UNIVERSITI PUTRA MALAYSIA

STRUCTURAL, OPTICAL AND ELASTIC PROPERTIES OF ZINC OXIDE

SODA LIME SILICATE GLASS

MOHD HAFIZ MOHD ZAID

FS 2011 58

© COPYRIG

HT UPM

STRUCTURAL, OPTICAL AND ELASTIC PROPERTIES OF ZINC OXIDE

SODA LIME SILICATE GLASS

By

MOHD HAFIZ MOHD ZAID

Thesis submitted to the School of Graduate Studies, Universiti Putra Malaysia, in

Fulfillment of the Requirements for the Degree of Master of Science

December 2011

© COPYRIG

HT UPM

ii

Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfillment of

the requirement for the degree of Master of Science.

STRUCTURAL, OPTICAL AND ELASTIC PROPERTIES OF ZINC OXIDE

SODA LIME SILICATE GLASS

By

MOHD HAFIZ MOHD ZAID

December 2011

Chair : Khamirul Amin Matori, PhD

Faculty : Faculty of Science.

So far, most research had been done to understand the properties and advantages of soda

lime silicate (SLS) glass compare to others glass and also to improve their quality.

Addition of oxide into the glass system had been a topic of research for nearly half

century, but many questions still remain unanswered concerning to the effect of the

addition of some oxide to the properties and the structure changes of the glass. In this

research, fabrication of a series of (ZnO)x(SLS)1-x glasses with weight percentage x from

0.05 to 0.40 were carried out by the melting and quenching technique. The chemical

composition of the (ZnO)x(SLS)1-x glasses were determined using Inductive Couple

Plasma (ICP) and Energy Dispersive X-ray Fluorescence (EDXRF). The amorphous

structure of the glass samples were confirmed using X-ray diffraction (XRD)

measurement. The glass density was measured by using Archimedes’ principle. The

© COPYRIG

HT UPM

iii

densities of the glass sample were increased with the addition of ZnO. The molar

volume of the glass samples shows a same trend with the density of the glasses which is

increased with the increased of ZnO content. Their physical properties such as elastic

properties were determined at room temperature by using non-destructive test; the

digital signal processing technique of Matec DSP MBS 8000. The experimental data of

wave velocities and densities were then used to determine the longitudinal modulus,

shear modulus, Young modulus, bulk modulus, Poisson’s ratio, fractal bond

connectivity and Micro-hardness in each series of (ZnO)x(SLS)1-x glass system. It was

found that the longitudinal modulus, shear modulus, Young modulus and bulk modulus

decreased with the addition of ZnO in the SLS glasses. These elastic properties of

glasses were found closely related to the strength of the glass structure. The values of

the elastic properties had been compared with the Rocherulle’s model and this model

shows a same trend which is the values of the longitudinal modulus, shear modulus,

Young modulus and bulk modulus of the glass samples decreased with the addition of

ZnO. The bonding in the (ZnO)x(SLS)1-x glasses were measured using IR Spectroscopy.

The shift band of IR spectroscopy must be occurs due to the addition of ZnO, which

means increase the non-bridging oxygens (NBOs) in the glass structure and resulting the

structural of the glass samples become weaker. The optical properties of the

(ZnO)x(SLS)1-x glass system were measured using UV-Visible spectroscopy. The values

of the optical band gap decreased with the addition of ZnO in the SLS glass system.

© COPYRIG

HT UPM

iv

Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk ijazah Master Sains.

STRUKTUR, OPTIK DAN SIFAT KEKENYALAN KACA ZINK OKSIDA

SODA LIME SILIKA

Oleh

MOHD HAFIZ MOHD ZAID

Disember 2011

Pengerusi : Khamirul Amin Matori, PhD

Fakulti : Fakulti Sains

Sehingga kini, banyak penyelidikan telah dilakukan untuk memahami sifat-sifat dan

kelebihan kaca soda lime silika (SLS) berbanding dengan kaca yang lain di samping

untuk meningkatkan kualiti kaca tersebut. Selain itu, penambahan oksida ke dalam

sistem kaca telah menjadi topik penyelidikan untuk hampir setengah abad, tetapi masih

terdapat banyak persoalan yang tidak terjawab mengenai kesan pernambahan oksida ke

atas sifat-sifat dan perubahan pada struktur kaca. Dalam kajian ini, fabrikasi siri kaca

