the electrons are excited to higher energy, conduction via localized electron
61
implies discrete jump across an energy barrier from one site to next. An electron may either
“hop” over or “tunnel” through the top of the barrier, and the availability of the relative
importance of these two mechanisms depending on the shape of the barrier thermal energy. For
variable range hopping, the electrical conductivity is given by,
To 1 / d +1
σ = σ o exp− ( ) (3.14)
T
Where, d → Dimensionality of transport (e.g., d = 2 for two dimensional motion etc.)
σ → Electrical conductivity
σ o → Initial values of conductivity
T o → Activation energy in terms of temperature
T → Absolute temperature
3.4.2 Theory of dielectrics
A material is classified as ‘dielectric’ if it has the ability to store energy when an external electric
field is applied. If a dc voltage source is placed across a parallel plate capacitor, more charge is
stored when a dielectric material is between the plates than if no material (a vacuum) is between
the plates. The dielectric material increases the storage capacity of the capacitor by neutralizing
charges at the electrodes, which ordinarily would contribute to the external field. The
capacitance with the dielectric material is related to dielectric constant. If an ac sinusoidal
voltage V is placed across the same capacitor (Fig. 3.9), the resulting current will be made up of
a charging current Ic and a loss current Il that is related to the dielectric constant. The losses in
the material can be represented as conductance (G) in parallel with a capacitor (C) [47].
I
+
A
V ‐ ‐ ‐ C G
‐ ‐
t + +‐ + +‐ + +‐ + +‐ +
Fig. 3.9: Parallel plate capacitor (AC case).
62
3.4.2.1 Dielectric polarization and its classification
A dielectric is subjected to a homogeneous field carries a dipole moment per unit volume. Dipole
moment per unit volume is called the polarization of the dielectric. When a polymer is subjected
to the influence of an applied electric field, different processes of polarization take place due to
the distortion and alignment of the molecules. With changing the field, both the distortion of the
molecules and their average orientations change. Different types of polarization occur at
different range of frequencies. The total polarization is consists by the following four types of
polarization:
Electronic polarization: If the atom is in the absence of the field then the system is neutral one
and has no dipole moment. In the absence of the field the system is still neutral, but has a non-
zero dipole moment because the nucleus and the centre of charge cloud are separated by a certain
distance. In this case the atom carries a dipole moment and this dipole moment is proportional to
the field strength and the proportionality factor is called the electronic polarizability of the atom.
The term “electronic” used here as this dipole moment results from a shift of the electron cloud
relative to nucleus.
Orientational polarization: If two different atoms A and B form a chemical bond, one of the
two is more apart with one or more of its valence electrons than the other. As a result, the bond
between A and B is at least partly ionic. If the bond between A and B has ionic character, it is
obvious that the molecule AB carries an electric dipole moment even in the absence of an
applied field, such a dipole moment is called permanent. The magnitude of the dipole moment is
given by the product of the average charge transferred from A to B and the internuclear distance.
For a molecule consisting of more than two atoms, several bonds may carry a permanent dipole
moment of the molecule as a whole is obtained by vector addition of the moments associated
with the various bonds. When an external field is applied to a molecule carrying a permanent
dipole moment, the permanent dipole moment aligns along the direction of the field. The
contribution of this process of orientation of the permanent dipoles to the polarization is called
orientational polarization.
Ionic polarization: When in a molecule some of the atoms have an excess positive or negative
charge (resulting from the ionic character of the bonds), an electric field will tend to shift
63
positive ions relative to negative ones. This leads to an induced moment of different origin from
the moment induced by electron clouds shifting relative to nuclei. The ionic polarization occurs
due to shift of the ions relative to each other.
Interfacial polarization: In a real crystal there inevitably exist a large number of defects such as
lattice vacancies, impurity centers, dislocations etc. Free charge carries, migrating through the
crystal, under the influence of an applied field, may be trapped by, or pile up against a defect.
The effect of this will be the creation of a localized accumulation of charge which will induce its
image charge on an electrode and give rise to a dipole moment. This constitutes a separate
mechanism of polarization in the crystal, and is given the name interfacial polarization.
The molar polarization of a material of a material is found to depend on the frequency of the
applied alternating electric field as shown in Fig 3.10.
α dipolar
Molar polarization, Rm
α atomic α electronic
103 106 109 1012 1015
Frequency (Hz)
Fig. 3.10: Dispersion of molar polarization in a dielectric (schematic).
In general the polarizability can be written as the sum of four terms i.e.,
α = αe + αa + αd + αi
Where, e is the electronic contribution, a is the atomic contribution, d is the dipolar contribution,
and i is the interfacial contribution.
64
3.4.2.2 Dielectric loss
When an electric field acts on any matter the latter dissipates a certain quantity of electric energy
that transforms into heat energy. This phenomenon is commonly known as ‘the expense’ or
‘loss’ of power, meaning an average electric power dissipated in matter during a certain interval
of time. Most of the dielectrics display a characteristic feature: under a given voltage the
dissipation of power in these dielectrics depends on the voltage frequency, the expense of power
frequency, voltage and capacitance and also depends on the material of dielectric.
The amount of power losses in a dielectric under the action of the voltage applied to it is
commonly known as ‘dielectric loss’. This is the general term determining the loss of power in
an electrical insulation both at a direct and an alternating voltage. If an alternating electric field E
is applied, which has amplitude Eo and angular frequency ω, across a dielectric material then
E = Eo cosωt
This will produce polarization which alternates in direction, and if the frequency is high enough,
the orientation of any dipoles which are present will inevitably lag behind the applied field.
Mathematically, this is expressed as a phase lag δ in the electric displacement. This parameter is
usually described by loss tangent, tanδ.
V = Voeiωt
Charging
V
Loss
Fig. 3.11: AC losses in a dielectric: (a) circuit diagram, and (b) simplified diagram of current
voltage relationship.
65
3.4.2.3 The Debye theory of dielectrics
A capacitor essentially consists of two conducting surface separated by a layer of an insulating

medium called dielectric. The conducting surfaces may be in the form of either circular or
rectangular plates or be of spherical or cylindrical shape. The purpose of a capacitor is to store
electrical energy by electrostatic stress in the dielectric. The capacitance of a parallel plate
capacitor having a dielectric medium is expressed as
C= (3.15)
Where, εo is the permittivity of free space, έ is the dielectric constant of the medium, A is the
surface area of each of the plates/electrodes and d is the thickness of the dielectric.
A real capacitor can be represented with a capacitor and a resistor. The parameters such as
angular frequency (ω) of the applied field, the parallel resistance Rp, parallel capacitance Cp, and
the series resistance Rs and series capacitance Cs are related to the dielectric constant έ , dielectric
dissipation factor ε And loss tangent as
έ = (3.16)
έ = (3.17)
and tanδ = = Gp/2πfCp (3.18)
The ac conductivity, σac, was calculated using eqn.
σ G d/A (3.19)
The dependence of ac conductivity, σac, on frequency may be described by the power law:
σ ω Aω (3.20)
Where, A is proportionality constant and ω is the angular frequency and n is the exponent, which
generally takes the value less than unity for Debye type mechanism and is used to understand the
conduction/relaxation mechanism in amorphous materials.
66
The dielectric behavior of a material is usually described by Debye dispersion equation:
ε ω, T ε′ iε′′ (3.21)
Where, ε*is the complex dielectric permittivity, ε′ (energy dissipated per cycle) is the real part of
complex dielectric permittivity and ε′′ (energy stored per cycle) is the imaginary part of the
complex dielectric permittivity.
ε ′ = ε∞ + (3.22)
ε ε∞ ωτ
ε′′ = (3.23)
ω τ
Where , εs is the static dielectric constant, ε∞ is the high frequency dielectric constant and the
quantity τ is a characteristic time constant, usually called the dielectric relaxation time, it refers
to a gradual change in the polarization following an abrupt change in applied field. The dielectric
loss tangent is expressed by
ε′′
tanδ = (3.24)
ε′
ε’ ε”
ωmax
εo
ε”
εx
log ωτ
Fig. 3.12: Debye dielectric dispersion curves.
The graphs of έ and ε" against frequency of the applied field (logarithmic scale) through the
dispersion regions show that the maximum loss value occurs when ωτ = 1, corresponding to a
67
critical frequency ωmax = 1/τ, and location of this peak provides the easiest way of obtaining the
relaxation time from the experimental results.
The activation energy (∆E) of the relaxation process is related to the relaxation time by the
Arrhenius equation:
∆
τ= = τo exp (3.25)
Where, fmax is the frequency of maximum loss for a given temperature, τo is a constant and T is
the absolute temperature and kB is the Boltzman constant. ∆E was evaluated in the present work
from the slope of the plot ln fmax, versus 1/T.
3.4.2.4 Dielectric nature of the polymer composites
It is well known that composites can be produced exhibiting enhanced properties that the
constituent materials may not exhibit. For instance, from the combination of different fibers or
fillers with polymer matrices one can produce polymer-matrix composites, a material important
to the electronic industry for its dielectric properties in the use capacitors [48]. The effective
utilization of filled polymers depends strongly on to disperse the fillers homogeneously
throughout the matrix. The interface properties also strongly affect the characteristics and
performance of these composites.
One of the most attractive features of these filled composites is that their dielectric properties can
be widely changed by choice of shape, size, and the conductivity of filled constituents in the
polymeric matrix. Most of the interesting properties of polymers are attributable to the complex
motions within their molecular matrix. In the polymeric system, molecular relaxations exhibit
various transitions. The polymeric interfaces act as charge – carrier trapping sites. Therefore, it
has become essential to study the effect of interfaces on the charge–carrier generation, transport
and storage in polymeric systems. The study of dielectric constant and dielectric loss as a
function of temperature and frequency is one of the most convenient and sensitive methods of
studying polymeric structure.
68
For polymer composites in the solid or visco elastic state, the physical structure is of great
importance in determining the dielectric behavior. The dielectric properties of polymer
composite materials have been studied with a view to modifying the properties of polymer
systems for practical applications. The conventional inorganic insulators and dielectrics have to a
large extent been replaced by polymers on account of their unique ability to be tailor made for
specific needs. Epoxies and polyesters have been used in electronics as insulators, dielectrics,
substrates, potting compounds, embedding materials and conformal coatings.
3.5 Theory of Thermal Analysis
Thermal analysis comprises of a group o techniques in which a physical property of a substance

is measured as a function of temperature, while the substance is subjected to a controlled
temperature programme [49–52]. Organic and inorganic polymers reinforced with natural fibers
may undergo structural, physical and chemical changes with temperature due to dehydration,
phase transition, molecular orientation, destruction of crystallinilty, oxidation and
decomposition, incorporation of some functional groups etc. A systematic investigation of
thermal behavior of polymers in gas, vacuum or in inert atmosphere provides information about
the nature of the changes of polymers. Such changes can conveniently be understood by
employing differential thermal analysis (DTA) and thermogavimetric analysis (TGA). These
analyses are techniques that rely on samples which decompose at elevated temperatures.
3.5.1 Differential thermal analysis
The technique of DTA is an important tool to study the structural and phase changes occurring
both in solid and in liquid materials during heat treatment. These changes may be due to
dehydration, transition from one crystalline from to another, destruction of crystalline structure,
melting, oxidation, decomposition, degradation temperatures, etc. DTA is a process of accurately
measuring the difference in the temperature between a thermocouple embedded to a sample and
a thermocouple in a standard inert material such as aluminum oxide while both are being heated
at a uniform rate [49].
69
The principal of DTA consists of measuring heat changes associated with the physical or
chemical changes occurring when any substance is gradually heated. The thermocouple
(platinum-platinum rhodium 13%) for DTA is incorporated at the end of each of the balance
beam ceramic tubes, and the temperature difference between the holder on the sample side and
the holder on the references side is detected. This signal is amplified and becomes the
temperature difference signal used to measure the thermal change of the sample. Fig. 3.13 shows
a schematic illustration of a DTA apparatus.
Fig. 3.13: Schematic diagrams showing different parts of a DTA apparatus.
These differences of temperatures appear because of the phase transitions or chemical reactions
in the sample involving the evolution of heat and are known as exothermic reaction or absorption
of heat known as endothermic reaction. The exothermic and endothermic reactions are generally
shown in the DTA traces as positive and negative deviations respectively from a base line. So
DTA offers a continuous thermal record of reactions in a sample. The areas under the bands or
peaks of DTA spectra are proportional to the amount of heat absorbs or evolved from the sample
under investigation, where temperature and sample dependent thermal resistance are the
proportionality factors. Thus DTA is needed primarily for the measurement of transition
temperature.
70
3.5.2 Thermogravimetric analysis
The TGA is a special branch of thermal analysis, which examines the mass change of a sample
as a function of temperature in the scanning mode or as a function of time in the isothermal
mode. Not all thermal events bring about a change in the mass of the sample (for example
melting, crystallization or glass transition), but there are some very important exceptions which
include absorption, sublimation, vaporization, oxidation, reduction and decomposition. The TGA
is used to characterize the decomposition and thermal stability of materials under a variety of
conditions, and to examine the kinetics of the physico-chemical process occurring in the sample.
Sample weight changes are measured as described in Fig.3.14.
Figure 3.14 shows the sample balance beam and reference balance beam are independently
supported by a driving coil/pivot. When a weight change occurs at the beam end, the movement
is conveyed to the opposite end of the beam via the driving coil/pivot, when optical position
sensors detect changes in the position of a slit. The signal from the optical position sensor is sent
to the balance circuit. The balance circuit supplies sufficient feedback current to the driving coil
so that the slit returns to the balance position. The current running to the driving coils to the
sample side and the current running to the driving coil on the reference side is detected and
converted into weight signals.
Heater
Reference holder Electro-magnetic
Sample
Optical
Heater
position
Fig. 3.14: A pictorial set-up for TGA measurements.
71
3.5.3 Differential thermogravimetry
Differential thermogravimetry is termed as DTG. If not the weight itself rather the first
derivative of the sample weight with respect to time at constant temperature or with respect to
temperature at constant value of heating is determined then this procedure is termed as DTG.
3.6 Theory of infrared spectroscopy
Infrared (IR) spectroscopy is an extremely effective method for determining the presence or
absence of a wide variety of functional groups in a molecule. Infrared spectroscopy measures
different IR frequencies by a sample positioned in the path of an IR beam and it reveals
information about the vibrational states of a molecule.
The main goal of IR spectroscopic analysis is to determine the chemical functional groups in the
sample. Different functional groups absorb characteristic frequencies of IR radiation and this
absorption results due to the changes in vibrational and rotational status of the molecules.
Actually, a molecule, when exposed to radiation produced by the thermal emission of a hot
source (a source of IR energy), absorbs only at frequencies corresponding to its molecular modes
of vibration in the region of the electromagnetic spectrum between visible (red) and short waves
(microwaves). These changes in vibraional motion give rise to bands in the vibrational spectrum;
each spectral band is characterized by its frequency and amplitude. The absorption frequency
depends on the vibrational frequency of the molecules, whereas the absorption intensity depends
on how effectively the infrared photon energy can be transferred to the molecule, and this
depends on the change in the dipole moment that occurs as a result of molecular vibration. As a
consequence, a molecule will absorb infrared light only if the absorption causes a change in the
dipole moment. Thus, all compounds except for elemental diatomic gases such as N2, H2 and O2
have infrared spectra and most components present in a flue gas can be analyzed by their
characteristic infrared absorption. Furthermore, using various sampling accessories, IR
spectrometers can accept a wide range of sample types such as gases, liquids, and solids. Thus,
IR spectroscopy is an important and popular tool for structural elucidation and compound
identification.
72
3.6.1 Infrared frequency range and spectrum presentation
Infrared radiation spans a section of the electromagnetic spectrum having wave-numbers from
roughly 3000 to 10 cm-1, or wavelength from 0.78 to 1000 µm. IR absorption positions are
generally presented as either wave-numbers ( ) or wavelengths (λ). Thus, wave-numbers are
directly proportional to frequency, as well as the energy of the IR absorption. In the contrast,
wavelengths are inversely proportional to frequencies and their associated energy. Wave-
numbers and wavelengths can be inter-converted using the following equation:
v cm 10 (3.26)
λ µ
Table 3.3: Three smaller areas in IR region.
Near IR Mid IR Far IR

