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UNIVERSITI PUTRA MALAYSIA

SHARUDIN BIN OMAR BAKI

FK 2013 61

PHYSICAL CHARACTERIZATION AND OPTICAL SPECTROSCOPY OF Er3/Yb3-DOPED MULTICOMPOSITION TELLURITE GLASS FOR

BROADBAND AMPLIFIERS

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PHYSICAL CHARACTERIZATION AND

OPTICAL SPECTROSCOPY OF Er3+/Yb3+-DOPED

MULTICOMPOSITION TELLURITE GLASS FOR



DOCTOR OF PHILOSOPHY

UNIVERSITI PUTRA MALAYSIA

2013

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PHYSICAL CHARACTERIZATION AND OPTICAL SPECTROSCOPY OF

Er3+

/Yb3+

-DOPED MULTICOMPOSITION TELLURITE GLASS FOR


By


Thesis Submitted to the School of Graduate Studies,

Universiti Putra Malaysia, in Fulfilment of the

Requirements for the Degree of

Doctor of Philosophy

June 2013

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Copyright Page

All material contained within the thesis, including without limitation text, logos,

icons, photographs and all other artwork, is copyright material of Universiti Putra

Malaysia unless otherwise stated. Use may be made of any material contained

within the thesis for non-commercial purposes from the copyright holder.

Commercial use of material may only be made with the express, prior, written

permission of Universiti Putra Malaysia.

Copyright © Universiti Putra Malaysia

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

of the requirement for the degree of Doctor of Philosophy

PHYSICAL CHARACTERIZATION AND OPTICAL SPECTROSCOPY OF

Er3+

/Yb3+

-DOPED MULTICOMPOSITION TELLURITE GLASS FOR


By


June 2013

Chairman: Professor Mohd Adzir bin Mahdi, PhD

Faculty: Engineering

The erbium ion doped (Er3+

)-tellurite glasses have been extensively studied in recent

decades as a potential host material for broadband applications at 1.5 m band. As

compared to other host glasses they possess variety interesting physical and optical

properties which further can be exploited especially in optical communications.

Therefore continuous investigation of appropriate glass compositions is very

important in order to synthesis high performance tellurite glass.

In this dissertation, series of selected oxide based tellurite glasses (TeO2) were

synthesized and characterized. Three ternary TeO2-AmOn-BmOn; TZT:TeO2-ZnO-

TiO2, TTB:TeO2-TiO2-Bi2O3, TPB: TeO2-PbO- Bi2O3 and two multicomposition

TeO2-AmOn-BmOn-CmOn-DmOn-EmOn (more than three components); TZPTiN:TeO2-

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ZnO-PbO-TiO2-Na2O (with difference PbO concentration) tellurite glasses were

studied (AmOn, BmOn, CmOn, DmOn, EmOn represent the oxide components,

m,n=integer). Selected batch composition was chosen as a ‘host’ glass for Er3+

/Yb3+

doping by substituting selected batch component with the rare earth oxide dopants

Er2O3/Yb2O3. All oxide components were above 99.9% purity and a quantitative

glass batching procedure based on mol% formulation calculation was performed. A

standard melt-quenching technique around 1000 oC for an hour and followed by

annealing at 250 oC was done for all glass batches. The physical characterization of

the glass samples involved X-Ray diffraction (XRD), thermal analysis, density,

molar volume and refractive index while the spectroscopic properties were obtained

through Fourier Transform Infra Red spectroscopy, Ultraviolet-Visible-Near Infra

Red absorption spectroscopy, Raman spectroscopy and fluorescence spectra of the

visible upconversion and near infra red emission under 980 nm laser diode (LD)

excitation. All measurement were performed at room temperature.

The non distinguishable intensity peaks with broad ‘halo’ diffraction of the XRD

spectrogram confirmed the amorphous nature of the selected host glasses. The

density of the glasses was observed higher with the incorporation of heavier mass

component of PbO and Bi2O3 in both TTB and TPB glasses where higher n values

were obtained in both glasses. All host glasses TZT, TTB, TPB, TZPTiN and

TZPTiN indicated higher n > 2. The FTIR analysis revealed higher transmission infra

red cut-off beyond 6m with distinct water (OH-) absorption between 2000-3500 cm

-

1 in most of the studied glass samples. The optical absorption edge analysis in most

samples showed an appreciable formation of non-bridging oxygen with respect to the

calculated optical energy gap trend. This was clearly supported by the obtained

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intensity parameters values t(t=2,4,6) through the Judd-Ofelt analysis. The

reduction of 2 and 6 values were strongly associated with enhancement of the

symmetrical behaviour at the Er3+

site with the creation of higher electron density on

the oxygen ligand ion; as consequences strong Er-O covalency are formed with the

increasing of Er3+

doping concentration. In addition this factor has also contributed

structural deformation of TeO2 by transformation of [TeO4] trigonal bypiramid to

[TeO3] trigonal pyramid via [TeO3+1] polyhedral units which was confirmed through

the Raman spectroscopy analysis with obtained maximum phonon vibration energy

lies between 730-750 cm-1

slightly lower than reference TeO2 glass value at

780 cm-1

. The upconversion spectra exhibited significant both green and red

emission upon 980 nm LD excitation especially in Er3+

-TZT and Er3+

/Yb3+

-TZPTiN

glasses where indicated by two or/and three photon absorption processes. Intense

with broad near infra red 1.5 m emission above 70 nm width and gain bandwidth

within (500-1300) x 10-28

cm3 were obtained in most Er

3+/Yb

3+-doped glass samples .

These characteristics suggest that the synthesized multicomposition tellurite glass is

a potential optical material for the future broadband telecommunication technology.