(ZnO)x(SLS)1-x dengan x peratusan berat 0.05-0.40 telah dijalankan dengan

menggunakan teknik lindapan leburan. Komposisi kaca (ZnO)x(SLS)1-x telah ditentukan

menggunakan (ICP) dan (EDXRF). Struktur amorfus sampel kaca telah disahkan

dengan menggunakan pengukuran XRD. Seterusnya, ketumpatan kaca telah diukur

dengan menggunakan prinsip Archimedes. Ketumpatan sampel kaca telah meningkat

dengan penambahan ZnO. Isipadu molar sampel kaca juga menunjukkan bentuk yang

© COPYRIG

HT UPM

v

sama dengan ketumpatan gelas yang meningkat dengan peningkatan kandungan ZnO.

Sifat-sifat fizikal kaca seperti sifat kenyal ditentukan pada suhu bilik dengan

menggunakan teknik pemprosesan isyarat digital Matec DSP MBS 8000. Data halaju

gelombang dan ketumpatan kemudian digunakan untuk menentukan nilai modulus

memanjang, modulus ricih, Young modulus, pukal modulus, nisbah Poisson,

penyambungan bond fraktal dan micro-kekerasan dalam siri setiap daripada kaca

(ZnO)x(SLS)1-x. Didapati bahawa modulus memanjang, modulus ricih, modulus Young

dan modulus pukal menurun dengan pernambahan ZnO dalam kaca SLS. Ciri-ciri

kenyal kaca ini telah didapati berkait rapat dengan kekuatan struktur kaca. Nilai ciri

kenyal kaca ini telah dibandingkan dengan nilai teori daripada model Rocherulle dan

model ini menunjukkan bentuk yang sama dengan nilai-nilai modulus membujur,

modulus ricih, modulus Young dan modulus pukal sampel kaca menurun dengan

penambahan ZnO yang diperolehi dari eksperimen. Ikatan dalam kaca (ZnO)x(SLS)1-x

dikaji dengan menggunakan IR spektroskopi. Jalur peralihan IR spektroskopi mesti

berlaku disebabkan oleh tambahan ZnO, yang bermakna meningkatkan (NBOs) dalam

struktur kaca dan mengakibatkan struktur sampel kaca menjadi lemah. Kemudiannya,

ciri-ciri optik kaca diukur dengan menggunakan spektroskopi UV-Visible. Nilai-nilai

jurang jalur optik menurun dengan penambahan ZnO dalam sistem kaca SLS.

© COPYRIG

HT UPM

vi

ACKNOWLEDGEMENTS

First of all, I glad to say thank you ALLAH for providing me an effort and courage to

complete my study efficiently.

I would like to express my gratitude and lot of thanks especially to my project

supervisor, Dr. Khamirul Amin Matori for his invaluable advice patience and

constructive critics during the preparation of this thesis. Without his persistent and

exceptional generosity, valuable advices, critical comment and suggestion, this work

would not have been possible. Especially thanks to my co-supervisor, Assoc. Prof. Dr.

Zaidan Abdul Wahab, Prof. Dr. Azmi Zakaria and Dr. Halimah Mohamed Kamari for

giving a lot of support and precious guidelines during my study.

I would like to acknowledge Malaysia Ministry of Higher Education and Universiti

Putra Malaysia for funding this research through Graduate Research Foundation scheme

(GRF) and giving the opportunity to undertake and complete this study.

Finally, grateful thanks also to my dearest father, Mr. Mohd Zaid bin A. Bakar, my

beloved mother, Mrs. Kamsiah binti Mustaffa and my sister that have been so

supportive throughout my study. Credits are given to all the lecturers in Physics

Department, all Faculty of Science staff and friends who have directly and indirectly

give me a helping hand.

© COPYRIG

HT UPM

vii

I certify that a Thesis Examination Committee has met on 13 December 2011 to conduct

the final examination of Mohd Hafiz Mohd Zaid on his thesis entitled "Structural,

Optical and Elastic Properties of Zinc Oxide Soda Lime Silicate Glass" in accordance

with the Universities and University Colleges Act 1971 and the Constitution of the

Universiti Putra Malaysia [P.U.(A) 106] 15 March 1998. The Committee recommends

that the student be awarded the degree of Master of Science.