Wave-number 13000–4000 cm-1 4000–200 cm-1 200–10 cm-1
Wavelength 0.78–2.5 µm 2.5–50 µm 50–1000 µm
The IR region is commonly divided into three smaller areas: near IR, mid IR, and far IR. Three
region of most interest for chemical analysis is the mid-infrared region (4,000 to 400 cm-1) which
corresponds to changes in vibratinal energies within molecules. The far infrared region (400 to
10 cm-1) is useful for molecules containing heavy atoms such as inorganic compounds but
requires rather specialized experimental techniques. The far and near IR are not frequently
employed because only skeletal secondary vibrations (overtones) occur in these regions
producing spectra that are difficult to interpret.
3.6.2 Infrared absorption
At temperatures above absolute zero, all the atoms in molecules are in continuous vibration with
respect to each other. When the frequency of a specific vibration is equal to the frequency of the
IR radiation directed on the molecule, the molecule absorbs the radiation.
73
For a molecule to absorb IR, the vibrations or rotations within a molecule must cause a net
change in the dipole moment of the molecule. The alternating electrical field of the
electromagnetic radiation interacts with fluctuations in the dipole moment of the molecule. If the
frequency of the radiation matches the vibrational frequency of the molecule then radiation will
be absorbed, causing a change in the amplitude of molecular vibration. The energy of a molecule
consists of translational, rotational, vibration, and electronic energy
E = E electronic + E vibrational + E rotational + E translational
Translation energy of a molecule is associated with the movement of the molecule as a whole,
for example in a gas. Rotational energy is related to the rotation of the molecule, whereas
vibrational energy is associated with the vibration of atoms within the molecule. Finally,
electronic energy is related to the energy of the molecule’s electrons.
Like radiant energy, the energy of a molecule is quantized too and a molecule can exist only in
certain discrete energy levels. Within an electronic energy level a molecule has many possible
vibrations energy levels. The vibrational energy of a molecule is not determined by the orbit of
an electron but by the shape of the molecule, the masses of the atoms and, eventually by the
associated vibronic coupling. For example, simple diatomic molecules have only one bond
allowing only stretching vibrations. More complex molecules may have many bonds, and
vibrations can be conjugated. The atoms in a CH2 group, commonly found in organic
compounds, can vibrate in six different ways: symmetrical and antisymmetrical stretching,
scissoring, rocking, wagging and twisting.
The major types of molecular vibrations are stretching and bending. The various types of
vibrations are illustrated in Fig. 3.15. Infrared radiation is absorbed and the associated energy is
converted into these types of motions. The absorption involves discrete, quantized energy levels.
However, the individual vibrational motion is usually accompanied by other rotational motions.
These combinations lead to the absorption bands, not the discrete lines, commonly observed in
the mid IR region.
Stretching: Change in inter-atomic distance along bond axis. There are two types of Stretching
vibrations: Symmetric and Asymmetric.
74
Bending: Change in angle between two bonds. There are four types of bend: Rocking,
Scissoring, Wagging, and Twisting.
Symmetrical Asymmetrical
Stretching
+ + + ‐
Rocking Scissoring Wagging Twisting
In‐plane deformations Out‐of‐plane deformations
Bending
Fig. 3.15: Stretching and bending vibrations.
In general, a polyatomic molecule with n atoms has 3n – 6 distinct vibrations. Each of these
vibrations has an associated set of quantum states and in IR spectroscopy the IR radiation
induces a jump from the ground (lowest) to the first excited quantum state. Although
approximate, each vibration in a molecule can be associated with motion in a particular group.
75
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79
Chapter 4 Materials and Methods
MATERIALS AND METHODS

4.1. Materials
4.1.1 Raw materials
Principal raw materials used for the samples are:
(a) Polyester resin

(b) Hardener
(c) Banana fiber and
(d) Sodium hydroxide
(a) Polyester resin is obtained from the local chemical market (commercial grade). Resin are
high molecular weight synthetic organic compounds, which are made by a chemical reaction
between two or more molecules of same or different compounds, usually with heat, pressure, and
catalyst. This particular reaction is called polymerization and products known as polymer. The
starting materials are called monomer. Polymers are made by a cross-linking of monomer
molecules. The molecular weight of polymer is a full number multiple of the molecular weight of
monomer of which it is made. However, resin may be regarded as intermediate products of
polymerization reaction in which phenomena of polymerization or cross linking between all
molecules has not been completed.
Resin is divided into two distinct groups. First is thermosetting resin and second one is
thermoplastic resin. Thermosetting resins are set or harden on heating into a permanent shape
due to an irreversible cross-linking reaction. Polyester resin is one of example of thermosetting
resin. On the other hand, thermoplastic resins do not undergo any permanent change on heating
and therefore can be reshaped any number of times.
(b) Hardener (methyl-ethyl ketone peroxide “MEKP”) is collected from the local chemical
market (commercial grade). In practice the peroxide curing system is blended into the resin
before applying the resin to the reinforcement. The peroxide is referred to as catalysts (though,
strictly speaking, these are polymerization initiators) for room temperature curing of polyester
resin.
80
(c) Figure 4.1 shows raw banana fiber, which is obtained from the stem of the banana plant
(shown in Fig. 3.1). It is obtained from the species Musa cavendishior Musa sapientum. About
37 kg (average weight) of stem yields about 1 kg of good quality fiber; the yield is 1–1.5%.
Fig. 4.1: Raw banana fiber extracted from banana plants.
(d) For the treatment of banana fibers with alkali, Sodium hydroxide (NaOH) (97% pure, Merck,
India) is collected from local chemical market.
4.2 Methods for Preparation of Banana Fibers
4.2.1 Collection and separation of fiber from their plants
A variety of banana fiber was collected from banana plant of this local area (Dhaka residential
model college campus). The fiber was about 30–150 cm long. These fibers can be extracted by
hand scraping, by retting, or by using raspador machines; it can also be extracted chemically, for
example by boiling in NaOH solution. When banana plants get mature, the bark of the plant was
cut down in small pieces and separated layers tied up in bundles. The bundles of plant were put
under close and dirty water in a pond for 15 days. When rotten, the fiber was taken out from the
plant layers and washed thoroughly with water several times and dried in air without exposure
sunlight.
81
4.2.2 Scouring of the fiber
The removal of impurities such as dirty materials and gummy substances from textile materials
are called scouring. It is carried out by the use of surface-active agents, such as soda and
detergents. Detergent agents were not used in this present work. The fibers were thoroughly
washed only with distilled water and dried in the open air and finally stored in a desiccator.
4.3 Methods for Preparation of Composites
4.3.1 Treatment of fibers with NaOH
Raw banana fibers were treated with NaOH solution to extract impurities from banana fiber,
such as hemicellulose, lignin, aromatic acids, esters etc. which might weaken the adhesion
between fibers and matrix. Banana fibers were immersed in 5% NaOH solution only for
removing the cementing agents (hemicellulose, lignin, pectin etc.). The treatment time was 1, 2
and 5 h at room temperature. It was reported that over treatment of natural fibers using NaOH
could have a negative effect on the base fiber properties [1]. Finally, the fibers were washed with
distilled water to neutralize the NaOH solution. They were dried at 80 oC for 24 h. The NaOH
treatment steps followed for the samples are given in Table 4.1.
4.3.2 Fiber cutting
To get sized fiber bundles (treated/untreated) were cut into length of about 60 mm, average, with
its help of a knife. This fiber kept at a dry environment for seven days for the partial removal of
moisture.
4.3.3 Hand lay-up
A milute paper was placed on dried S/S sheets. A mixture of polyester resin (filler) and hardener
was spread evenly on S/S sheets. Then required banana fibers as weight percentage were placed
on the resin. Fibers were aligned in the same direction and spread up over the resin as possible as
82
minimized voids. Again mixture resin was spread on the banana fibers. Then another milute
paper was placed over the mixture. The balance of the mixture was made up of the polyester,
always to give a total weight batch size of 100%. Finally, banana fiber reinforced polyester resin
composites were produced using molding method.
4.3.4 Casting
A special molding device is made by steel to very close tolerance for the molding process. The
mixture of fiber and matrix is cast by simply pouring the mixture into the mold and sufficient
pressure of 20 kg is applied to get the desired shape and possible homogeneity. This pressure
was kept for one hour. After that remove the composite from milute paper and cut it along 60
mm length and 10 mm width for mechanical measurement and around 10 mm diameter for
electrical measurement. The sample descriptions are summarized with NaOH treatment steps in
Table 4.1.
Table 4.1: The NaOH treatment steps followed for the samples.
Sl. Sample description Sample code NaOH Fiber
No. treated content
time (h) (wt.%)
1 Polyester resin PR - -
2 Untreated banana fiber UBF - -
3 Treated banana fiber TBF1 1 -
6 Untreated banana fiber-polyester resin composite UBF-PR(5%) 0 5
9 Treated banana fiber-polyester resin composite TBF1-PR(5%) 1 5
83
4.4 Methods for Measuring Physical and Mechanical Properties
To evaluate the properties of prepared composite the following test are performed:
1. Measurement of bulk density

2. Measurement of water absorption
3. Tensile strength testing
4. Flexural strength testing
4.4.1 Equipments used for the testing of samples (Physical and Mechanical)
For the testing of the samples the following equipments are used-
1. Hounsfield test equipment

2. Electronic balance
3. Oven
UTM machine (Hounsfield test equipment)
Hounsfield UTM 10kN (H10KS) was used for test of tensile and flexural strength, compression
shear and other mechanical and physical properties of materials. The following photograph (Fig.
4.2) shows the machine.
Fig. 4.2: Photograph of UTM machine.
84
Electronic balance
A digital balance (RADWAG, AS220/C/2, Poland) was used for measurement of weight of the
sample. The balance is sensitive and it can measure 0.0001 g capacity.
Oven
The oven (Memmart, UE600) was used for removing moisture content at 80 oC for 24 h.
4.4.2 Measurement of bulk density
The bulk density of the composites was determined according to ASTM C 134-76 [2] by using
the formula
D = Ws / V (4.1)
Where, D = Density of the specimen, kg/m3
Ws = mass of the specimen, kg, and
V = Volume of the specimen, m3.
4.4.3 Water absorption /Water intake
The water absorption test of the composites was carried out according to ASTM D 570-81 [3]
*{ASTM Designation: D 570-81 (Reapproved 1988) Standard test method for water absorption
of plastic. 141-143 ;}. The test specimens was 60 mm length, width above 10 mm. Description of
the procedure are given below.
Conditioning:
Three specimens for each batch were conditioned as follows:
¾ The cut edges were made by finishing with No.0 Emery paper.
¾ Dried in oven (Time: 24 h, Temp.: 80 oC).
¾ Cooled in a desiccator and immediately weighed to the nearest 0.001 g (Wc).
Repeated immersion:
¾ The conditioned specimens were placed in a container of distilled water at a temperature
of 23 + 1 oC, made rest on edge and entirely immersed.
85
¾ Kept there for 1 h.

