ENHANCEMENT OF TENSILE STRENGTH PROPERTIES OF

BIOPOLYMER SODIUM ALGINATE NANOCOMPOSITE

FILMS BY INCORPORATION OF NITROGEN DOPED
GRAPHENE
A THESIS
Submitted in the partial fulfillment of the requirements for the award of the
degree of
MASTER OF TECHNOLOGY
in

NANOTECHNOLOGY
By
KOTTAPALLI VENKATESH
[Registration no: 15IS1D9608]
Under The Guidance of
Dr. Ch. Kiran Kumar
DST – Inspire Faculty
JNTUK, Kakinada

SCHOOL OF NANOTECHNOLOGY
INSTITUTE OF SCIENCE AND TECHNOLOGY
JAWAHARLAL NEHRU TECHNOLOGICAL UNIVERSITY KAKINADA
KAKINADA – 533 003
2015 – 2017
 DECLARATION

I, KOTTAPALLI VENKATESH hereby declare that the work which is

being described in this dissertation report entitled “ENHANCEMENT OF
TENSILE STRENGTH PROPERTIES OF BIOPOLYMER SODIUM
ALGINATE NANOCOMPOSITE FILMS BY INCORPORATION OF
NITROGEN DOPED GRAPHENE” is entirely original and was carried out by me
independently at Nanotechnology laboratory JNTUK, Kakinada, under the
supervision of Dr. Ch. KIRAN KUMAR, DST – INSPIRE Faculty, School of
Nanotechnology, Institute of Science and Technology, JNTU Kakinada, encouraged
me to work in JNTU Kakinada. I further declare that this dissertation has not been
submitted to any other degree or diploma in any university or institute.

Date: KOTTAPALLI VENKATESH

Place: Regd. No: 15IS1D9608
 ACKNOWLEDGEMENT

It is a great pleasure to express my sincere gratitude to my supervisor, Dr . C h . Ki r an Kum a r ,

forgiving me an opportunity to work in his lab and for his valuable guidance and continuous
encouragement and also for the facilities provided in accomplishing my project work.

I am very much grateful to Dr. K. Babulu, Director, IST, and Dr. B. Prabhakara Rao, Programme
Director School of Nanotechnology, JNTUK Kakinada for their continuous support and for
providing me with necessary facilities in the laboratory.

I take this opportunity to express my sincere thanks to Dr. A. Gopala Krishna, Director of Design
and Innovation centre who helped me throughout my project.

I also extend my sincere thanks to all the other faculty Mr. P. Srinivasa Subbarao, Mr.S.S.S.Rao,
Mr.Ch. Krishnarao, for their valuable guidance and help.

I also extend my sincere thanks to Dr. Rama Krishna, head of the department, vignan university,
who helped me in conducting of tensile test for polymer films in his laboratory.

I also extend my sincere thanks to Vijay kumar, faculty of chemistry department of Andhra
university who helped me in conducting of XRD in his lab.

My family members receive my deepest gratitude and love for their extreme support throughout
my academic years.
I am thankful to one and all who contributed my work directly or indirectly.
 ABSTRACT

Different concentrations of n-doped graphene was prepared and these powder concentrations was
mixed seperately with with sodium alginate solution followed by magnetic stirring and ultra
sonication process. These concentration was poured separately in a petty dish followed by
being left undisturbed for 36 h at 40 °C, allowing formation of the nano-composite film. Sodium
alginate (SA) is a water-soluble salt of alginic acid originating from a naturally occurring
nontoxic polysaccharide found in all species of brown algae isolated from brown Seaweeds.
Three polymer matrix nano composite films (film-1, film-2, film-3) followed by one neutral (i.e,
only sodium alginate solution)and g-c3n4 and only graphene polymer were characterized by
using characterization techniques UV absorbance spectrum, X Ray Diffraction Technique,
Scanning Electron Microscopy, Fourier Transform Infra Red. Mechanical Properties of Films like
tensile strength was determined by using Extensometer (Electro Tensile Testing Machine) and it
is found that film formed by inducing nano powders of graphene in 1:4 ratio is observed to
exhibit highest tensile strength.