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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk ijazah Doktor Falsafah

PENCIRIAN FIZIKAL DAN SPEKTROSKOPIK

KACA TELURIT KEPELBAGAIAN KOMPOSISI TERDOP-Er3+

/Yb3+

UNTUK PENGUAT JALUR-LEBAR

Oleh


Jun 2013

Pengerusi: Profesor Mohd Adzir bin Mahdi, PhD

Fakulti: Kejuruteraan

Kaca telurit terdop-ion erbium (Er3+

) telah dikaji dengan giatnya sejak beberapa

kurun kebelakangan ini setelah dikenal pasti sebagai bahan hos berpotensi untuk

aplikasi jalur lebar pada jalur 1.5 m. Sebagai perbandingan dengan hos kaca yang

lain, ianya mempunyai pelbagai sifat fizikal dan optikal yang menarik di mana perlu

diekploitasikan lebih lanjut khususnya di dalam teknologi komunikasi optik. Oleh

yang demikian penyelidikan yang berterusan bagi komposisi kaca yang tepat adalah

amat penting bagi mensintesis kaca telurit berprestasi tinggi.

Di dalam disertasi ini, sesiri kaca berasaskan oksida telurit (TeO2) tepilih telah

disintesis dan dicirikan. Sebanyak tiga ternari TeO2-AmOn-BmOn; TZT:TeO2-ZnO-

TiO2, TTB:TeO2-TiO2-Bi2O3, TPB: TeO2-PbO- Bi2O3 dan dua pelbagai komposisi

TeO2-AmOn-BmOn-CmOn-DmOn-EmOn (lebih dari tiga komponen); TZPTiN:TeO2-

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ZnO-PbO-TiO2-Na2O (dengan kepekatan PbO berbeza) kaca-kaca telurit telah dikaji

(AmOn, BmOn, CmOn, DmOn, EmOn sebagai komponen-komponen oksida,

m,n=integer). Komposisi pengkelasan tertentu telah digunakan sebagai hos kaca

untuk pengedopan Er3+

/Yb3+

melalui penggantian komponen pengkelasan dengan

dopan oksida nadir bumi Er2O3/Yb2O3. Kesemua komponen oksida adalah

berketulinan melebihi 99.9% dan prosedur pengkelasan secara kuantitatif yang

dilakukan adalah berasaskan pengiraan formulasi mol%. Teknik sepuh lindap piawai

pada 1000 oC selama sejam dan diikuti penempaan pada 250

oC telah dilakukan ke

atas semua kelas kaca. Pencirian fizikal sampel-sampel kaca meliputi belauan sinar-

X (XRD), analisis terma, ketumpatan, isipadu molar dan indeks biasan manakala

sifat optik diperolehi melalui spektroskopi Transformasi Fourier Infra Merah,

spektroskopi penyerapan Ultra Lembayung-Sinar Nampak-Infra Merah Dekat,

spektroskopi Raman dan spektra floresen sinaran nampak perubahan-atas dan sinaran

infra merah dekat melalui pengujaan diode laser (LD) 980 nm. Kesemua pengukuran

dilakukan pada suhu bilik.

Ketiadaan puncak keamatan yang jelas dengan belauan ‘halo’ yang lebar

spectrogram XRD mengesahkan sifat amorfus hos kaca pilihan. Ketumpatan kaca

didapati tinggi dengan kehadiran komponen berat seperti PbO dan Bi2O3 untuk

kedua-dua kaca TTB dan TPB di mana n yang tinggi diperolehi untuk kedua-duanya.

Kesemua hos kaca TZT3, TTB3, TPB3, TZPTiN10 dan TZPTiN20 mencatatkan

yang tinggi iaitu n > 2. Analisis FTIR memperlihatkan penggalan ketelusan infra

merah melebihi 6 m dengan penyerapan air (OH-) yang ketara di antara 2000-3500

cm-1

di dalam kebanyakan sampel kaca yang dikaji. Analisis penyerapan optik

sempadanan di dalam kebanyakan sampel menunjukkan pembentukan sejumlah

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oksigen yang tidak-berkait yang saling bersandar dengan perubahan jurang tenaga

optic hitungan. Ini dengan jelasnya disokong oleh nilai parameter keamatan

t(t=2,4,6) yang diperolehi melalui analisis Judd-Ofelt. Pengurangan nilai 2 dan

6 adalah sangat berkait dengan peningkatan sifat simetri pada sekitaran Er3+

dengan

pembentukan ketumpatan electron yang tinggi pada ligan ion oksigen; atas kerana itu

sifat kovalen yang kuat Er-O terbentuk dengan peningkatan kepekatan pengedopan

Er3+

. Tambahan lagi faktor ini telah menyumbangkan perubahan struktur TeO2

melalui transformasi struktur [TeO4] piramid tiga-penjuru kepada [TeO3] piramid

dua-penjuru disamping perantaraan unit-unit polihedral [TeO3+1] yang dapat

ditentusahkan oleh analisis spektroskopi Raman yang turut mencatatkan tenaga

getaran maksimum fonon di antara 730-750 cm-1

lebih rendah sedikit berbanding

nilai rujukan TeO2 pada 780 cm-1

. Spektra floresen sinaran nampak perubahan-atas

dengan jelasnya memperlihatkan kedua-dua sinaran hijau dan merah setelah

pengujaan LD 980 nm terutamanya bagi kaca-kaca Er3+

-TZT dan Er3+

/Yb3+

-TZPTiN

yang dicirikan oleh proses penyerapan dua atau/dan tiga foton. Sinar infra merah 1.5

m berkeamatan tinggi dengan lebar melebihi 70 nm dan lebar-jalur pengganda

berjulat (500-1300) x 10-28

cm3 diperolehi di dalam kebanyakan sampel-sampel kaca

terdop Er3+

/Yb3+

. Ciri-ciri ini mencadangkan kaca telurit kepelbagaian komposisi

yang dihasilkan berpotensi sebagai bahan optik untuk teknologi komunikasi jalur-

lebar di masa hadapan.

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ACKNOWLEDGEMENTS

Bismillahirrahmanirrahim, In the name of Allah, the Most Beneficent, the Most

Merciful. Alhamdulillah, all the praises and thanks be to ALLAH the Almighty. All

blessing to Prophet Muhammad, Allah blessing be upon him.