¾ Removed the specimen one at a time.
¾ The surface water wiped off with a dry tissue paper and immediately weighed to the
nearest 0.001 g (Ww).
¾ Repeat of the process after 2, 3, 6, 12, 24, 48, and 72 h.
Reconditioning:
¾ Dried in oven for 24 h at 80 oC.
¾ 2. Cooled in a desiccator.
¾ Immediately weighed to the nearest 0.001 g (Wrc).
Calculations:
At last the total water absorption was calculated following the rules given below.
¾ Increase in weight, %Wi = (Ww-Wc)÷Wc×100.
¾ Soluble matter lost, %Ws = (Wc-Wrc)÷Wc×100.
¾ % water absorbed, W = Wi + Ws.
In all cases a protective gel coat (araldite) was applied on the cut sides to prevent penetration of
water from cut sides.
4.4.4.1 Tensile test
The tensile test of the composites was performed according to ASTM D 3039/D 3039/M-00 [4].
Test specimen:
The test specimens were sawed from the composite samples so as to have smooth edges free
from cracks. The cut edges were made smooth by finishing with No. 0 Emery cloth. The
specimens were in the form of rectangular bars of 60 mm by 10 mm by thickness.
Test steps:
¾ Before the test to be carried out, the specimens were kept in the incubator (Memmart) at
80 oC for 24 h, then removed and cooled in the desiccator.
86
¾ The preconditioned test specimen was gripped into the jaws of the Universal Testing
Machine with 10 kN load cell for tensile test such that the length of the specimen
between the tips of the jaws was 40 mm, i.e., the gage length of the sample was 40 mm.
The test was monitored with a computer through QMat Professional ( Tinius Olsen, UK)
software.
¾ The test was carried out to failure at the cross-head speed of 2 mm/min.
¾ Tensile strength, tensile modulus, and energy were easily found from the software output.
¾ Average was obtained from the results of three specimens for each batch.
4.4.4.2 Theory for determining tensile properties from load Vs displacement curve
If there are not equipped with the QMat Professional software, the tensile properties can be
determined from the force versus displacement curve of the test specimen.
Tensile strength (Ultimate Tensile Strength or UTS): Tensile strength (σ) is defined as the
ratio of the load (P) needed to fail the specimen to its initial cross-sectional area (A).
P
σ= (4.2)
Tensile strain: Tensile strain (ε) is defined as the ratio of the total extension to the initial length
(Li). If Lf is the final length of a material,
ε= (4.3)
% elongation = x 100 (4.4)
Young’s modulus: The slope of the initial straight-line portion of the stress-strain curve is the
elastic modulus of a material. In a tensile test, this modulus is Young’s modulus and is calculated
by:
E= (4.5)
Where, dσ = Stress at yield σy

dε = strain at yield εx.
87
Energy calculation: The total energy absorbed by a specimen is calculated from the area under
the load versus displacement curve of that specimen. The area under the curve is calculated by
using the trapezoidal method as shown in Fig. 4.3.
Let us consider a segment where the X values are from X1 mm to X2 mm and the corresponding
Y values are from Y1 N to Y2 N respectively.
So the width of the defined trapezoid = (X2 –X1) mm
The average height = N
So, the area of the trapezoid, A = width × average height
= (X2 –X1) × N-mm
Fig. 4.3: Typical tensile load Vs displacement curve.
The energy absorbed per cross-section = kJ/m2 (4.6)
Where, A is the cross-sectional area (in mm2) of the specimen.
Similarly, the area under all the segments can be calculated and then by summing up all the
values of these segments, the total area under the curve can be obtained.
88
Thus, the total energy absorbed will be = ∑ A

And the total energy absorbed per unit cross-sectional area
∑
= (4.7)
But, in the present study, all the tensile results were directly observed from the output of the
QMat Professional software, and, therefore, the procedure above did not need to be executed.
4.4.5.1 Flexural test:
The flexural tests (3-point bending) were carried out according to ASTM D790-00 [5].
Test specimen
The test specimens were in the form of rectangular bars of by 60 mm by 4d (d = thickness of the
specimen) mm by thickness. The specimens were first cut from the composite samples by
sawing, and then the cut edges were polished with No. 0 Emery cloth.
Fig. 4.4: Typical flexural test set-up for polymer composites.
Test steps
¾ Prior to test to be run, the specimens were kept in the incubator (Memmart) at 80o C for
24 h, then remove and cooled in the desiccator
89
¾ The preconditioned specimen was place flat on the support rods of the three points
bending system maintaining a span length of 16d (d = thickness of the specimen). The
loading nose of the UTM with a 110 kN load cell was brought in contact to the upper
surface at the mid span of the sample.
¾ The test was performed at crosshead speed of that was determine d by the following
equation:
R= (4.8)
Where, R = rate of crosshead motion, mm/min

L = support span, mm
D = depth of beam, i.e., thickness of the sample, mm
Z = rate of straining of the outer fiber, mm/mm/min. ‘Z’ should be equal
to 0.01.
4.4.5.2 Theory for determining flexural properties from load Vs deflection curve
If there are not equipped with the QMat Professional software, the flexural properties would be
determined from the load versus deflection curve of the test specimen.
Flexural stress (σf): When a homogeneous elastic material is tested in flexural as a simple beam
supported at two points and loaded at the midpoint, the maximum stress in the outer surface of
the test specimen occurs at the midpoint. This stress may be calculated for any point on the load-
deflection curve by means of the following equation:
P
σf = (4.9)
Where, σf = stress in the outer surface at midpoint, MPa

P = load at a given point on the load-deflection curve, N
b = width of beam tested, mm
d = depth of beam tested, mm
Equation 4.9 applies strictly to materials for which stress is linearly proportional to strain up to
the point of rupture and for which the strains are small. Since this is not always the case, a slight
90
error will be introduced if equation 4.9 is used to calculate stress for material that are not true
Hookean material. The equation is valid for obtaining comparison data and for specification
purposes, but only to a maximum fiber strain of 5% in the outer surface of the test specimen.
Flexural strength (σfm): This is defined as the maximum flexural stress sustained by the test
specimen during a bending test. It is calculated according to equation 4.9.
Flexural strain (εf): This is the nominal fractional change in the length of an element of the
outer surface of the test specimen at mid span, where the maximum strain occurs. It may be
calculated for any deflection using the following equation:
εf = (4.10)
Where, εf = strain in the outer surface, mm/min

D = maximum deflection of the center of the beam, mm
Tangent modulus of elasticity or flexural modulus (EB): The tangent modulus of elasticity,
often called the ‘modulus of elasticity’, is the ratio, within the elastic limit, of stress to
corresponding strain. In a flexural test, this is flexural modulus. It is calculated by drawing a
tangent to steepest initial straight-line portion of the load-deflection curve and using equation
4.11.
EB = (4.11)
Where, EB = modulus of elasticity in bending, MPa

b = width of beam tested, mm
m = slope of the tangent to the initial straight-line portion of the load-deflection
curve, N/mm
But, in the present study, all the flexural results were taken from the output of the QMat
Professional software instead of executing the procedure.
91
4.5 Methods for Measuring Electrical Properties
4.5.1 Instrument used for electrical measurements
Different types of equipments used for Ac measurements are as follows:
(a) Oil rotary pump

An oil rotary pump was to evacuate the specimen chamber. A pressure of about 10-² torr can be
attained using this pump.
(b) Keithley microvolt meter

A digital Keithley autoranging microvolt meter MVM (Model 197 A) was used for the
measurement of e.m.f across a Chromel–Alumel (Cr–Al) thermocouple attachéd to the specimen.
(c) Specimen chamber

Specimen chamber shown in Fig.4.5 is designed and fabricated in the laboratory with the help of
university workshop. It consists of two main parts, mainly the stainless steel tube and the sample
holder (Fig. 4.6). A stainless steel tube having inner diameter of 0.045 m and length 0.24 m is
used. The lower end of the tube is closed by welding a circular piece of stainless steel. At the top
of the tube one flat stainless steel sheet (0.092 x 0.09 m2); with a circular hole (diameter 0.045
m) at its center is welded. Another stainless with a hole of the same dimension is welded to a
stainless steel tube of diameter 0.045 m and of length 0.24 m. A O–ring is placed in between the
two stainless steel sheets. This prevents the air leakage when it is evacuated. The upper portion
can be fixed to the lower portion by screws. The top opening is closed tightly with teflon stopper.
Two copper leads (electrodes) which hold the specimen holder and a (Cr–Al) thermocouple are
inserted through this teflon stopper. A thick layer of mica sheet is placed on to the inside wall
and bottom of the stainless steel tube for electrical insulation. The distance between the leads is
about 0.014 m. This is a side tube welded to the main stainless steel tube which acts as an outlet
of the chamber. A rotary vacuum pump is connected to the chamber through the side tube with
the help of rubber tube. By this pump a pressure of about 10 −2 torr can be obtained. Required
temperature in the chamber can be maintained by a heating tape which is wrapped outside the
steel tube and its temperature is controlled by a variable transformer. Sample holder is a spring
system.
92
Fig. 4.5: The schematic diagram of the specimen chamber.
(d) Heating tape

A heating tape (ISOPAD LTD BOREH AMWOOD, HERTS, ENGLAND)was used to heat the
specimen chamber. It is about 1.75 m long and 0.03 m width tape. It can be wrapped around the
specimen chamber easily.
(e) Variac
A Yamabishi volt-slider (Type SS-260-10 NO. 38 -1) was connected to the heating tape.
93
(f) Impedance analyzer

The impedance analyzer (Model AGILENT 4192 A) was used for ac measurements. By this we
can measure 5 Hz – 13 MHz.
Specimen Chamber Specimen Holder
Fig. 4.6: Photographs of the specimen chamber and holder.
4.5.2 AC electrical measurements for conductivity and dielectric
The samples were cut into circle in shape having 10 mm diameter and (0.95 – 0.98) mm
thickness and polished by sand paper to remove any roughness of the samples. AC electrical
measurements samples coated with silver paste on both sides of the polished samples were
placed in between the electrodes inside the specimen chamber. The chamber was evacuated
using a rotary vacuum pump to about 10 −2 torr. Impedance analyzer was used for ac
measurement. The calculation was performed using the observed values of conductance (Gp) and
capacitance (Cp) at different frequencies and temperatures. The photograph of AC electrical
measurement set-up is shown in Fig. 4.7.
94
Fig. 4.7: AC electrical measurement set-up.
Working formula
For conductivity
d
σ ac = ( )G p
A
Where, Gp → AC conductance
d → Thickness
A → Area of the effective electrode on both sides of sample.
For dielectric constant
Cpd
ε′ =
Aε o
Where, Cp → Capacitance
ε o → Permittivity of free space
For dielectric loss tangent
Gp Gp
tan δ = =
ωC p 2πfC p
Where, f → Linear frequency.
95
4.6 Methods for Measuring Thermal Properties
4.6.1 Procedure of thermal analysis
The thermal stability of original material, the compositions and thermal stability of intermediate
compounds and the composition of the residue can be obtained from an examination of the
weight change vs temperature curve of a substance. The technique of thermogravimetric analysis
is concerned with an analysis of the sample weight change curve. Technique involves change in
weight of a system under examination as the temperature is increased at a predetermined
preferably at a linear rate. Although manual recording methods have been employed, but by the
use of an automatic recording thermbalance, a curve of weight changes of the sample vs sample
temperature can be obtained directly.
Thermal analysis includes a group technique where some physical property of the sample is
monitored under controlled conditions with variation of temperature at a programmed rate. When
the mass change is monitored the results, which indicated chemical reactions are called TG.
When heat absorption monitored, the result indicates crystallization, phase change etc. as well as
reactions. This is called DTA. Together, they are power methods of analysis.
Principle of TG measurement
The TG/DTA module uses a horizontal differential system balance mechanism. Sample weight
changes are measured as described below:
Sample balance beam and reference balance beam are independently supported by driving
coil/pivot. When a weight change occurs at the beam end, the movement is conveyed to the
opposite end of the beam via the driving coil/pivot, when the optical position sensors detect
changes in the position of a slit. The signal from the optical position sensor is sent to the sample
side; the current to the driving coil on the reference side is detected and converted into weight
signal.
Principle of DTA measurement