Key Words: g-C3N4, sodium alginate, melamine, Fourier Transform Infra Red Spectroscopy,
Nano Composite film, Extensometer, Tensile Strength.
 Table of Contents
Page
Content no
Acknowledgement
Abstract
List of Figures
List of Abbreviations

Chapter
Chapter Name
no

1 Introduction

1.1 Nanotechnology-A Small science, Big dreams 2

1.2 Nanotechnology 3
1.3 Nanotechnology Improvements
3

1.4 Nanoparticles 4
1.5Synthesis of Nanoparticles 5
1.5.1 Physical Methods 5
1.5.2 Chemical Techniques 6
1.5.3 Biological Methods
1.5.4 Synthesis of Nanoparticles via Hybrid Methods
1.6 Structure and Properties of Nanoparticles
1.7 Applications of Nanotechnology 10
1.8 Nanotechnology in Renewable Energy 12

2 Literature Survey

2.1 Effect of graphene on sodium alginate 16

2.2 Tensile Strength of sodium alginate films 16
2.3 Polymer Matrix Nano Composite Films 17

3 Polymer Matrix Nano Composites

3.1 Classification of Polymers 20

3.2 Classification of Composites 20
 3.3 Functions of Matrix 20
3.4 Desired Properties of Matrix 21
3.5 Sodium Alginate 21
3.6 Use of Sodium Alginate 22
3.7 g-C3N4 24

4 Synthesis

4.1 Synthesis N-Doped Graphene in Different Concentrations 26

4.2 Synthesis of g- C3N4 27
4.3 Synthesis of Sodium Alginate Solution 28
4.4 Synthesis of Sodium Alginate Based g-C3N4 film
29

4.5 Synthesis of Sodium Alginate based N-Doped graphene film in 1:1

concentration of graphene and melamine

30
4.6 Synthesis of Sodium Alginate based N-Doped graphene film in 1:2 31
4.7 Synthesis of Sodium Alginate based N-Doped graphene film in 1:4 32
4.8 Synthesis of Sodium Alginate based Only graphene film 33

5 Characterization Techniques
5.1 X-ray Diffraction 35
5.2 Tensile Testing 38
5.3 UV- Spectroscopy 40
5.4 Fourier Transform Infrared (FTIR) Spectroscopy 42
5.5 Scanning Electron Microscope 44

6 Results and Discussions

6.1 Tensile Test 50
6.2 Result of The Sodium Alginate Based N-Doped Graphene in 1:4 52
6.3 XRD 53
6.4 SEM 55
6.5 EDX – Energy Dispersive X-Ray Analyzer 63