First and foremost, I would like to express my gratitude to Professor Dr. Mohd Adzir

bin Mahdi , for his continuous guidance and advice directing me in this research. I

extended my appreciation also to both members of the supervisory committee, Dr

Ahmad Shukri bin Muhammad Noor and Dr Halimah binti Mohamed Kamari. My

gratitude also goes to the Universiti Putra Malaysia and Kementerian Pengajian

Tinggi Malaysia for providing the opportunity and allowing me to pursue my PhD

degree.

My thanks also goes to Low Dimensional Materials Research Center of Jabatan Fizik

Universiti Malaya Kuala Lumpur for the use of UVvis-NIR Spectrophotometer,

FTIR Spectrophotometer and X-ray diffractometer and NANO-SciTech Centre

UiTM Shah Alam Selangor for the use of microRaman-PL instruments. Also my

special thanks to Mr Azham (Ornets Sdn Bhd) and Ms Tan Loo Sing, Mr Kan Chee

Siong (Aseptec Sdn Bhd) for their kindly assistance in fluorescent measurements.

Not to forget as well to all my friends in Photonic and Fiber Optics System

Laboratory, Engineering Faculty, Universiti Putra Malaysia. Last and not least,

millions of loves and appreciations are bound for my parents and family, which I

dedicated this dissertation for the understanding and support.

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Members of the Examination Committee were as follows:

Date: 2 August 2013

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

accepted as fulfilment of the requirement for the degree of Doctor of Philosophy.

The members of the Supervisory Committee were as follows:

Mohd Adzir bin Mahdi, PhD

Professor

Faculty of Engineering

Universiti Putra Malaysia

(Chairman)

Ahmad Shukri bin Muhammad Noor, PhD

Senior Lecturer

Faculty of Engineering


(Member)

Halimah binti Mohamed Kamari, PhD

Senior Lecturer

Faculty of Science


(Member)

_________________________________

BUJANG BIN KIM HUAT, PhD

Professor and Dean

School of Graduate Studies


Date:

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DECLARATION

I hereby declare that the thesis is based on my original work except for quotations

and citations, which have been duly acknowledged. I also declare that it has not been

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

Malaysia or at any other institution.

____________________________


Date: 14 JUNE 2013

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TABLE OF CONTENTS

Page

ABSTRACT ii

ABSTRAK v

ACKOWLEDGEMENTS viii

APPROVAL ix

DECLARATION xi

LIST OF TABLES xii

LIST OF FIGURES xix

LIST OF ABBREVIATIONS xxx

CHAPTER

1 INTRODUCTION 1

1.1 Rare Earth Doped Tellurite Oxide Glasses 1

1.2 Problem Statement 2

1.3 Objectives 3

1.4 Thesis Outlines 4

2 LITERATURE REVIEW 7

2.1 Glass Forming Characteristics 7

2.1.1 Glass Definition 8

2.1.2 Glass Transformation Behaviour 9

2.2 Theories of Glass Formation 10

2.2.1 Structural Models 11

2.2.1.1 Goldschmidt’s- Ionic Radius Ratio 11

2.2.1.2 Zachariasen’s –The Random Network Model 12

2.2.1.3 Energetic based Models 14

2.2.2 Kinetic Models 18

2.3 Tellurite Glasses Overview 20

2.3.1 Structural and Physical Characteristics 20

2.3.2 Thermal Properties 26

2.3.3 Optical Properties 29

3 THEORY 32

3.1 Spectroscopy of rare earth ions 32

3.3.1 Energy level transitions 32

3.3.2 Electronic structure 36

3.3.3 The Crystal Field effect 38

3.2 Intensity Calculation: The Judd-Ofelt Theory 41

3.3.1 The Judd-Ofelt parameters 41

3.3.2 Transition Probabilities 44

3.3 Nonradiative transitions in rare earth ions 48

3.4 Energy transfer and ions interaction 50

3.4.1 Cross relaxation 51

3.4.2 Excited state absorption 52

3.4.3 Sensitization 53

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3.4.4 Concentration quenching effect 54