The thermocouple (platinum-platinum rhodium) for DTA measurement is incorporated in the
end of each of the balance beam ceramic tubes, and the temperature difference between the
holder on the sample side and holder on the reference side is detected. The signal is amplified
and become the temperature signal used to measure the thermal change of the sample.
96
4.6.2 Thermal analysis of banana fibers and composites
The TG/DTA/DTG scans of polyester resin (PR)-sheet , fibers and composites were taken in
nitrogen atmosphere (at a flow rate of 200 ml/min) using a TG/DTA 6300 system controlled by
an EXSTAR 6000 controller (Seiko Instruments Inc., Japan) with mass of samples 10±1 mg.
This was a computer controlled thermal analyzer. The TG/DTA module had a horizontal system
balance mechanism. Alumina was used as reference material and furnace temperature was
programmed by software controlled converter. These analyses were run at heating rate of 20
o
C/min within temperature range 20 – 600 oC. Different thermal parameters such as maximum
degradation temperature, onset temperature of major degradation, phase transition temperature
and mass loss at various temperature stages were obtained by analyzing the recorded profile with
the software. The photograph of thermal analyzer (TG/DTA 6300) is shown in Fig. 4.8.
Fig. 4.8: TG/DTA 6300.
4.7 Methods for Measuring Structural Properties
4.7.1 Fourier transform infrared spectroscopy
The Fourier Transform Infrared (FTIR) spectra of composites were recorded at room temperature
by using a double beam IR spectrophotometer (Shimadzu, FTIR-8900 spectrophotometer, Japan)
in the wave-number range of 500 – 4000 cm-1. The FTIR spectrum of the banana fiber-polyester
resin composites were obtained by putting sample in a potassium bromide (KBr) measuring cell.
97
The FTIR spectra of the composites were recorded in transmittance (%) mode. The photograph
of double beam FTIR spectrophotometer is shown in Fig. 4.9.
Fig. 4.9: Double beam FTIR spectrophotometer.
98
References
[1] Symington M.C., Banks W. M., West O. D., and Pethrick R. A., “ Tensile Testing of
Cellulose Based Natural Fibers for Structural Composite Applications”, J. Compos. Mater.,
43, 1083–1108, 2009.
[2] ASTM Designation: C134–76, Standard Test Method for size, dimensional measurements,
and bulk density refractory brick and insulating fabric.
[3] ASTM (Reapproved 1988) Designation; D 570–81; Standard Test Method for Water
Absorption of Plastic.
[4] ASTM Designation: D 3039/D 3039–00, Standard Test Method for Tensile Properties of
Polymer Matrix Composite Materials.
[5] ASTM Designation: D 790–00, Standard Test Method for Flexural Properties of
Unreinforced and Reinforced Plastics and Electrical Insulating Materials.
99
Chapter 5 Results and Discussion
RESULTS AND DISCUSSION

5.1 Physical Properties of Composite
The properties of natural fiber largely depend on the chemical composition of the fiber and the
properties of composites made from natural fibers are strongly influenced by the fiber properties.
The average chemical compositions of banana fibers are shown below [1]:
Table 5.1: Average chemical compositions of banana fibers.

Constituents Amounts (percentage dry basis)
α-Cellulose 65.112
Hemicellulose 17.325
Legnin 8.018
Pectin and related product 2.124
Ash, Wax 2.502
Others 4.919
Cellulose is the main structural unit in natural fiber whereas lignin and hemicellulose are
cementing materials, which are interlinked in fiber. In the present work, the fibers were treated
with NaOH to increase the wettability. Banana fibers are used as reinforcement in polyester resin
and the effect of fiber volume fraction in the composite is studied.
5.1.1 Bulk density calculation
The bulk density of the composites was determined according to ASTM C134–137 [2] by
measuring the weight and dimensions of the respective samples. Prior to measuring density, the
samples were conditioned at 80 oC for 24 h placing them into incubator. Average densities were
obtained using results from three specimens of each batch.
Figure 5.1(a) shows the effect of fiber addition on density of untreated banana fiber-polyester
resin composites. The density of the composites decreases with the increase of fiber content. This
can be attributed to the fact that the fiber density is lower than the resin. Similar effect was found
100

on the study of banana fiber reinforced vinyl ester resin composites by R. Ghosh et al. [3]. The
density of polyester resin is 1.195 g/cc whereas it is 1.15 g/cc found in literature. It reveals that
the density of fabricated product is slightly higher than that of actual density. It happens due to
the presence of voids in fabricated product.
(a) (b)
Fig. 5.1: Effect of fiber addition on density for the samples of (a) untreated banana fiber-
polyester resin composites and (b) 5% NaOH treated (for different hours) banana fiber-polyester
resin composites.
The bulk density of treated samples is higher than that of untreated sample. Fig. 5.1(b) shows the
effect of treated fiber content on the density of composites. It reveals that the density increases
with the increase of fiber content up to 10% after which it decreases. It also reveals the density is
higher for higher treatment time. In the present study, the density of the treated sample (for five
hours) of 10% fiber content exhibits maximum which is 1.215 g/cc. This can be due to the fact
that the fiber looses hemicellulose, lignin and other soluble matters (usually of low molecular
weights, i.e. pectin, wax, etc.) from the outer surfaces and becomes packed on treatment with
alkali [4].
101

5.1.2 Water absorption/Water intake
(a) (b)
Fig. 5.2: Effect of soaking time on water absorption of different % of fiber content of (a)
untreated banana fiber-polyester resin composites and (b) 5% NaOH treated (for five hours)
banana fiber-polyester resin composites.
Figure 5.2(a) represents the water absorption (%) of untreated banana fiber-polyester resin
composites at soaking time of 1, 2, 3, 6, 12, 24, 48, and 72 h of 5%, 10%, and 20% fiber content.
It reveals that the water absorption depends on amount of fiber loading and soaking time. The
initial water absorption is higher, but as it time elapsed it decreases and comes to a saturation
point. The rate of water absorption increases rapidly with soaking time up to 12 h and then
reaches a maximum or saturation point and after that it remains more or less constant. It can be
seen that the percentage of water absorption increases also with the increase of fiber content, as it
is diffusion phenomenon. Water absorption is higher with addition of fiber content. Water
absorption is responsible only for fiber and higher the fiber addition, higher rate will be the water
intake.
The same trend of water absorption effect is observed on treatment with NaOH of banana fiber
composites as seen in Fig. 5.2(b). But the water absorption rate is slightly decreased for all % of
fiber content comparing with untreated sample. This can be due to the fact that the fiber losses
hemicellulose, lignin and other alkali soluble matters (pectin, wax, etc.) from the outer surfaces
and become packed on treatment with alkali [4].
102

Fig. 5.3: Effect of soaking time on water absorption of untreated and treated (for different hours)
banana fiber-polyester resin composites of 5% of fiber content.
Figure 5.3 shows that the rate of water absorption decreases with the increase of NaOH treatment
time. This can be attributed to possible decrease in cellulose content. α-cellulose tends to
dissolve in a solution of NaOH of concentration above 17.5% [5], the content of hydrophilic
constituents of fibers will decrease with increase in concentration of alkali, resulting in decrease
in moisture absorption of fibers.
103

5.2 Mechanical Properties of Composite
The mechanical properties of the composites such as tensile strength, Young’s modulus, tensile
energy, % of elongation, flexural strength, flexural modulus have been measured and the results
are presented below.
a. Stress-strain (tensile) curve of untreated banana fiber-polyester resin composites for 5%

of fiber content.
b. Stress-strain (flexural) curve of untreated banana fiber-polyester resin composites for 5%

of fiber content.
Fig. 5.4: Stress-strain curves (before toe correction) of composites as obtained from QMat
professional software.
104

Typical stress-strain plots for the composites are shown in Fig. 5.4. These plots show linear
deformation behavior with the stress. Here stress (force) increases with the increase of strain
(elongation). It reaches to a maximum and after that the stress falls down. The Young’s modulus
of the composites was calculated from the slop of the curve.
(a) (b)
Fig. 5.5: Effect of fiber addition on tensile strength of (a) untreated banana fiber-polyester resin
composites and (b) 5% NaOH treated (for different hours) banana fiber-polyester resin
composite.
Figure 5.5(a) shows the variation of tensile strength with the increase in weight percentage of
banana fiber. The tensile strength decreases during the initial stages of fiber loading. This shows
that the load is not properly transmitted to the fibers. The sole purpose of reinforcement is not
properly served at lower fiber content. But the fiber percentage increases from 5% the tensile
strength increases. This should be because of the increased bonding between the fiber and the
matrix. The load sharing is easily transmitted to the fibers. Similar results were found by R.
Ghosh et al. [3] in banana fiber/vinyl ester resin composites. The tensile strength of the banana
fiber is 500 MPa [6]; compared to fabricate polyester resin is 43.66 MPa, which is less than that
of literature value 63 MPa [7]. So it is expected that an increase in the fiber content would
considerably increase the tensile strength of the composite.
105

Figure 5.5(b) shows the effect of fiber addition on tensile strength of 5% NaOH treated banana
fiber-polyester resin composite for 1, 2, and 5 h. It shows that the strength of the composites
decreases at initial stage (only for lower treated sample) and then increases with the increase of
fiber content. At the initial stage (5%) the interfacial bonding between the fiber and matrix is
poor. It can be attributed that the critical volume below which the strength is decreased. After
addition of 10% the fibers are finely distributed and the interfacial bonding between the fiber and
matrix is good. The tensile properties of the composites are summarized in Table 2. It shows that
the tensile strength of the composites also increases with the increase of NaOH treatment time.
This suggests that due to treatment of fibers with alkali (5% NaOH solution), the interfacial
strength might have slightly increased and aided mechanical interlocking between the fiber and
matrix by roughening up the fiber surface [8], though not sufficient to transfer the load at the
fiber-matrix interface. The increase in tensile strength can be attributed to an increase in the
cellulose crystallinity as a result of alkali treatment. The increase in the crystallinity index
percentage of alkali treated fibers occurs because of the removal of cementing materials (i.e.,
lignin, pectin and hemicellulose), which leads to better packing of the cellulose chain [9].
Fig. 5.6: Effect of fiber addition on Young’s modulus of untreated and NaOH treated (for
different hour) banana fiber-polyester resin composites.
The Effect of fiber addition on Young’s modulus of untreated and NaOH treated (for different
hour) banana fiber-polyester resin composites is shown in Fig. 5.6. This shows that the Young’s
modulus of composites increases with the increase of fiber addition. The Young’s modulus of
106

untreated fiber composites is 2.167 GPa. Young’s modulus is a measure of stiffness of a

material. Thus the stiffness of banana fiber composites increases with the increase of fiber
addition continuously within the limit of the present study. It is apparent that the % of elongation
decreases with increasing fiber content as shown in Table 5.2. The presence of fiber restricts the
slip resulting in lesser ductility. This figure also represents that the Young’s modulus of treated
banana fiber composites is higher than that of untreated fiber composites and modulus increases
with increasing NaOH treatment time. The strength of the composites depends on the dimension,
distribution and orientation of its filler along with interfacial bond strength between filler and
matrix [10–11]. With no change in interfacial strength and keeping other conditions unchanged,
a composite with long fillers aligned in the parallel direction is potentially stronger than itself
when its fillers are short and randomly oriented. So, in the present case, the tensile strength and
modulus increased due to increase in content of load carrying filament aligned in the same
direction.
Table 5.2: Effect of fiber treatment with 5% NaOH solution (for different hours) on tensile
properties of composites.
Sample NaOH treated Tensile Young’s Elongation at Tensile
hour – Fiber strength modulus max force energy (J/m2)
content (wt. %) (MPa) (GPa) (%)
PR - 43.66 2.046 - 0.4576
UBF-PR 0h–5 35.94 2.167 3.775 0.3983
TBF-PR 1h–5 38.73 2.257 3.101 0.3533
TBF-PR 2h–5 39.02 2.393 3.050 0.2503
TBF-PR 5h–5 44.45 2.435 3.258 0.3656
UBF-PR 0 h – 10 44.58 2.388 3.450 0.3983
TBF-PR 1 h – 10 44.84 2.393 3.180 0.3342
TBF-PR 2 h – 10 45.05 2.488 2.550 0.2243
TBF-PR 5 h – 10 51.05 2.556 3.325 0.3256
UBF-PR 0 h – 20 64.08 3.475 3.401 0.4750
TBF-PR 1 h – 20 52.43 3.208 2.802 0.3485
TBF-PR 2 h – 20 53.56 3.267 3.675 0.2334
TBF-PR 5 h – 20 56.32 3.656 4.050 0.3656
107

Fig. 5.7: Effect of fiber addition on tensile energy of untreated and treated (for different hour)
banana fiber-polyester resin composites.
Figure 5.7 shows the effect of fiber addition on tensile energy of untreated and treated (for
different hour) banana fiber-polyester resin composites. The figure shows that 0% fiber loading
sample is higher energy. The tensile energy or fracture energy of a material is a quantitative
measure of the fracture toughness of it. The tensile energy gradually decreases with the increase
of fiber addition up to 10% and then increases or constant. This happen due to the fact that, with
fiber addition composite specimens show more brittle behavior and thus come to the peak load
quickly, which ultimately causes less area under the load displacement curve. Figure shows that
the tensile energy of treated sample is lower than that of untreated fiber composites and energy is
improved with treatment time of NaOH.
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Fig. 5.8: Effect of fiber addition on flexural strength of untreated and treated (for different hour)
banana fiber- polyester resin composites.
Figure 5.8 shows the effect of fiber addition on flexural strength of untreated and treated (for
different hour) banana fiber composites. It reveals that the flexural strength decreases with the
increase of fiber addition up to certain percentage (up to 10%), afterwards this strength increases
with composition for untreated fiber composites. The interfacial bonding is poor due to presence
of lignin, fatty and waxy materials. So, the fibers do not share the load with matrix. That is why
the flexural strength of untreated banana fiber composite decreases. In further addition of fiber
(20%), both the fiber and matrix bear the load and make resistance to slip as in the case of age
hardening of metals [11]. In this range the fibers are finely distributed and the interfacial bonding
between the fiber and matrix is high.
In comparison of treated banana fiber composites with 5% NaOH, the flexural strength is always
higher than that of untreated composites. Flexural strength increases with the increase of fiber
treatment time. But the same trend of untreated samples that of flexural strength decreases with
the increase of fiber addition up to 10% is observed for lower treated samples. For 0% fiber the
polymer strength is obtained 66.55 MPa. It increases with the increase of fiber addition of higher
treated samples. For the higher treated (five hours) samples the flexural strength of 20% fiber
content is found 73.5 MPa.
109