Members of the Thesis Examination Committee were as follows:

Wan Mahmood Mat Yunus, PhD

Professor

Faculty of Science

Universiti Putra Malaysia

(Chairman)

Sidek Hj. Ab. Aziz, PhD

Professor

Faculty of Science

Universiti Putra Malaysia

(Internal Examiner)

Chen Soo Kien, PhD

Senior Lecturer

Faculty of Science

Universiti Putra Malaysia

(Internal Examiner)

Rosli Hussin, PhD

Professor

Department of Physics, Faculty of Science

Universiti Teknologi Malaysia

Malaysia

(External Examiner)

SEOW HENG FONG, PhD

Professor and Deputy Dean

School of Graduate Studies

Universiti Putra Malaysia

Date:

© COPYRIG

HT UPM

viii

This thesis was submitted to the Senate of Universiti Putra Malaysia and has been

accepted as fulfilment of the requirement for degree of Master of Science. The members

of the Supervisory Committee were as follows:

Khamirul Amin Matori, PhD

Lecturer

Faculty of Science

Universiti Putra Malaysia

(Chairman)

Zaidan Abdul Wahab, PhD

Associate Professor

Faculty of Science

Universiti Putra Malaysia

(Member)

Halimah Mohamed Kamari, PhD

Lecturer

Faculty of Science

Universiti Putra Malaysia

(Member)

Azmi Zakaria, PhD

Professor

Faculty of Science

Universiti Putra Malaysia

(Member)

------------------------------------------------

BUJANG BIN KIM HUAT, PhD

Professor and Dean

School of Graduate

Universiti Putra Malaysia

Date:

© COPYRIG

HT UPM

ix

DECLARATION

I declare that the thesis is my work except for quotations and citations which have been

duly acknowledged. I also declare that it has not been previously and is not

concurrently, submitted for any other degree at Universiti Putra Malaysia or at any other

institutions.

--------------------------------------

MOHD HAFIZ MOHD ZAID

Date: 13 December 2011

© COPYRIG

HT UPM

x

TABLE OF CONTENTS Page

ABSTRACT ii

ABSTRAK iv

ACKNOWLEDGEMENT vi

APPROVAL vii

DECLARATION xi

LIST OF TABLES xiii

LIST OF FIGURES xv

LIST OF ABBREVIATIONS xvii

CHAPTER

1.0 INTRODUCTION 1

1.1 Research background 1

1.2 Problem statement 4

1.3 Objectives 5

1.4 Scope of the study 6

1.5 Important of the study 7

2.0 LITERATURE REVIEW 9

2.1 Introduction 9

2.2 Glass 11

2.2.1 Glass formation 13

2.2.2 Glass chemical composition 15

2.3 Soda lime silicate glass 17

2.4 Structure studies of glasses 19

2.5 Ultrasonic properties of glasses 23

2.6 Elastic properties of glasses 25

2.7 Rocherulle’s model 27

© COPYRIG

HT UPM

xi

2.8 Optical properties of glasses 29

3.0 EXPERIMENTAL TECHNIQUE 34

3.1 Introduction 34

3.2 Preparation of raw materials of glasses 35

3.2.1 Weighing, mixing and milling 36

3.2.2 Glass melting and casting procedure 37

3.2.3 Annealing 38

3.2.4 Cutting and polishing 38

3.3 X-ray diffraction 39

3.4 Chemical composition measurement 41

3.4.1 Inductive couple plasma spectroscopy 42

3.4.2 Energy dispersive X-ray fluorescence spectroscopy 45

3.5 Density measurement 48

3.6 Molar volume 50

3.7 Fourier transforms infrared spectroscopy 50

3.8 Ultrasonic wave velocity measurement 52

3.9 UV-Visible spectroscopy 56

4.0 RESULTS AND DISCUSSION 58

4.1 Introduction 58

4.2 XRD analysis 58

4.3 Chemical composition analysis 59

4.4 Density and molar volume analysis 63

4.5 Structure analysis by IR spectra 66

4.6 Ultrasonic velocities analysis 70

4.7 Elastic properties analysis 74

4.8 Optical properties analysis 95

5.0 CONCLUSIONS AND FURTHER RESEARCH 100

© COPYRIG

HT UPM

xii

5.1 Conclusions 100

5.2 Further study 102

REFERENCES/BIBLIOGRAPHY 105

APPENDICES 119

BIODATA OF STUDENT 121

LIST OF PUBLICATIONS 122