3.5 Upconversion 56

4 SAMPLE PREPARATION AND CHARACTERIZATION 58

4.1 Preparation of Glass Samples 58

4.1.1 Glass Composition 58

4.1.2 Glass Batching 61

4.1.3 Melting and Glass Formation 65

4.2 Structural Measurement 67

4.2.1 X-ray diffraction (XRD) 68

4.2.2 Thermal Profiling 68

4.2.3 Density and Molar Volume 70

4.3 Refractive Index Measurement 72

4.3.1 Method and instrumentation 73

4.3.2 Imaging Analysis 76

4.4 Optical Measurement 77

4.4.1 FTIR spectroscopy 78

4.4.2 Raman Spectroscopy 80

4.4.3 Uv-Vis-NIR Absorption 82

4.4.4 Upconversion Spectra 83

4.4.5 Near infra-red (NIR) Emission 85

5 EXPERIMENTAL RESULTS AND ANALYSIS 86

5.1 Structure Properties 86

5.1.1 X-Ray Diffraction (XRD) 91

5.1.2 Thermal Stability 93

5.1.3 Density and Molar Volume 101

5.2 Refractive Index Analysis 114

5.3 Hydroxyl Band Analysis 129

5.4 Raman Spectra Analysis 164

5.5 Optical Energy Gap and Tail Width Analysis 182

5.6 Judd-Ofelt Analysis 205

5.7 Upconversion Analysis 226

5.8 Near infra-red and Emission Cross Section Analysis 240

6 DISCUSSION

6.1 Judd-Ofelt Parameters: Er3+

Nature in Tellurite Glass Structure 257

6.2 Optical Transition Mechanism in Er3+

-doped Tellurite Glasses 266

6.3 1.5 m Emission of Er3+

-doped Tellurite Glasses 279

7 CONCLUSION AND SUGGESTIONS 296

REFERENCES 301

APPENDICES 310

BIODATA OF STUDENT 331

PUBLICATIONS 332

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LIST OF TABLES

Table Page

2.2.1 Classification of Cations as Network Formers, Network Modifiers,

and Intermediates

13

2.2.2 Pauling Electronegativities 15

2.2.3 Bond strength for selected oxides 16

2.3.1 Range (mol%) of glass formation in tellurite glass system 23

2.3.2 Types of coordination of TeO2 in crystalline and glass forms 24

2.3.3 Physical properties among potential glasses 25

2.3.4 Some of related physical properties for selected glass composition 26

2.3.5 The effects of RE dopants on Tg ,Tx and (Tx-Tg) on

[TeO2-ZnO- Na2O] glasses

28

2.3.6 Some of related optical properties for selected glass composition 29

2.3.7 Basic properties for EDTFA and EDSFA 31

3.1.1 The number of 4f electrons (n) in most common trivalent

lanthanides ions

33

4.1.1 (a) Ternary A-TZT (TeO2-ZnO-TiO2) glass compositions 59

(b) Ternary B-TTB (TeO2-TiO2-Bi2O3) glass compositions 59

(c) Ternary C-TPB (TeO2-PbO-Bi2O3) glass compositions 60

4.1.2 Multicomponent-TZPTiN (TeO2-ZnO-PbO-TiO2-Na2O) glass

compositions

60

4.1.3 Glass components and chemicals used to batch glasses, molecular

weight (MW), purity and sources

62

4.1.4 Batching calculation using Excel program 62

4.3.1 Reference table of tabulated d’ values for any possible range of

thicknesses versus the refractive indices

77

5.1.1 Summary of the thermal analysis parameters Tg, Tx, Tc, Tm and

glass stability

100

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5.1.2 Density and Molar Volume of Ternary A-TZT (TeO2-ZnO-TiO2)

glasses

103

5.1.3 Density and Molar Volume of Ternary B-TTB (TeO2-TiO2-Bi2O3)

glasses

106

5.1.4 Density and Molar Volume of Ternary C-TPB (TeO2-PbO-Bi2O3)

glasses

109

5.1.5 Density and Molar Volume of Multicompositions-TZPTiN (TeO2-

ZnO-PbO-TiO2-Na2O) glasses

112

5.2.1 Summarizes of the refractive indices analysis for the host glasses 128

5.3.1 Percentage of OH groups in glass series

(75-x)TeO2-20ZnO-5TiO2-xEr2O3 mol. %

(where x = 0, 0.2, 0.5, 1.0 and 1.5)

135

5.3.2 Er3+

contents, thickness, the free-OH absorption coefficients at

maximum peaks and the free-OH concentrations of (75-x)TeO2-

20ZnO-5TiO2-xEr2O3 mol. % glass series (where x = 0, 0.2, 0.5,

1.0 and 1.5)

137


85TeO2-10TiO2-(5-x)Bi2O3-xEr2O3 mol. %

(where x = 0, 0.2, 0.5, 1.0 and 1.5)

142

5.3.4 Er3+


maximum peaks and the free-OH concentrations of 85TeO2-

10TiO2-(5-x)Bi2O3-xEr2O3 mol. % glass series

(where x = 0, 0.2, 0.5, 1.0 and 1.5)

143


60TeO2-35PbO-(5-x)Bi2O3-xEr2O3 mol. %

(where x = 0, 0.5, 1.0 and 1.5)

148

5.3.6 Er3+



35PbO-(5-x)Bi2O3-xEr2O3 mol. % glass series

(where x = 0, 0.2, 0.5, 1.0 and 1.5)

149


60TeO2-20ZnO-(3-x)PbO-5TiO2-5Na2O-xEr2O3-2Yb2O3 mol. %

(where x = 0.1, 1, 2 and 2.5)

154

5.3.8 Er3+



20ZnO-(3-x)PbO-5TiO2-10Na2O-xEr2O3-2Yb2O3 mol. % glass

series (where x = 0, 0.1, 1, 1and 2.5)

156

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5.3.9

Percentage of OH groups in glass series

60TeO2-20ZnO-(8-x)PbO-5TiO2-5Na2O-xEr2O3-2Yb2O3 mol. %

(where x = 0.1, 1, 2 and 2.5)

161

5.3.10 Er3+



20ZnO-(8-x)PbO-5TiO2-5Na2O-xEr2O3-2Yb2O3 mol. % glass

series (where x = 0, 0.5, 1.0, 2 and 2.5)

163

5.4.1 Summary of the Raman band assignments investigated by

different workers on TeO2 glass systems

166

5.4.2 Peak position, width (FWHM) and integrated area

of the assigned Raman Gaussian bands for TTB3 host glass

168


of the assigned Raman Gaussian bands for TTB22 glass

169


of the assigned Raman Gaussian bands for TTB24 glass

170

5.4.5 Summary of the percentage area of the assigned Raman Gaussian

bands for the TTB glasses.

171


of the assigned Raman Gaussian bands for TPB3 host glass

172


of the assigned Raman Gaussian bands for TPB22 glass

173


of the assigned Raman Gaussian bands for TPB24 glass

174

5.4.9 Summary of the percentage area of the assigned Raman Gaussian

bands for the TPB glasses.

175


of the assigned Raman Gaussian bands for TZPTiN10 host glass

177


of the assigned Raman Gaussian bands for TZPTiN11 glass

178



179



180

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181

5.4.15 Summary of the percentage area of the assigned

Raman Gaussian bands for the TZPTiN1 glasses.