Fig. 5.9: Effect of fiber addition on flexural modulus of untreated and treated (for different hour)
banana fiber- polyester resin composites.
Table 5.3: Effect of fiber treatment with 5% NaOH solution (for different hour) on the flexural
properties of composites.
Sample NaOH treated Flexural strength Flexural modulus Flexural
hour – Fiber (MPa) (GPa) to Fmax
content (wt. %) (%)
PR - 66.55 - 2.869
UBF-PR 0h–5 55.50 3.154 2.936
TBF-PR 1h–5 58.52 3.315 3.414
TBF-PR 2h–5 58.94 3.404 3.389
TBF-PR 5h–5 71.50 3.550 2.015
UBF-PR 0 h – 10 54.60 2.994 2.354
TBF-PR 1 h – 10 57.75 3.439 3.810
TBF-PR 2 h – 10 57.95 3.653 3.410
TBF-PR 5 h – 10 71.80 3.728 2.765
UBF-PR 0 h – 20 58.80 2.615 2.940
TBF-PR 1 h – 20 59.80 3.619 2.850
TBF-PR 2 h – 20 60.74 3.790 2.931
TBF-PR 5 h – 20 73.50 4.005 2.168
110

Figure 5.9 shows the effect of fiber addition on flexural modulus of untreated and treated (for
different hours) banana fiber- polyester resin composites. The flexural modulus decreases with
the increase of fiber addition of untreated sample and this modulus increases with the increase of
fiber addition of treated samples. On the other hand, it is observed from the Table 3 that the
flexural strain to Fmax (i.e., flexural strain up to the maximum bending force) decreased with the
increase in fiber loading. These imply that the composites became stiff and brittle on introducing
the fiber, and the degrees of stiffness and brittleness increased within the fiber content. The
results of flexural properties are similar to those of tensile properties. The flexural strength and
modulus improves with the increase of NaOH treatment time as seen in Table 5.3.
5.3 Electrical Measurements
The information of the conduction mechanism and relaxation process of banana fiber-polyester
resin composites can be obtained from the AC conductivity and dielectric relaxation process. The
measured values of the conductance and capacitance as a function of frequency (100 Hz – 2
MHz) at temperatures of 300, 323, 348 and 373 K were used to calculate the AC conductivity,
dielectric constant and dielectric loss tangent of the samples of untreated and treated banana
fiber-polyester resin composites with 5%, 10%, and 20% fiber content. The fibers were treated
with 5% NaOH solution for 1, 2 and 5 h.
5.3.1 Variation of AC conductivity with frequency
Figure 5.10(a) – (b) show the AC conductivity (σac) as a function of frequency curves taken at
temperature range (300 – 373 K) of untreated banana fiber-polyester resin composites. It is
observed that AC conductivity increases with the increase of frequency at all temperatures. At
low frequency conductivity increases steadily up to 105 Hz whereas at high frequency (>105 Hz)
it increases faster. The increase in frequency enhances the hopping frequency of charge carriers
resulting in an increase in the conduction process thereby increasing the AC conductivity. The
maximum conductivity occurred when the frequency of the hopping charges is equal to the
111

applied AC electric field. There is no significant change of conductivity between air and vacuum
atmosphere.
(a) (b)
Fig. 5.10: AC conductivity as a function of frequency curves of untreated banana fiber-polyester
resin composites of 5% fiber content taken at (a) 300 K in air and vacuum atmosphere and (b)
300, 323, 348 and 373 K in vacuum atmosphere.
(c) (d)
Fig. 5.10: AC conductivity as a function of frequency curves taken at different temperature of
banana fiber-polyester composites of 10% fiber content treated with NaOH for (c) two hours and
(d) five hours.
Figure 5.10(c) – (h) AC conductivity as a function of frequency curves of treated banana fiber-
polyester resin composites for 1, 2 and 5 h of different percentage of fiber content taken at
temperature range (300 – 373 K). It is observed that AC conductivity increases with the increase
112

of frequency at all temperatures. But AC conductivity decreases with the increase of NaOH
treatment time as shown in Fig. 5.10(e) – (f). AC conductivity decreases also with increasing the
percentage of fiber content as in Fig. 5.10(g) – (h). AC conductivity improves with increasing
the temperature as seen in Fig. 5.10(c) – (d). With increasing the frequency and temperature the
AC conductivity of the materials increases due to the oscillation of the dipolar molecules in out
of phase with the applied field and random movement of the dipolar molecules [12].
(e) (f)
Fig. 5.10: AC conductivity as a function of frequency curves of treated banana fiber-polyester
composites with NaOH for different hours of 5% fiber content taken at (e) 300 K and (f) 373 K.
(g) (h)
Fig. 5.10: AC conductivity as a function of frequency curves of treated banana fiber-polyester
composites with NaOH for five hours of 5%, 10% and 20% fiber content taken at (g) 300 K and
(h) 373 K.
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Table 5.4: Values of n in σac(ω) = Aωn of untreated and treated banana fiber composites.
Composites NaOH treated Temperature Value of ‘n’ in Value of ‘n’ in
(%) time (h) T (K) 103 to 104 (Hz) 105 to 106 (Hz)
UBF-PR(5) 0 300 0.55 1.23
373 0.54 1.18
TBF-PR(5) 1 300 0.57 1.27
373 0.55 1.13
TBF-PR(5) 2 300 0.64 1.41
373 0.60 1.21
TBF-PR(5) 5 300 0.58 1.29
373 0.56 1.12
UBF-PR(10) 0 300 0.60 1.40
373 0.58 1.19
TBF-PR(10) 1 300 0.55 1.16
373 0.53 1.09
TBF-PR(10) 2 300 0.65 1.50
373 0.59 1.23
TBF-PR(10) 5 300 0.64 1.40
373 0.58 1.23
UBF-PR(20) 0 300 0.62 1.34
373 0.57 1.18
TBF-PR(20) 1 300 0.61 1.34
373 0.56 1.14
TBF-PR(20) 2 300 0.65 1.44
373 0.56 1.23
TBF-PR(20) 5 300 0.61 1.33
373 0.58 1.17
It is clear that the variation in the logarithmic AC conductivity is almost linear with the variation
in logarithmic frequency and that σac(ω) increases with increasing frequency. The observed
frequency dependence of σac reveals that the mechanism responsible for AC conduction could be
due to hopping. The values of the exponent ‘n’ in σac(ω) = Aωn for various frequency region at
114

different temperature as recorded in Table 5.4 is also supported this view. The values of ‘n’ are
found to be 0.53 – 0.65 in the low frequency (1 – 10 kHz) and 1.09 – 1.50 above 10 kHz. The
value of index ‘n’ is high enough that is required for Debye type relaxation process. The
observed frequency dependence of AC conductivity indicates that the mechanism of carrier
conduction in banana fiber-polyester resin composites at low temperatures and at low
frequencies is due to hopping of carriers between the localized states and movement of the
thermally excited carriers from the energy levels within the band gap in the high temperature
region.
5.3.2 Variation of AC conductivity with temperature
(a) (b)
Fig. 5.11: AC conductivity as a function of temperature curves taken at different frequency of
banana fiber-polyester composites of 5% fiber content treated with NaOH for (a) one hour and
(b) five hours.
The AC conductivity data are plotted against the inverse of absolute temperature in Fig. 5.11(a) –
(b) for different fixed frequencies. It is seen that the AC conductivity is very weakly dependent
on temperature. This suggests a very small value of activation energy of the conduction carriers.
At high frequency region, the variation of conductivity with temperature is small. Thus it
becomes apparent that the conductivity is more temperature dependent at low frequencies
compared to high frequencies. The activation energies for all composites are given in Table 5.5.
115

This low value of activation energies implies that the conduction mechanism may be hopping of
the charge carriers in these materials.
Table 5.5: Activation energies of untreated and treated banana fiber composites.
Composites NaOH treated hour – Frequency Activation
Fiber content (wt. %) (Hz) energy ( eV)
UBF-PR 0h–5 500 0.020
10000 0.017
TBF-PR 1h–5 500 0.098
10000 0.083
TBF-PR 2h–5 500 0.139
10000 0.108
TBF-PR 5h–5 500 0.121
10000 0.108
UBF-PR 0 h – 10 500 0.144
10000 0.102
TBF-PR 1 h – 10 500 0.064
10000 0.045
TBF-PR 2 h – 10 500 0.103
10000 0.074
TBF-PR 5 h – 10 500 0.112
10000 0.085
UBF-PR 0 h – 20 500 0.091
10000 0.090
TBF-PR 1 h – 20 500 0.016
10000 0.015
TBF-PR 2 h – 20 500 0.091
10000 0.058
TBF-PR 5 h – 20 500 0.137
10000 0.105
116

5.3.3 Variation of dielectric constant with frequency
(a) (b)
Fig. 5.12: Dielectric constant as a function of frequency curves of untreated banana fiber-
polyester resin composites of 5% fiber content taken at (a) 300 K in air and vacuum atmosphere
and (b) 300, 323, 348 and 373 K in vacuum atmosphere.
Frequency has an important influence on dielectric properties. Fig. 5.12(a) – (b) show the
variation of dielectric constant with frequency from (100 Hz – 2 MHz) at the temperature range
(300 – 373 K) of untreated banana fiber-polyester resin composites. It is seen that the dielectric
constant decreases with increasing frequency and this constant improves with increasing
temperature. All specimens exhibit a normal dielectric behavior of materials, which may be due
to the interfacial polarization [12]. Dielectric constant depends on atmosphere as shown in Fig.
5.12(a). At low frequency the value of dielectric constant is much high of vacuum atmosphere
compare to air atmosphere and at high frequency these value are incorporated. Dielectric
constant decreases sharply at low frequency (100 – 900 Hz) region and smoothly decreases at
high frequency region. For interfacial polarization dielectric constant is high at low frequency
compare to high frequency.
117

(c) (d)
Fig. 5.12: Dielectric constant as a function of frequency curves taken at different temperatures of
treated banana fiber-polyester composites with NaOH for five hours of (c) 10% fiber content and
(d) 20% fiber content.
The variation of dielectric constant with frequency at temperature range (300 – 373 K) of treated
banana fiber composites for different hours is shown in Fig. 5.12(c) – (h). It is observed
dielectric constant decreases with increasing frequency and this constant improves with
increasing temperature as shown in Fig. 5.12 (c) – (d). At low frequency the value of dielectric
constant is much high as compare to high frequency. For interfacial polarization dielectric
constant is high at low frequency compare to high frequency. It is seen also that the value of
dielectric constant is high for this materials. It can be happen because of the oxygen vacancy or
interfaces between the banana fiber and matrix. Dielectric constant also decreases with
increasing NaOH treatment time as in Fig. 5.12 (g) – (h). But at lower treatment time (for one
hour) this constant increases. Dielectric contant of treated fiber composites is much lower than
that of untreated fiber composites. This constant decreases with increasing the percentage of
fiber content as shown in Fig. 5.12 (g) – (h). It may happen because of the oxygen vacancy,
hydroxyl ion motion or interfaces between the fiber and matrix [13]. For ionic effect dielectric
constant is high at low frequency compare to high frequency.
118

(e) (f)
Fig. 5.12: Dielectric constant as a function frequency curves of treated banana fiber-polyester
composites with NaOH for different hours of 5% fiber content taken at (e) 300 K and (f) 373 K.
(g) (h)
Fig. 5.12: Dielectric constant as a function frequency curves of treated banana fiber-polyester
composites with NaOH for five hours of 5%, 10% and 20% fiber content taken at (g) 300 K and
(h) 373 K.
All the samples have high value of dielectric constant at low frequencies. The maximum value of
dielectric constant is observed at room temperature for 100 Hz. The high value at lower
frequency region is due to the interfacial polarization for the homogeneous double layer
dielectric structure, which is in agreement with Koop’s phenomenological theory [12]. At low
frequency the dipoles line up in the field, reverse direction when the field is reversed, and so
contribute to a high dielectric constant. Owing to their inertia, and to retain their original
119

configuration, the dipoles take a certain time to reverse direction: this is characterized by their
relaxation time. Decreasing nature of the dielectric constant value with increasing frequency is
due to the dielectric relaxation which is the cause of anomalous dispersion. At higher frequencies
the orientation of polar molecules along the direction of the applied electric field is disturbed.
When the frequency becomes so high, that the reversal of field takes place at intervals
comparable to the relaxation time, then the dipoles would cease to follow the change of field
completely and the dielectric constant would decrease. At higher frequencies it reaches to a
minimum value because polarizability is determined by the localized electronic states. In this
case, the rotation of the dipole is varied with alternating electric field and the distance of the
dipole between the charges is changed under the influence of an applied field.
5.3.4 Variation of dielectric loss tangent with frequency
(a) (b)
Fig. 5.13: Dielectric loss tangent as a function of frequency curves of untreated banana fiber-
polyester resin composites of (a) 5% fiber content taken at 300 K with air and vacuum
atmosphere and (b) 10% fiber content taken at 300, 323, 348 and 373 K with vacuum
atmosphere.
The plots of dielectric loss tangent (tanδ) as a function of frequency taken at temperature range
(300 – 373 K) of untreated banana fiber-polyester resin composites are shown in Fig. 5.13(a) –
(b). There is a big dip in the loss tangent behavior. The dip is found to maximum at around 100
120

kHz. The loss tangent gradually decreases with increasing frequency up to 100 kHz and after that
it increases sharply with increasing frequency. The value of loss tangent is higher at high
frequency compare to low frequency. The loss tangent value increases with increasing
temperature.
(c) (d)
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of banana fiber-polyester
composites taken at different temperature treated with NaOH for (c) one hour of 5% fiber
content and (d) five hour of 10% fiber content.
(e) (f)
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of treated banana fiber-
polyester composites with NaOH for different hours of 5% fiber content taken at (e) 300 K and
(f) 373 K.
121