7 Conclusion & Future Scope 73

8 References 75
 LIST OF FIGURES

Figure 1.1 Materials in Nanometer scale………………………………………………………3

Figure 1.2 Classification of NPs……………………………………………………………….4
Figure 1.3 Methods of NPs ynthesis…………………………………………………………...5
Figure 1.4 Laser Ablation……………………………………………………………………...5
Figure 1.5 Inert Gas Condensation…………………………………………………………….6
Figure 1.6 Chemical Vapour Deposition………………………………………………………7
Figure 1.7 Hydrothermal Synthesis……………………………………………………………7
Figure 1.8 Nanoparticles in comparison with biological entities…………………………….10
Figure 3.1 Composites classification…………………………………………………………20
Figure 4.1 g-C3N4 stored in a crucible after preparation……………………………………...27
Figure 4.2 Film formed by only sodium alginate solution for reference purpose……………28
Figure 4.3 g-C3N4 induced sodium alginate based nanocomposite film……………………..29
Figure 4.4 Polymer film formed by 1:1 concentration with sodium alginate………………...30
Figure 4.5 Polymer film formed by 1:2 concentration with sodium alginate………………...31
Figure 4.6 Polymer film formed by 1:4 concentration with sodium alginate………………...32
Figure 4.7 Polymer film formed by only graphene with sodium alginate…………………... 33
Figure 5.1 Diffraction of X-ray from Crystal Surface………………………………………..36
Figure 5.2 X- Ray diffract meter……………………………………………………………..37
Figure 5.3 Universal testing machine (UTM)………………………………………………..40
Figure 5.4 UV spectroscopy………………………………………………………………….41
Figure 5.5 Fourier Transform Infrared Spectrometry………………………………………...42
Figure 5.6 Fourier Transform Infrared Instrumentation……………………………………...43
Figure 5.7 Scanning electron microscope…………………………………………………….45
Figure 5.8 Schematic diagram of SEM………………………………………………………46
Figure 5.9 Electron gun………………………………………………………………………47
Figure 5.10 SEM detectors…………………………………………………………………….48
Figure 6.1 Extensometer………………………………………………………………….…..51
Figure 6.2 Testing tensile strength of sodium alginate based films………………………….51
Figure 6.3 Indication of force at which 3 films breaks………………………………………52
Figure 6.4 Graph showing load for the 1:4 sample…………………………………………..52
Figure 6.5 XRD of g – C3N4 …………………………………………………………………………………………………..53
Figure 6.6 XRD of powder 2…………………………………………………………………54
Figure 6.7 First SEM image of n-doped graphene 1:1 ratio………………………………….55
Figure 6.8 Second SEM image of n-doped graphene 1:1 ratio………………………………56
Figure 6.9 Third SEM image of n-doped graphene 1:1 ratio………………………………...56
Figure 6.10 Fourth SEM image of n-doped graphene 1:1 ratio……………………………….57
Figure 6.11 Fifth SEM image of n-doped graphene 1:1 ratio…………………………………57
Figure 6.12 First SEM image of n-doped graphene 1:2 ratio………………………………….58
Figure 6.13 Second SEM image of n-doped graphene 1:2 ratio………………………………58
Figure 6.14 Third SEM image of n-doped graphene 1:2 ratio………………………………...59
Figure 6.15 Fourth SEM image of n-doped graphene 1:2 ratio……………………………….59
Figure 6.16 Fifth SEM image of n-doped graphene 1:2 ratio…………………………………60
Figure 6.17 First SEM image of n-doped graphene 1:4 ratio………………………………….60
Figure 6.18 Second SEM image of n-doped graphene 1:4 ratio………………………………61
Figure 6.19 Third SEM image of n-doped graphene 1:4 ratio………………………………..61
Figure 6.20 Fourth SEM image of n-doped graphene 1:4 ratio…………………………...…62
Figure 6.21 Fifth SEM image of n-doped graphene 1:4 ratio………………………………..62
Figure 6.22 Sixth SEM image of n-doped graphene 1:4 ratio………………………………..63
Figure 6.23 Image of n-doped graphene 1:1 ratio showing electron image………………….63
Figure 6.24 Graph of n-doped graphene 1:1 ratio……………………………………………64
Figure 6.25 Image of n-doped graphene 1:1 ratio showing electron image………………….65
Figure 6.26 Graph of n-doped graphene 1:1 ratio……………………………………………65
Figure 6.27 Image of n-doped graphene 1:2 ratio showing electron image………………….66
Figure 6.28 Graph of n-doped graphene 1:2 ratio……………………………………………67
Figure 6.29 Image of n-doped graphene 1:2 ratio showing electron image………………….68
Figure 6.30 Graph of n-doped graphene 1:2 ratio……………………………………………68
Figure 6.31 Image of n-doped graphene 1:4 ratio showing electron image………………….69
Figure 6.32 Graph of n-doped graphene 1:4 ratio……………………………………………69
Figure 6.33 Image of n-doped graphene 1:4 ratio showing electron image………………….70
Figure 6.34 Graph of n-doped graphene 1:4 ratio……………………………………………71
 List of Abbreviations

1. NPs: Nanoparticles
2. g-C3N4: Graphitic Carbon Nitride
3. SEM: Scanning Electron Microscope
4. UV- vis : Ultra Violet visible Spectroscopy
5. EDX: Energy Dispersive X-Ray Spectroscopy
6. DLS: Dynamic Light Scattering
7. GMR: Giant Magneto Resistance
8. TEM: Transmission Electron Microscopy
9. FTIR: Fourier Transform Infrared Spectroscopy
10. SPR: Surface Plasmon Resonance
11. SERS: Surface-enhanced Raman Spectroscopy
12. DNA: Deoxyribonucleic Acid
13. mM: Millimolar
14. min: Minutes
15. ml: Milliliter
16. µL: Micro liter
17. rpm: Rotations Per Minute
18. nm: Nanometer