182

5.5.1 Optical energy gap Eopt and Urbach energy EU for TZT glass series

((75-x)TeO2-20ZnO-5TiO2-xEr2O3 mol. %, x = 0, 0.2, 0.5, 1.0 and

1.5)

187

5.5.2 Optical energy gap Eopt and Urbach energy EU for TTB glass

series (85TeO2-10TiO2-(5-x)Bi2O3-xEr2O3 mol. % glass series

(where x = 0, 0.2, 0.5, 1.0 and 1.5)

191

5.5.3 Optical energy gap Eopt and Urbach energy EU for TPB glass series

(60TeO2-35PbO-(5-x)Bi2O3-xEr2O3mol. % ,x = 0, 0.5, 1.0 and 1.5)

195

5.5.4 Optical energy gap Eopt and Urbach energy EU for TZPTiN1 glass

series (60TeO2-20ZnO-(3-x)PbO-5TiO2-10Na2O-xEr2O3-2Yb2O3

mol. %, x = 0.1, 0.5, 1, 2 and 2.5)

199

5.5.5 Optical energy gap Eopt and Urbach energy EU

for TZPTiN2 glass series (60TeO2-20ZnO-(8-x)PbO-5TiO2-

5Na2O-xEr2O3-2Yb2O3 mol. %, x = 0, 0.5, 1.0, 2 and 2.5)

203

5.6.1 Density () and Er3+

concentration (N) for Er3+

doped TZT glasses 208

5.6.2 Tables of selected manifold integrated areas, dipole line strengths

S and calculated JO intensity parameters t=(t=2,4,6) value for

TZT21 glass

209

5.6.3 Table of selected manifold integrated areas, dipole line strengths S

and calculated JO intensity parameters t=(t=2,4,6) value for

TZT22 glass

209



TZT23 glass

210



TZT25 glass

210

5.6.6 Summary of the calculated JO intensity parameters t=(t=2,4,6)

value for Er3+

doped TZT glasses

211



doped TTB glasses 211

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TTB21 glass

212



TTB22 glass

213



TTB23 glass

213



TTB24 glass

214


value for Er3+

doped TTB glasses

214



doped TPB glasses 215



TPB22 glass

216



TPB23 glass

216



TPB24 glass

217


value for Er3+

doped TPB glasses

217



doped

TZPTiN1 glasses

218



TZPTiN13 glass

219



TZPTiN14 glass

219

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TZPTiN15 glass

220

5.6.22

Summary of the calculated JO intensity parameters t=(t=2,4,6)

value for Er3+

doped TZPTiN1 glasses

220



doped

TZPTiN2 glasses

221



TZPTiN22 glass

222



TZPTiN23 glass

222



TZPTiN24 glass

223



TZPTiN25 glass

223


value for Er3+

doped TZPTiN2 glasses

224

5.6.29 Summary of the calculated JO intensity parameters

of Er3+

ion in different tellurite glass hosts

225

5.7.1 Summary of the total absorption photons in different

Er3+

doped tellurite glasses

239

5.8.1 Summary of the NIR spectroscopic parameters:

peak, Imax , FWHM, peak for selected Er3+


246

5.8.2 Table of ECS parameters (max , ECSmax), Effective

NIR width and gain bandwidth (GBW) for selected Er3+

doped

tellurite glasses

254

5.8.3 Calculated values for ACS and ECS parameters using McCumber

procedure: peak value (p and p), energy spread (E1, E2), net

free energy (ε) and scaling factor (K)

256

6.1.1 List of JO intensity parameters t (t = 2, 4 and 6) in selected

tellurite host glasses for comparison

265

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6.3.1 JO intensity parameters and related NIR emission parameters,

max, FWHM of the selected Er3+

/Yb3+


279

6.3.2

Comparison of the JO intensity parameters and related NIR

emission parameters, max, FWHM for Er3+

/Yb3+

doped tellurite

glasses

284

6.3.3 JO intensity parameters and related NIR emission parameters: Sed,

ARad and Rad values for 4I13/2

4I15/2 transition of Er

3+

in selected tellurite glasses

286

6.3.4 Er3+

/Yb3+

concentration and corresponding NR factor values for

free-OH, ET and CR (labelled as A, B/C/D and E columns

respectively)

290

6.3.5 NIR emission parameters: INIR-max, ARad, m, Rad and QE values

for 4I13/2

4I15/2 transition of Er

3+ in selected tellurite glasses

293

6.3.6 Comparison of the NIR emission parameters: ECS, FWHM

and GBW for Er3+

/Yb3+


295

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LIST OF FIGURES

Figure Page

2.1.1 Structural model molecular arrangement for crystal and glass 8

2.1.2 The glass transformation behaviour 9

2.2.1 Time–temperature-transformation (TTT) curve 20

2.3.1 Structural units in TeO2-ZnO glasses 21

2.3.2 The structural units type and mechanism that involved for M2O

addition

22

2.3.3 The coordination crystal structure of TeO2 24

2.3.4 The typical thermal profile of DSC/TGA 28

2.3.5 The stimulated emission cross section (e) of the 4I13/2-

4I15/2

transition of Er3+

ion in tellurite, fluoride and silica-based glasses

30

3.1.1 Transition mechanisms between two energy levels (a) absorption,

(b) spontaneous emission, and (c) stimulated emission

33

3.1.2 Transition rates between two energy levels at equilibrium 36

3.1-3 The energy levels of some of the trivalent lanthanide ions: Nd3+

,

Er3+

, Yb3+

, Eu3+

, Tb3+

, Sm3+

, Gd3+

, and Pr3+

38

3.2.1 Summary of overall steps for the Judd–Ofelt analysis 47

3.3.1 Non-radiative decay rate as a function of energy gap for glass and

crystal host materials

50

3.4.1 The cross relaxation between two ions 51

3.4.2 Excited state absorption (ESA) mechanism in Er3+

system 52

3.4.3 Direct and indirect excitation involving sensitizer on lanthanide

ions

53

3.4.4 The near infra red emission intensity at 1.5 m as a function of

concentration of Er3+

55

3.5.1 Upconversion mechanisms involves between energy levels and

types: (A) Sequential 2-photon absorption, (B) Energy transfer (ET)

and cross relaxation (CR)

57

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4.1.1 Steps of chemical batching procedures 64

4.1.2 Bench-top high temperature muffle furnace for melting process and

typical temperature profile

66

4.1.3 The mould used in the process of glass quenching 67

4.2.1 The typical glass thermal profile 69

4.2.2 DSC-Mettler Toledo thermal analyzer and aluminium crucibles for

thermal measurements

70

4.2.3 Density measurement via Archimedes’s principle 71

4.3.1 Measurement of glass refractive index (n) through an ‘apparent

depth’ method

74

4.3.2 The refractive index imaging analysis via Image Comparer 3.8

Build 711 (Copyright© 2002-2011 Bolide Software)