(g) (h)
Fig. 5.13: Dielectric loss tangent as a function frequency of curves of treated banana fiber-
polyester composites with NaOH for five hours of 5%, 10% and 20% fiber content taken at (g)
300 K and (h) 373 K.
Figure 5.13(c) – (h) show that the plots of dielectric loss tangent as a function of frequency of
treated (for different hour) banana fiber-polyester resin composites at temperature range (300–
373 K). Dip behavior is observed in all samples. The values of loss tangent decreases slightly
with increasing the treatment time as shown in Fig. 5.13(c) – (d). But this values gradually
increases with increasing temperature as in Fig. 5.13(e) – (f). There may be some relaxation
peaks in the low frequency region at 100 Hz or below and then it decreases with a broad
minimum at 100 kHz and then again increases. The loss tangent decreases with increasing
percentage of fiber content as seen in Fig. 5.13(g) – (h). These are the indication of loss of
energy due to the interfacial relaxation.
5.4 Thermal Analysis
Thermogravimetry (TG), Differential thermogravimetry (DTG) and Differential thermal analysis

(DTA) were performed using a TG/DTA 6300 system controlled by an EXSTAR 6000 controller
(Seicko Instrument Inc., Japan) with mass of samples 10±1 mg. These analyses were run under a
stream of nitrogen (200 mL/min.) at heating rate of 20 oC/min within temperature range 20 – 600
o
C. The thermal properties of the polyester resin (PR)-sheet, fiber and composites were carried
122

out of different spectra like TG (upper line), DTA (middle line) and DTG (lower line) from
thermal graph. Thermal analysis describes on a macroscopic scale the removal of all water
molecules present in the structure. Therefore, the weight loss could be attributed to dehydration
of water molecules absorbed around exchangeable cataions, absorbed to internal and external
surfaces, or condensed in pore space.
5.4.1 Thermal analysis of polyester resin sheet
2.000 25.00
100.0
358.5Cel
92.3 %
20.00 387.7 Cel

48.7%
50.0
1.500 86.9 %
3 9 3 .8 C e l
3 9 .8 %
15.00
417.0Cel 0.0
5.4%
DTG mg/min
DTA uV
TG %
1.000
10.00
3 9 5 .3 C e l -50.0
9 .1 1 u V
5.00 3 9 4 .3 C e l
0.500 0 .4 6 2 m g / m in
-100.0
0.00
0.000
216 .0C el
0.0 30m g /m in -150.0
-5.00
50.0 100.0 150.0 200.0 250.0 300.0 350.0 400.0 450.0 500.0 550.0
T e m p Ce l
Fig. 5.14: TG/DTA/DTG curves of polyester resin sheet.
Observations
TG curve: Onset temperature of major degradation (ID) is at 358.5 oC.
Decomposition of polyester resin ranges from 185oC to 450.5 oC corresponding to
the extrapolated masses of 92.3% and 5.4% respectively.
50% degradation (MD) temperature is at 387.7 oC.
Maximum slop of degradation line is at 393.8 oC. Total degradation loss is 86.9%.
Final residual mass is 5.6%.
123

DTA curve: Endothermic peak is at 395.3 oC.

DTG curve: Maximum degradation rate is at 394.3 oC.
In Fig. 5.14 TG curves exhibits the weight loss of polyester resin sheet. Polyester resin
undergoes two separate degradation steps under heating and is stable at low temperature (0 – 175
o
C). The initial weight loss is found to start at 185 oC and the termogravimetric percentage (TG
%) slowly drops to 50% at 387.7 oC and 5.4% at 417 oC. However, it is a common practice to
consider the degradation temperature at 50% weight loss of the sample as an indicator for the
structural destabilization. DTG means the differential of TG, the apparent changes observed
DTG are complementary to TG obviously, and DTG is the maximum when the slope of the fall
is the maximum. The maximum slope temperature (393.8 oC) on TG curve, the endothermic
peak temperature (395.3 oC) on DTA curve and the maximum degradation rate temperature
(394.3 oC) on DTG curve are closely related to the degradation of polyester resin. The major
mass loss is due to thermal decomposition of polyester resin, mainly into lighter hydrocarbons
(e.g. CH4) and H2.
5.4.2 Thermal analysis of untreated banana fiber
It is a common fact that the major components of lignocellulosic fibers are hemicellulose,
cellulose, and lignin. According to Yang et al. [14], the main thermal decomposition of
lignocellulosic materials generally occurs over the temperature range of 200 – 400 oC.
Hemicelluloses, being the light fraction component decompose at the low temperature region
between 220 and 315 oC. Cellulose is the last component to decompose at the high temperature
range of 315 – 400 oC. Among the three components, lignin was the most difficult component to
decompose. The degradation of lignin was represented by the high temperature tails.
In Fig. 5.15, the mass loss observed in the first temperature range (up to 150 oC) is mainly due to
dehydration of fibers, i.e., moisture loss. In this region, the slight steepness (up to 84.2 oC) of TG
curve indicates that the greater portion of dehydration (3.7%) is from the outer layers of fibers.
The remaining mass loss of 4.2% in this region may be due to dehydration of fibers from its
inner layers. A mass loss of lighter matters (wax, fatty matters, etc.) may also present over this
region. Therefore, the first step of major degradation is mainly due to decomposition of lighter
124

materials (hemicellulose) coupled with decomposition of cellulose and the second step, the
steepest portion as indicated by the peak on DTG curve, is mainly due to decomposition of
heavier materials (lignin) coupled with partial decomposition of cellulose and hemicellulose. The
presence of this two step decomposition is also clarified by the first (not clearly visible) and
second peak on DTG and DTA curves. Final residual mass of 18.9% is mainly carbonaceous
char.
2.000 20.00 3.7 % 100.0

84 .2C el 32 1.0C el
96 .6% 90 .4%
1.800 3 7 2 .3 C e l
4 0 .0 %
15.00 35 5.8C el
54 .8%
1.600 71.2% 50.0
1.400
10.00
393 .4C el
19.2 %
1.200
0.0
3 7 1 .1 C e l
DTG mg/min
2 93.7 C el 7 .2 2 u V
DTA uV
6 .70u V
TG %
1.000 5.00
0.800
-50.0
0.00
0.600
3 0 1 .7 C e l 3 7 2 .3 C e l
0 .1 4 4 m g / m in 0 .4 3 3 m g / m in
0.400
-5.00 -100.0
0.200
0.000
-10.00
-150.0
100.0 200.0 300.0 400.0 500.0
T e m p Ce l
Fig. 5.15: TG/DTA/DTG curves of untreated banana fiber.
Observations
TG curve: Mass-loss events are parted into three stages. Major degradation stage spans over
200 oC to 480 oC corresponding to the extrapolated masses of 90.4% and 19.2%
respectively
Onset temperature of major degradation (ID) is at 321 oC.
50% degradation (MD) temperature is at 355.8 oC.
Maximum slop of degradation line is at 372.3 oC. Major degradation loss is
71.2%. Final residual mass is 18.9%.
DTA curve: Endothermic peak is at 371.1 oC.
DTG curve: Maximum degradation rate is at 372.3 oC.
125

5.4.3 Thermal analysis of NaOH treated banana fiber
4.000 30.00
3.7% 100.0
327.4Cel
242.9Cel 92.8%
3.500 109.7Cel 94.9%
80.0
25.00 95.8%
357.2C el 60.0
3.000 54.7%
76.4% 3 7 1 .0 C e l
20.00 3 8 .6 %
40.0
2.500
20.0
15.00 388.9Cel
495.1C el
16.4%
2.000 13.5%
0.0
DTG mg/min
DTA uV
TG %
10.00 -20.0
1.500
3 7 3 .0 C e l
9 .5 2 u V
-40.0
1.000 5.00
3 7 1 .3 C e l -60.0
73.8C el
4.18u V 0 .7 3 9 m g / m in
0.500 -80.0
0.00
-100.0
0.000 67.8C el
0.055m g /m in
-5.00 -120.0
-0.500
-140.0
-10.00
50.0 100.0 150.0 200.0 250.0 300.0 350.0 400.0 450.0 500.0 550.0 600.0
T e m p Ce l
Fig. 5.16: (a) TG/DTA/DTG curves of NaOH treated (for one hour) banana fiber.
4.000 30.00
3.3%
100.0
249.9C el 331.0C el
45.5C el 115.7C el 94.7% 93.3%
3.500 25.00 99.5% 96.3% 80.0
358.3C el
60.9% 3 6 9 .7 C e l
4 8 .9 % 60.0
64.8%
3.000 20.00
40.0
388.2C el
550.7Cel
28.4% 20.0
2.500 24.9%
15.00
0.0
DTG mg/min
DTA uV
TG %
2.000
10.00 -20.0
3 7 5 .9 C e l
8 .9 9 u V -40.0
1.500
5.00
3 6 9 .7 C e l -60.0
79.3C el 1 .2 5 3 m g / m in
3.63uV
1.000 -80.0
0.00
-100.0
0.500
-5.00 -120.0
76.7Cel
0.077m g /m in
-140.0
0.000
-10.00
50.0 100.0 150.0 200.0 250.0 300.0 350.0 400.0 450.0 500.0 550.0 600.0
T e m p Ce l
Fig. 5.16: (b) TG/DTA/DTG curves of NaOH treated (for five hours) banana fiber.
126

The TG, DTA and DTG curves of treated banana fiber with 5% NaOH solution are shown in Fig.
5.16(a) – (b). The data are summarized in Table 5.6 – 5.7. The DTG curve of the treated banana
fibers shows an initial peak between 67.8 and 76.7 oC, which corresponds to a mass loss of
absorbed moisture with 3.7 – 3.3%. The second peak (major peak) at 369.7 – 371.3 oC is
probably attributed to hemicelluloses, cellulose decomposition. The char residue at 600 oC is
13.5 – 24.9%. An increase in the degradation temperature is observed as a results mass loss (%)
decrease. This was due to the removal of more non-cellulosic material; hence, the high degree of
structural order was retained. This revealed a relationship between the structure and the thermal
degradation of cellulose. A greater crystalline structure required a higher degradation
temperature [15]. However, both the non-cellulosic components and the crystalline order of
cellulose played an important role in the thermal degradation of the fibers. Mercerization disrupts
the hydrogen bonding in the network structure, and thus increases the surface roughness. This
treatment removes a certain amount of lignin, wax, and oils from the external surface of the fiber
cell wall, depolymerizes cellulose, and exposes the short length crystallites.
5.4.4 Thermal analysis of untreated banana fiber-polyester resin composites
The TG, DTA and DTG curves of untreated and treated banana fiber-polyester resin composites
are shown in Fig. 5.17 – 5.18. The data are summarized in Table 5.6 – 5.7. It can be considered
that the mass loss event of the composites is divided into three stages. The mass loss at the first
stage (50 – 180 oC) is mainly due to dehydration of composites. In second stage of TG curve
(180 – 450 oC), the mass loss is due to almost complete decomposition of banana fiber and
partial decomposition of PR sheet. The third stage (450 – 600 oC) is due to decomposition of
lignin. The major mass loss depends on the percentage of fiber content. But the onset
temperature of degradation, maximum degradation rate, and endothermic peak is not much
affected with increasing the fiber content. The endothermic peak of treated composites is
observed at higher temperatures (within 394.6 – 399.7 oC) compare to that of PR sheet, fibers
and untreated composites. The maximum slope temperature on TG curve, the endothermic peak
temperature on DTA curve and the maximum degradation rate temperature on DTG curve are
127