75

4.4.1 The configuration of an Fourier Transform InfraRed (FTIR)

Spectrometer by Michelson interferometer basis

80

4.4.2 The microRaman spectroscopy analysis via Horiba Jobin Yvon

micro Raman PL spectrometer

81

4.4.3 Schematic block diagram of the system set-up for the the absorption

spectra spectrophotometers

83

4.4.4 Experimental setup for the upconversion spectra measurements 84

4.4.5 Experimental setup for the near infra red spectra measurements 85

5.1.1 Ternary A-TZT (TeO2-ZnO-TiO2) glass compositions 87

5.1.2 Ternary B-TTB (TeO2-TiO2-Bi2O3) glass compositions 88

5.1.3 Ternary C-TPB (TeO2-PbO-Bi2O3) glass compositions 89

5.1.4 Multicomponent-TZPTiN (TeO2-ZnO-PbO-TiO2-Na2O) glass

compositions

90

5.1.5 XRD traces of TZT3, TTB3, TPB3, TZPTiN10 and TZPTiN20 92

5.1.6 Typical glass thermal profiles in this work 93

5.1.7 Thermal profile for glasses TZT3 (75TeO2–20ZnO-5TiO2 mol%)

and TZT23 (74TeO2–20ZnO-5TiO2-1Er2O3 mol%)

95

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5.1.8 Thermal profile for glasses TTB3 (85TeO2–10TiO2-5Bi2O3 mol%)

and TTB21 (85TeO2–10TiO2-4.8Bi2O3-0.2Er2O3 mol%)

96

5.1.9 Thermal profile for glasses TPB3 (60TeO2–35PbO-5Bi2O3 mol%)

and TPB22 (60TeO2–35PbO-4.5Bi2O3-0.5Er2O3 mol%)

97

5.1.10 Thermal profile for glasses TZPTiN10 (60TeO2–20ZnO2-5PbO-

5TiO2-10Na2O mol%) and TZPTiN12 (60TeO2–20ZnO2-2.5PbO-

5TiO2-10Na2O-0.5Er2O3-2Yb2O3 mol%)

98

5.1.11 Thermal profile for glasses TZPTiN20 (60TeO2–20ZnO2-10PbO-

5TiO2-5Na2O mol%) and TZPTiN22 (74TeO2–20ZnO-5TiO2-

1Er2O3 mol%)

99

5.1.12 Density and molar volume behaviours of TZT glasses as a function

of TiO2 concentration

102

5.1.13 Density and molar volume relationship for TZT3-Er3+

glasses as a

function of Er2O3 concentration

104

5.1.14 Density and molar volume behaviours of TTB glasses as a function

of Bi2O3 concentration

105

5.1.15 Density and molar volume relationship for TTB -Er3+

glasses as a


107

5.1.16 Density and molar volume behaviours of TPB glasses as a function

of Bi2O3 concentration

108

5.1.17 Density and molar volume relationship for TPB -Er3+

glasses as a


110

5.1.18 Density and molar volume relationships for multicomposition

TZPTiN1 glasses as a function of Er2O3 concentration

111

5.1.19 Density and molar volume relationships for TZPTiN2 glasses as a


113

5.2.1

(a)

(b)

The cumulative number of best image pairing (CNB Image Pairing)

at respective travelling microscope (TM) vernier positions for

Corning glass

Captured images comparison for Corning glass

115

116

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5.2.2

(a)

(b)



TZT3 host glass

Captured images comparison for TZT3 host glass

117

118

5.2.3

(a)

(b)



TTB3 host glass

Captured images comparison for TTB3 host glass

119

120

5.2.4

(a)

(b)



TPB3 host glass

Captured images comparison for TPB3 host glass

121

122

5.2.5

(a)

(b)



TZPTiN10 host glass

Captured images comparison for TZPTiN10 host glass

123

124

5.2.6

(a)

(b)



TZPTiN20 host glass

Captured images comparison for TZPTiN20 host glass

125

126

5.3.1 Infrared transmission spectrum for TZT3 glass 129

5.3.2 Infrared transmission spectra for erbium-doped TZT glasses 130

5.3.3 Infrared absorption spectra for TZT glasses 131

5.3.4 Gaussian deconvolution of OH bands in TZT3 host glass (75TeO2-

20ZnO-5TiO2 mol. %).

132

5.3.5 Gaussian deconvolution of OH bands in TZT21 glass

(74.8TeO2-20ZnO-5TiO2-0.2Er2O3 mol. %).

133


(74.5TeO2-20ZnO-5TiO2-0.5Er2O3 mol. %).

133

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(74 TeO2-20ZnO-5TiO2-1Er2O3 mol. %).

134


(73.5 TeO2-20ZnO-5TiO2-1.5Er2O3 mol. %).

134

5.3.9

OH percentage behaviour in TZT glasses as a function of Er3+

concentration

136

5.3.10 Calculated free-OH content in the TZT glasses with respect to Er3+

doping concentration

137

5.3.11 Infrared transmission and absorption spectra for TTB glasses 139

5.3.12 Gaussian deconvolution of OH bands in TTB3 glass

(85TeO2-10TiO2-5Bi2O3 mol. %)

140


(85TeO2-10TiO2-4.8Bi2O3-0.2Er2O3 mol. %)

140



141


(85TeO2-10TiO2-4Bi2O3-1Er2O3 mol. %)

141



142

5.3.17 OH percentage behaviour in TTB glasses as a function of Er3+

concentration

143

5.3.18 Calculated free-OH content in the TTB glasses with respect to Er3+


144

5.3.19 Infrared transmission and absorption spectra for TPB glasses 145

5.3.20 Gaussian deconvolution of OH bands in TPB3 host glass

(60TeO2-35PbO-5Bi2O3 mol. %)

146

5.3.21 Gaussian deconvolution of OH bands in TPB22 glass

(60TeO2-35PbO-4.5Bi2O3-0.5Er2O3mol. %)

146


(60TeO2-35PbO-4Bi2O3-1Er2O3mol. %)