4 .0 0 0
1 0 0 .0
0 .9 %1 8 2 .0 C e l
25 .0 0 4 3 .9 C e l 9 8 .7 % 3 4 5 .8 C e l
1 0 0 .0 % 9 4 .5 %
3 .5 0 0 8 0 .0
20 .0 0 6 0 .0
3 8 2 .7 C e l
8 3 .4 % 5 2 .8 %
3 .0 0 0 3 9 3 .2 C e l
4 1 .2 % 4 0 .0
15 .0 0
2 0 .0
2 .5 0 0
4 1 9 .9 C e l 5 4 4 .3 C e l
1 1 .1 % 9 .8 % 0 .0
10 .0 0
DTG mg/min
DTA uV
TG %
2 .0 0 0 -2 0 .0
5.00 3 9 0 .5 C e l -4 0 .0
1 .5 0 0 5 .3 2 u V
3 9 3 .9 C e l -6 0 .0
1 .4 8 4 m g / m in
0.00
-8 0 .0
1 .0 0 0
-1 0 0 .0
-5 .0 0
0 .5 0 0
-1 2 0 .0
-1 0.00
-1 4 0 .0
0 .0 0 0
1 0 0 .0 2 0 0 .0 3 0 0 .0 4 0 0 .0 5 0 0 .0 6 0 0 .0 7 0 0 .0 8 0 0 .0
T e m p Ce l
Fig. 5.17: (a) TG/DTA/DTG curves of untreated banana fiber-polyester resin composites of 5%
fiber content.
5 .0 0 0 30 .0 0
1 0 0 .0
2 0 0 .3 C e l
9 7 .0 % 3 4 4 .3 C e l
4 .5 0 0
8 9 .7 % 8 0 .0
25 .0 0
2 .5 %
3 8 7 .2 C e l
4 .0 0 0 3 8 2 .1 C e l 4 6 .3 % 6 0 .0
5 1 .5 %
7 6 .4 %
20 .0 0
4 0 .0
3 .5 0 0
2 0 .0
15 .0 0 4 1 9 .8 C e l
3 .0 0 0 5 4 8 .1 C e l
1 3 .3 % 1 1 .8 % 0 .0
DTG mg/min
DTA uV
TG %
2 .5 0 0
10 .0 0 -2 0 .0
3 8 9 .2 C e l
6 .1 3 u V
-4 0 .0
2 .0 0 0
5.00
3 9 3 .7 C e l -6 0 .0
9 0 .6 C e l 1 .7 1 0 m g / m in
1 .5 0 0
3 .5 6 u V
-8 0 .0
0.00
1 .0 0 0
-1 0 0 .0
0 .5 0 0 -5 .0 0 -1 2 0 .0
-1 4 0 .0
0 .0 0 0 7 7 .4 C e l
-1 0.00 0 053 / i
5 0 .0 1 0 0 .0 1 5 0 .0 2 0 0 .0 2 5 0 .0 3 0 0 .0 3 5 0 .0 4 0 0 .0 4 5 0 .0 5 0 0 .0 5 5 0 .0 6 0 0 .0
T e m p Ce l
Fig. 5.17: (b) TG/DTA/DTG curves of untreated banana fiber-polyester resin composites of 20%
fiber content.
128

5.3.5 Thermal analysis of NaOH treated banana fiber-polyester resin composites
6 .0 0 0 3 0 .0 0
1 0 0 .0
3 0 .1 C e l
5 .5 0 0 9 9 .9 % 2 5 0 .4 C e l
2 0 0 .3 C3e.1
l % 9 4 .0 % 3 5 1 .2 C e l
2 5 .0 0 9 6 .8 % 8 7 .1 %
5 .0 0 0
3 9 3 .7 C e l
4 1 .0 %
6 9 .2 % 3 8 2 .3 C e l 5 0 .0
4 .5 0 0 2 0 .0 0 5 2 .6 %
4 .0 0 0
1 5 .0 0 4 1 4 .8 C e l 5 5 0 .8 C e l
1 8 .0 % 1 6 .8 %
3 .5 0 0
0 .0
DTG mg/min
DTA uV
TG %
3 .0 0 0
1 0 .0 0
2 .5 0 0
3 9 4 .6 C e l
7 .4 1 u V -5 0 .0
5 .0 0
2 .0 0 0 1 0 1 .6 C e l
4 .5 4 u V
3 9 4 .1 C e l
1 .5 0 0 1 .4 6 0 m g / m in
0 .0 0
1 .0 0 0 -1 0 0 .0
-5 .0 0 3 5 1 .4 C e l
0 .5 0 0 0 .7 1 1 m g /m in
0 .0 0 0
-1 0 .0 0 -1 5 0 .0
5 0 .0 1 0 0 .0 1 5 0 .0 2 0 0 .0 2 5 0 .0 3 0 0 .0 3 5 0 .0 4 0 0 .0 4 5 0 .0 5 0 0 .0 5 5 0 .0
T e m p Ce l
Fig. 5.18: (a) TG/DTA/DTG curves of NaOH treated (for one hour) banana fiber-polyester resin
1 0 .0 0 3 0 .0 0
1 0 0 .0
21 .4
9 9%.2 C e l
1 9 8 .6 C e l 9 7 .4 % 3 5 4 .2 C e l
9 .0 0 9 7 .5 % 9 1 .7 %
2 5 .0 0
3 9 9 .8 C e l
3 8 .7 %
8 .0 0 3 8 8 .1 C e l
7 9 .5 % 5 1 .9 % 5 0 .0
2 0 .0 0
7 .0 0
1 5 .0 0
6 .0 0 4 2 2 .5 C e l 5 4 9 .9 C e l
1 2 .2 % 1 1 .4 % 0 .0
DTG mg/min
DTA uV
TG %
5 .0 0 1 0 .0 0
4 .0 0
5 .0 0 -5 0 .0
3 .0 0 9 6 .4 C e l
2 .8 5 u V 3 9 5 .2 C e l
3 .3 1 u V
4 0 0 .2 C e l
0 .0 0 2 .4 7 m g / m in
2 .0 0
-1 0 0 .0
-5 .0 0
1 .0 0
1 0 5 .3 C e l
0 .0 4 m g /m in
0 .0 0 -1 0 .0 0 -1 5 0 .0
1 0 0 .0 2 0 0 .0 3 0 0 .0 4 0 0 .0 5 0 0 .0
T e m p Ce l
Fig. 5.18: (b) TG/DTA/DTG curves of NaOH treated (for five hours) banana fiber-polyester
resin composites of 5% fiber content.
129

Table 5.6: Effect of heating on mass loss (%) events at different temperature intervals, onset of
major degradation, and maximum slop of degradation observed on TG curve.
Sample NaOH Mass loss (%) Onset of major Maximum slop of

treated degradation degradation
hour –
Fiber % 1st stage 2nd stage 3rd stage Temp. Mass Temp. Mass
of comp. (50-180oC) (180-450oC) (450-600oC) (oC) loss (%) (oC) loss (%)
PR ---- 0 86.9 0 358.5 92.3 393.8 39.8
UBF ---- 3.7 71.2 0.3 321.0 90.4 372.3 40.0
TBF 1 h – 0% 3.7 76.4 2.9 327.4 92.8 371.0 38.6
TBF 5 h – 0% 3.3 64.8 3.5 331.0 93.3 369.7 48.9
UBF-PR 0 h – 5% 1.3 83.4 1.3 345.8 94.5 393.2 41.2
UBF-PR 0 h–10% 1.6 82.6 1.4 345.0 90.7 390.0 45.2
UBF-PR 0 h–20% 2.5 76.4 1.5 344.3 89.7 387.2 46.3
TBF-PR 1 h – 5% 3.2 69.2 1.2 351.2 87.1 393.7 41.0
TBF-PR 2 h – 5% 1.9 75.7 0.7 363.2 88.0 397.0 41.2
TBF-PR 5 h – 5% 2.5 79.5 0.8 354.2 91.7 399.8 38.7
Table 5.7: Effect of heating on the peak positions and rates observed on DTA and DTG curves.
Sample NaOH treated Peak position of DTA Peak position of DTG

hour – Fiber % Position Rate Position Rate
of composites (oC) (uv) (oC) (mg/min.)
PR ---- 395.3 9.11 394.3 0.462
UBF ---- 371.1 7.22 372.3 0.433
TBF 1 h – 0% 373.0 9.52 371.3 0.739
TBF 5 h – 0% 375.9 8.99 369.7 1.253
UBF-PR 0 h – 5% 390.5 5.32 393.9 1.484
UBF-PR 0 h–10% 390.0 5.95 393.8 1.568
UBF-PR 0 h–20% 389.2 6.13 393.7 1.710
TBF-PR 1 h – 5% 394.6 7.41 394.1 1.460
TBF-PR 2 h – 5% 399.7 6.92 397.0 1.610
TBF-PR 5 h – 5% 395.2 3.31 400.2 2.470
130

closely related. The peak position of DTG increases from 394.1 to 400.2 oC with the increase of
NaOH treatment time which is also higher than that of PR sheet, fibers and untreated composites.
This is, because, on treatment of NaOH solution, the fiber looses hemicelluloses, cellulose, lignin
and other soluble matters from its surface. Thus, it can be concluded that the banana fibers-
polyester resin composites are thermally more stable than PR heet and fibers.
5.4 Structural Analysis
5.5.1 Infrared spectroscopy analysis
Fig. 19: FTIR spectra of (a) untreated banana fiber (UBF), (b) untreated banana fiber-polyester
resin composite (UBF-PR), (c) treated banana fiber (TBF) for 1 h and treated banana fiber-
polyester resin composite (TBF-PR) for 5 h.
The FTIR spectra of raw banana fiber and banana fiber-polyester resin composites are shown in
Fig. 5.19(a) – (b). The spectra bands are clarified in Table 5.8. Lignocellulosic natural fibers
consist of the primary components: cellulose, hemicellulose, and lignin. The same is observed
from the FTIR spectra. Peaks in the region around 1029 – 1255 cm-1 are predominantly due to
the C–O–C and C–O stretching of primary and secondary hydroxyl groups in cellulose, lignin
and their glycosidic linkage [16–18]. Similarly, peaks near 1317 – 1506 cm-1 correspond to C=O
131

starching, which is due to the ketonic groups that belongs to the cellulose chain. The peaks
around 700 – 896 cm-1 belongs to typical structure of cellulose. Additionally –OH stretching
peak in a region around 3188 – 3327 cm-1 and absorption around 1600 cm-1 reveals the moisture
which may be broad and diffused with treatment of NaOH. The peaks at 2954 and 2872 cm-1 are
due to aliphatic groups –C–H that reveals from polyester resin [17]. The bands around 1681 –
1718 cm-1 correspond to carbonyl stretching vibrations of acetate group in polyester resin. The
vibrational modes after NaOH treatment did not suffer significant changes and the main bands
appeared approximately in the same range of the wave numbers.
Table 5.8: Assignments of FTIR absorption bands for banana fiber and banana fiber-polyester
resin composites.
Assignments Wave number (cm-1)

UBF UBF-PR TBF for 1 h TBF-PR for 5 h
–OH stretching 3207, 3286, 3288, 3323
3327, 3188
–C–H 2954 2954
CH2 symmetric 2872, 2881
stretching
Carbonyl stretching 1718 1681, 1714
Moisture 1595 1598, 1577 1579, 1598
C=O stretching 1317, 1419, 1338, 1369, 1317, 1371, 1338, 1371,
1456, 1506 1490, 1448 1419, 1454 1444, 1492
C–O stretching 1234, 1255, 1234, 1261 1253
C–O–C skeletal 1031, 1049, 1039, 1066, 1029, 1101, 1039, 1066,
stretching 1105, 1157 1118 1157 1116
Typical structure of 806, 823, 833, 700, 740, 852, 871, 896 700, 740, 848,
cellulose 860, 896 873 871
547, 563, 582 549 557, 611 503, 650
132

5.5 Summary of this Chapter
Physical observations of banana fiber-polyester resin composites
It is observed that the bulk density of untreated (raw) banana fiber-polyester resin composites
decreases with the increase of fiber content. The density is always improved on treatment of fiber
with NaOH. The bulk density of treated samples is higher than that of untreated sample. The
density of the treated sample (for five hours) of 10% fiber content exhibits maximum which is
1.215 g/cc whereas at the same fiber content for untreated sample, it is 1.011 g/cc. This can be
due to the fact that the fiber looses hemicellulose, lignin and other soluble matters (i.e. pectin,
wax, etc.) from the outer surfaces and becomes packed on treatment with alkali.
The water absorption of banana composites depends on amount of fiber loading and soaking
time. The rate of water absorption increases rapidly with soaking time up to 12 h and then
reaches a maximum or saturation point and after that it remains more or less constant. Water
absorption is also increased with addition of fiber content indicating diffusion phenomenon. But
the water absorption rate is decreased with the increase of NaOH (5% solution) treatment time.
This can be attributed to possible decrease hemicellulose, lignin and other alkali soluble matters
(pectin, wax, etc.).
Mechanical observations of banana fiber-polyester resin composites
The tensile strength of banana composites decreases during the initial stages of fiber loading
which indicates that the load is not properly transmitted to the fibers. But this strength increases
with increasing the fiber percentage from 5%. This should be because of the increased bonding
between the fiber and the matrix. The load sharing is easily transmitted to the fibers. The
Young’s modulus of composites increases with fiber addition indicating that the increase of
stiffness. It is apparent that the % of elongation decreases with increasing fiber content resulting
in lesser ductility. The tensile energy gradually decreases with the increase of fiber addition up to
10% and then increases or constant. This energy of treated sample is lower than that of untreated
fiber composites. The tensile properties of composites also increase with the increase of NaOH
treatment time. This suggests that due to treatment of fibers with alkali, the interfacial strength
might have slightly increased and aided mechanical interlocking between the fiber and matrix.
133

The results of flexural properties are similar to those of tensile properties. The flexural strength
of these composites decreases with the increase of fiber content up to 10% and then increases
with composition. At lower content of fiber, the interfacial bonding is poor due to presence of
lignin, fatty and waxy materials. So, the fibers do not share the load with matrix. In further
addition of fiber (20%), both the fiber and matrix bear the load and make good interfacial
bonding between the fiber and matrix. The flexural strain to Fmax decreases with the increase in
fiber loading. These imply that the composites became stiff and brittle on introducing the fiber.
The flexural properties are improved with the increase of NaOH treatment time.
Electrical observations of banana fiber-polyester resin composites
In the case of electrical measurement, it is shown that AC conductivity increases with the
increase of frequency and not much dependent on temperature. At lower frequency region
conductivity increases steadily up to 105 Hz whereas at higher frequency region (>105 Hz) it
increases faster. The conduction mechanism may be hopping of charge carriers in these
materials. The values of the exponent ‘n’ in σac(ω) = Aωn for various frequency region at
different temperature is also supported this view. The values of ‘n’ are found to be 0.53 – 0.65 in
the low frequency region (1 – 10 kHz) and 1.09 – 1.50 in the high frequency region (above 10
kHz). The value of index ‘n’ is high enough that is required for Debye type relaxation process.
The dielectric constant decreases with increasing frequency and this constant improves with
increasing temperature. The value of dielectric constant is high and all specimens exhibit a
normal dielectric behavior of materials, which may be due to the interfacial polarization.
Dielectric constant decreases sharply at low frequency region (100 – 900 Hz) and smoothly
decreases at high frequency region. At lower frequency the value of dielectric constant is much
high as compare to higher frequency indicating ionic effect. At low frequency the dipoles line up
in the field, reverse direction when the field is reversed, and so contribute to a high dielectric
constant. There is a big dip observed in the loss tangent behavior. The dip is found to maximum
at around 100 kHz. The loss tangent gradually decreases with increasing frequency up to 100
kHz and after that it increases sharply with increasing frequency. Electrical properties are
decreased with increasing fiber content and treatment time of NaOH. It may happen because of
the oxygen vacancy, hydroxyl ion motion or interfaces between the fiber and matrix. Interfacial
type relaxation is observed in these composites.
134

TG/DTA/DTG observations of banana fiber-polyester resin composites
The mass loss profile of polyester resin undergoes two separate degradation steps under heating
whereas mass loss profile of banana fibers and composites are parted three stages. Mass loss
profile of banana fibers changes considerably when they are treated with NaOH solution. On
treatment with alkali, mass loss (%) in major degradation region decreases with an increase in
amount (%) of final residual mass (carbonaceous char). This may be due to removal of lignin,
hemicelluloses and other alkali soluble components from the surface of the fiber as result of the
treatments increasing the number of reactive hydroxyl groups on the fiber surface. Major
degradation stage of the banana fiber shifts towards higher temperature along with increase in
maximum degradation rate on treatment with alkali. The treatment enhances thermal stability of
the fiber.
The TG/DTA/DTG profiles of banana fiber-polyester resin composites reflect those of fibers and
resin. The banana fibers played as an initial source of ignition in fiber-polyester resin
composites. The major mass loss (%) depends on the percentage of fiber content. Major
degradation stage, maximum degradation rate, and endothermic peak of composites shifts
towards higher temperature as compare to polyester resin and fibers. Therefore, the banana
composites are thermally more stable than that of fibers and polyester resin.
FTIR observations of banana fiber-polyester resin composites
The observed FTIR spectra of banana fiber and composites are characterized of lignocellulosic
fiber, which consist of cellulose, hemicellulose, and lignin. The band (peck) in the region around
1029 – 1255 cm-1 are predominantly due to the C–O–C and C–O stretching of primary and
secondary hydroxyl groups in cellulose, lignin and their glycosidic linkage. The peaks at 2954
and 2872 cm-1 are due to aliphatic groups –C–H that reveals from polyester resin. The bands
around 1681 – 1718 cm-1 correspond to carbonyl stretching vibrations of acetate group in
polyester resin. The vibrational modes after NaOH treatment did not suffer significant changes
and the main bands appeared approximately in the same range of the wave numbers. So, the
cellulose is not affected by treatment of NaOH.
135

References
[1] Islam M. N., Gafur M. A., and Khan A. H., “Natural fiber-polypropylene (Banana-PP)
matrix composites – fabrication and study of mechanical properties”, Jahangirnagar
Physics Studies, 13, 1–7, 2007.
[2] ASTM Designation: C134–137, Standard test method for size and bulk density refractory
brick and insulating fabric.
[3] Ghosh R., Krishna A. R., Reena G., and Raju Bh. L., "Effect of fiber volume fraction on
the tensile strength of banana fiber reinforced vinyl ester resin composites”, Int. J. Adv.
Eng. Sci. and Technol., 4, 089–091, 2011.
[4] Pickering K. L., Abdalla A., Ji C., McDonald A. G., and. Franich R. A, Composites Part A:
Appl. Sci. and Manufac., 34, 915–926, 2003.
[5] http://en.wikipedia.org/wiki/cellulose.
[6] Nayak S. K., Mohanty S., and Samal S. K., “Influence of interfacial adhesion on the
structural and mechanical behavior of PP-banana/glass hybrid composites”, Polym.
Compos., 1247–1257, 2010.
[7] Davallo M., Pasdar H., and Mohseni M., “Mechanical properties of unsaturated polyester
resin”, Int. J. Chem. Tech. Res., 2, 2113–2117, 2010.
[8] Mwaikambo L. Y. and Ansell M. P., Compos. Sci. and Tech., 63, 1297–1305, 2003.
[9] Beckermann G. W., Pickering K. L., and Foreman N. J., The 2nd international conference
on structure, processing and properties of materials. Dhaka, Bangladesh, SPPM2004, 257–
265, February, 2004.
[10] Khanna O. P., “A text book of material science and metallurgy” Published by Dhanpat Rai
Publications (P) Lit., New Delhi, India, 23–25, First Edn. 1999, Reprint 2004.
[11] Alam S. N., Pickering K. L., and Fernyhough., “The characterization of natural fibers and
their interfacial and composites properties”, The 2nd International Conference on Structure,
Processing and Properties of Materials, Dhaka, Bangladesh, SPPM2004, 248–256,
February 2004.
[12] Koops C. G., “On the dispersion of resistivity and dielectric constant of some
semiconductors at audio frequencies”, Phys. Rev., 83, 121–124, 1951.
[13] Tashdidd Benta Islam, “An investigation of the AC electrical properties of polypropylene
bijoypur white clay composites”, M. Sc. Thesis, Dept. of Physics, University of Dhaka,
July 2009.
[14] Yang H. P., Yan R., Chen H. P., Zheng C. G., Lee D. H., and Liang D. T., “Mechanism of
palm oil wastes pyrolysis in a packed bed”, Energy Fuels., 20, 1120–1128, 2006.
136

[15] Ouajai S., and Shanks R. A., “Composition, structure and thermal degradation of hemp
cellulose after chemical treatments”, Polym Degrad Stab., 89, 327–335, 2005.
[16] Yang H., Yan R., Chen H., Lee D. H., and Zheng C., “Characteristics of hemicellulose,
cellulose and lignin pyrolysis” Fuel, 86, 1781–1788, 2007.
[17] Barreto A. C. H., Costa M. M., Sombra A. S. B., Rosa D. S., Nascimento R. F., Mazzetto
S. E., and Fechine P. B. A., “Chemically modified banana fiber: structure, dielectrical
properties and biodegradability”, J. Polym. Environ., 18, 523–531, 2010.
[18] Jandas P. J., Mohanty S., Nayak S. K., Srivastava H., ” Effect of surface treatments of
banana fiber on mechanical, thermal, and biodegradability properties of PLA/banana fiber
biocomposites”, Polym. Compos., 00, 1689-1700, 2011.
137

Chapter 6 Conclusions
CONCLUSIONS
6.1 Conclusions
Fiber-matrix interactions play a crucial role in determining the properties of their relative
composites. The incorporation of hydrophilic nature of banana fiber in polyester resin
composites leads to heterogeneous systems, whose properties are inferior respect to those of the
unfilled system as a result of the poor adhesion at the fiber matrix interface. The pre-treatment of
the fiber with a suitable additive of NaOH prior to processing leads to good fiber dispersion in
the composite and significantly improve mechanical properties. A simple hand lay-up press
molding process was used to produce banana fiber-polyester resin composites using different
weight percentage of fiber content. The various physical, mechanical, electrical, thermal and
structural analyses were carried out to understand the nature of this composite. The results
obtained in the present work are summarized as follows:
• Banana fibers and composites consist of cellulose, hemicellulose and legnin. Cellulose is
not affected by treatment of 5% NaOH solution.
• Banana fiber-polyester resin composites are more stable than fiber and matrix.
• Bulk density of composites are decreased with fiber addition and always improved on
treatment of NaOH. Water absorption rate is increased with soaking time and addition of
fiber content indicating diffusion phenomenon. But the water absorption rate is decreased
with the increase of treatment time.
• Tensile and flexural properties of composites are increased with the increase of fiber
content and treatment time. The interfacial strength might have increased and aided
mechanical interlocking between the fiber and matrix due to treatment of alkali.
• AC conductivity is increased with the increase of frequency and not much dependent on
temperature. The conduction mechanism is due to hopping of charge carriers. The value
of dielectric constant is high and all specimens exhibit a normal dielectric behavior of
materials, which may be due to the interfacial polarization. Electrical properties are
decreased with increasing fiber content and treatment time of NaOH.
138

Chapter 6 Conclusions
Thus, the outcome of this study indicates that the reinforcement of banana fiber in polyester resin
composites can be used in the industrial and household application because it has high
mechanical, lower water absorption capacity, good electrical and stable thermal properties.
6.2 Suggestions for future work
The physical, mechanical, AC electrical, thermal and structural (FTIR) behavior of banana fiber
as reinforcing agent in polyester resin matrix are investigated in the present work. More
investigations are needed to explain different characteristics elaborately, which will help finding
suitable application of these composites. The following investigations may be carried out for
further study.
For better mixing and distribution, the fiber should be extruded with polymer. Further detail
physical and mechanical properties should be investigated. Microhardness can be measured.
For better understanding, surface morphology of the fiber and fracture surface of the composite
should be investigated with scanning electron microscope (SEM). X-ray diffraction can be
studied for more structural investigation.
In AC electrical measurement relaxation time can be studied. For current-voltage relationship

DC electrical measurement can be observed. These investigations can help to identify the
dominant charge conduction mechanism operative under DC field in composites.
Optical properties can be carried out by UV spectroscopy study.
139

Electrical and Mechanical Properties of Banana Fiber Reinforced Polyester Composites

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Electrical and Mechanical Properties of Banana Fiber Reinforced Polyester Composites

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ELECTRICAL AND MECHANICAL PROPERTIES OF

BANANA FIBER REINFORCED POLYESTER

A THESIS SUBMITTED TO THE DEPARTMENT OF PHYSICS, BANGLADESH

Certification of Thesis Work

The thesis titled “ELECTRICAL AND MECHANICAL PROPERTIES OF BANANA

2.1 Review of the Earlier Research Works

5.1 Physical Properties of Composites

Chapter 2: Literature Survey (10–23)

Chapter 3: Theoretical Background (24–79)

Chapter 4: Materials and Methods (80–99)

Chapter 5: Results and discussion (100–137)

Chapter 6: Conclusions (138–139)

Table 3.1: Properties of select natural fibers. 33

is concrete. It consists of a binder and reinforcement. Adding another reinforcement transforms

Particle-reinforced Fiber-reinforced Structural

Large- Dispersion- Continuous Discontinuous Laminates Sandwich

Aligned Randomly oriented

1.2 Objective of the Present Study

1.3 Outline of this Thesis

1.4 Summary of this Thesis

Chapter 2: Literature Survey

Chapter 3: Theoretical background

Chapter 4: Materials and methods

Chapter 5: Results and discussion

References are added at the end of each chapter.

2.1.1 Study of chemical modification of natural fibers

Acetylation is beneficial in reducing the moisture absorption of natural fibers. Reduction of

2.1.2 Study of banana fiber reinforced polymer composites

2.1.3 Study of other natural fibers reinforced polymer composites

3.1.1 Classification of polymers

Polymers are also classified as organic and inorganic polymers:

In polymer chemistry, polymerization is a process of reacting monomer molecules together in a

Chain-growth polymerization: Chain growth polymerization (or addition polymerization)

Other forms of chain-growth polymerization include cationic addition polymerization and

Step-growth polymerization: Step-growth polymers are defined as polymers formed by the

Copolymerization: The process of polymerizing a single monomer or a single monomer pair is

Homopolymerization: A +A + A… → AAA… (homopolymer)

3.1.3 Polymer properties

crystalline [11]. The crystallinity of polymers is characterized by their degree of crystallinity,

Glass transition temperature: A parameter of particular interest in synthetic polymer

3.2 Natural Fiber

Table 3.1: Properties of select natural fibers [15].

Property Jute Banana Sisal Pineapple Coir

3.2.1 Structure and occurrence of natural fibers

3.2.2 Classification of fibers

Reinforcing natural fibers/ fillers

Non-wood natural fibers Wood fibers

Soft and hard woods

Straw Bast Leaf Seed/ fruit Grass

Examples: Example: Examples: Examples: Examples:

3.2.3 Banana fibers

3.2.4 Chemical composition of natural fibers

Table 3.2: Average chemical amounts of some natural fiber.

Constituents Amounts (percentage dry basis)

The structure of cellulose :

Fig. 3.3: Structure of cellulose.

Fig. 3.4: Hydrogen bonding in adjacent chains.

between the adjacent chain molecules of cellulose [22].

Hemicellulose: Hemicellulose is a group of cell wall polysaccharides. The isolated hemicellulose

S tru ctu ra l u n it of lig n in :

Over all structure of lignin:

Fig. 3.6: Structure of lignin.

3.2.5 Physico-mechanical properties of natural fibers