147


(60TeO2-35PbO-3.5Bi2O3-1.5Er2O3mol. %)

147

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5.3.24 OH percentage behaviour in TPB glasses as a function

of Er3+

concentration

148

5.3.25 Calculated free-OH content in the TPB glasses with respect to Er3+


149

5.3.26

Infrared transmission and absorption spectra for TZPTiN1 glasses

(TZPTiN10, TZPTiN11, TZPTiN13, TZPTiN14, and TZPTiN15)

151

5.3.27 Gaussian deconvolution of OH bands in TZPTiN10 host glass

(60TeO2-20ZnO-5PbO-5TiO2-10Na2O mol. %)

152

5.3.28 Gaussian deconvolution of OH bands in TZPTiN11 glass

(60TeO2-20ZnO-2.9PbO-5TiO2-10Na2O-0.1Er2O3-2Yb2O3 mol.

%)

152


(60TeO2-20ZnO-2PbO-5TiO2-10Na2O-1Er2O3-2Yb2O3 mol. %)

153



153


(60TeO220ZnO-0.5PbO-5TiO2-10Na2O-2.5Er2O3-2Yb2O3 mol. %)

154

5.3.32 OH percentage behaviour in TZPTiN1 glasses as a function of Er3+

concentration

155

5.3.33 Calculated free-OH content in the TZPTiN1 glasses with respect to

Er3+


156

5.3.34 Infrared transmission and absorption spectra for TZPTiN2 glasses

(TZPTiN20, TZPTiN22, TZPTiN23, TZPTiN24, and TZPTiN25)

158

5.3.35 Gaussian deconvolution of OH bands in TZPTiN20 host glass

(60TeO2-20ZnO-10PbO-5TiO2-5Na2O mol. %)

159

5.3.36 Gaussian deconvolution of OH bands in TZPTiN22 glass (60TeO2-

20ZnO-7.5PbO-5TiO2-5Na2O-0.5Er2O3-2Yb2O3 mol. %)

159


20ZnO-7PbO-5TiO2-5Na2O-1Er2O3-2Yb2O3 mol. %)

160


(60TeO220ZnO-6PbO-5TiO2-5Na2O-2Er2O3-2Yb2O3 mol. %)

160


20ZnO-5.5PbO-5TiO2-5Na2O-2.5Er2O3-2Yb2O3 mol. %)

161

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5.3.40 OH percentage behaviour in TZPTiN2 glasses as a function of

Er3+

concentration

162

5.3.41 Calculated free-OH content in the TZPTiN2 glasses with respect to

Er3+


163

5.4.1 Typical Raman spectra for TeO2 glass system 165

5.4.2 Gaussian deconvolution of Raman spectra for

TTB3 host glass (85TeO2-10TiO2-5Bi2O3 mol. %)

168


TTB22 glass (85TeO2-10TiO2-4.5Bi2O3-0.5Er2O3 mol. %)

169


TTB24 glass (85TeO2-10TiO2-3.5Bi2O3-1.5Er2O3 mol. %)

170


TPB3 host glass (60TeO2-35PbO-5Bi2O3 mol. %)

172


TPB22 glass (60TeO2-35PbO-4.5Bi2O3-0.5Er2O3mol. %)

173


TPB24 glass (60TeO2-35PbO-3.5Bi2O3-1.5Er2O3mol. %)

174

5.4.8 Gaussian deconvolution of Raman spectra for TZPTiN10 host

glass (60TeO2-20ZnO-5PbO-5TiO2-10Na2O mol. %)

177

5.4.9 Gaussian deconvolution of Raman spectra for TZPTiN11 glass


%)

178



%)

179



180



181

5.5.1 Tauc’s plot of (h)1/2

vs. hfor TZT3 host glass 185


vs. hfor Er3+

doped glasses:

TZT21, TZT22, TZT23 and TZT24

185

5.5.3 Plot of ln() vs. hfor TZT3 host glass 186

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5.5.4 Plot of ln() vs. h for Er3+

doped glasses:

TZT21, TZT22, TZT23 and TZT24

186

5.5.5 Eopt variation with respect to Er3+

content for TZT glasses 188


vs. hfor TTB3 host glass 189


vs. hfor Er3+

doped glasses:

TTB21, TTB22, TTB23 and TTB24

189

5.5.8 Plot of ln() vs. hfor TTB3 host glass 190


doped glasses:

TTB21, TTB22, TTB23 and TTB24

190


content for TTB glasses 192


vs. hfor TPB3 host glass 193

5.5.12 Figure 5.5-12. Tauc’s plot of (h)1/2

vs. hfor Er3+

doped glasses:

TPB22, TPB23 and TPB24

193

5.5.13 Plot of ln() vs. hfor TPB3 host glass 194


doped glasses:

TPB22, TPB23 and TPB24

194


content for TPB glasses 196


vs. hfor TZPTiN10 host glass 197


vs. hfor Er3+

doped glasses: TZPTiN11,

TZPTiN12, TZPTiN13, TZPTiN14, and TZPTiN15

197

5.5.18 Plot of ln() vs. hfor TZPTiN10 host glass 198


doped glasses:

TZPTiN11, TZPTiN12, TZPTiN13, TZPTiN14, and TZPTiN15

198


content for TZPTiN1 glasses 200


vs. hfor TZPTiN20 host glass 201


vs. hfor Er3+

doped glasses:

TZPTiN22, TZPTiN23, TZPTiN24and TZPTiN25

201

5.5.23 Plot of ln() vs. hfor TZPTiN20 host glass 202

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doped glasses:

TZPTiN22, TZPTiN23, TZPTiN24and TZPTiN25

202


content for TZPTiN2 glasses 204

5.6.1 Typical absorption spectra of the Er3+

doped glass in the visible and

near-infrared region

206

5.6.2 Typical Gaussian fitting for measuring the integrated area

of the Er3+

absorption bands

207

5.6.3 The UV-VIS-NIR absorption spectra for Er3+

doped TZT glasses

208


doped TTB glasses 212


doped TPB glasses 215


doped TZPTiN1

glasses

218


doped TZPTiN2

glasses

221

5.7.1 Upconversion spectra for TZT21 glass 227

5.7.2 Log-log plot of power dependence analysis for TZT21 glass 228

5.7.3 Normalized upconversion spectra of TZT glasses

in different concentration of Er3+

229

5.7.4 Upconversion spectra for TTB22 glass 230

5.7.5 Log-log plot of power dependence analysis for TTB22 glass 230

5.7.6 Normalized upconversion spectra of TZT glasses in different


231

5.7.7 Upconversion spectra for TPB24 glass 232

5.7.8 Log-log plot of power dependence analysis for TPB24 glass 233

5.7.9 Normalized upconversion spectra of TPB glasses in different


234

5.7.10 Upconversion spectra for TZPTiN15 glass 235

5.7.11 Log-log plot of power dependence analysis for TZPTiN15 glass 235

5.7.12

Normalized upconversion spectra of TZPTiN1 glasses


236

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5.7.13 Upconversion spectra for TZPTiN25 glass 237

5.7.14 Normalized upconversion spectra of TZPTiN25 glasses


238

5.7.15 Normalized upconversion spectra of TZPTiN2 glasses


239

5.8.1 Near infrared (NIR) fluorescence emission for TZT21 glass 240

5.8.2 Near infrared (NIR) fluorescence emission for TZT24 glass 241

5.8.3 Near infrared (NIR) fluorescence emission for TTB21 glass 241

5.8.4 Near infrared (NIR) fluorescence emission for TTB22 glass 242

5.8.5 Near infrared (NIR) fluorescence emission for TPB23 glass 242

5.8.6 Near infrared (NIR) fluorescence emission for TPB24 glass 243

5.8.7 Near infrared (NIR) fluorescence emission for TZPTiN13 glass 243




5.8.11 Absorption and emission cross sections spectra for TZT21 glass 249

5.8.12 Absorption and emission cross sections spectra for TZT24 glass 249

5.8.13 Absorption and emission cross sections spectra for TTB21 glass 250

5.8.14 Absorption and emission cross sections spectra for TTB22 glass 250

5.8.15 Absorption and emission cross sections spectra for TPB23 glass 251

5.8.16 Absorption and emission cross sections spectra for TPB24 glass 251

5.8.17 Absorption and emission cross sections spectra for TZPTiN13 glass 252




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6.1.1 Relationship between the t (t=2, 4, 6) parameters as a function of

Er3+

concentration (NEr3+

) in ternary TZT, TTB and TPB glass

composition

263

6.1.2 Relationship between the t (t=2, 4, 6) parameters as a function of

Er3+

concentration (NEr3+

) in multicomposition TZPTiN1 and

TZPTiN2 glass composition

264

6.2.1 Simplified energy level scheme and optical transition of the Er3+

under 980 nm excitation

266

6.2.2 Schematic optical transition mechanisms for Er3+

-doped TZT

glasses

271


-doped

TTB glasses

273


-doped TPB

glasses

275

6.2.5 Schematic optical transition mechanisms for

multicomposition Er3+

-Yb3+

doped TZPTiN glasses

278

6.3.1 Relationship between 6 and max for the

selected Er3+

/Yb3+

doped tellurite glasses 281

6.3.2 Relationship between 2 and FWHM for the

selected Er3+

/Yb3+

doped tellurite glasses 283

6.3.3 Relationship between intensity parameter 6 parameter, line

strength Sed, and radiative lifetime Rad of Er3+

in selected tellurite

glasses

286

6.3.4 Proposed quenching mechanism between the Er3+

ions and free-OH

group

288

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LIST OF ABBREVIATIONS

CN Coordination number

CNB Cumulative number of best image pairing

CR Cross relaxation

DSC Differential scanning calorimetry

DTA Differential thermal analysis

ECS Emission cross section

ED Electric dipoles

EDSFA Silica based erbium-doped fiber amplifier

EDTFA Tellurite-based erbium-doped fiber amplifier

ESA Excited state absorption

ET Energy transfer

FTIR Fourier Transform Infra Red Spectroscopy

FWHM Emission width /Full width at half maximum

GBW Optical gain bandwidth

GSA Ground state absorption

HMO Heavy metal oxide

HR Hruby’s parameter (or ratio)

IR Infrared

JO Judd-Ofelt

LD Laser diode

MD Magnetic dipole line strength

MRP Multiphonon relaxation process

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MW Molecular weight

NBO Non-bridging oxygen

NIR Near infra red

OD Optical density

RE Rare earth

RNM Random Network Model

TM Travelling microscope

TTT Time–temperature-transformation

UV Ultraviolet

VIS Visible

XRD X-ray diffraction

ε Net free energy required to excite one Er3+

from the 4I15/2 to

4I13/2

Wnr Nonradiative rate

VM Molar volume

Tx Crystallization onset temperature

tp Trigonal pyramid

Tm Melting temperature

Tg Glass transformation/transition temperature

tbp Trigonal bipyramid

Smeas Measured line strength

Sed Electric dipole line strength

Scalc Theoretically/calculated electric dipole line strength

n Refractive index

k(λ) Absorption coefficient

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Imax Maximum intensity

EU Urbach energy

Er3+

erbium ions

Eopt Optical energy gap

AT Spontaneous transition probabilities

t JO intensity parameters

Rad Radiative lifetimes

peak/max Peak wavelength

exp Experimental/Measured lifetime

e Emission cross section

a Absorption cross section

peak Effective width of the emission band

Lifetime

Quantum efficiency

Branching ratios

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CHAPTER 1

INTRODUCTION

1.1 Rare Earth Doped Tellurite Oxide Glasses

Tellurite oxide (TeO2) glasses have been identified an attracted optical glass

materials due to their interesting properties as compared to other glass types. The

glasses have advantages of good combination of physical and thermal stability,

mechanical strength and chemical durability. Among oxide based glasses such as

germinate, phosphate, borate and silicate glasses, TeO2 based glasses posses

comparatively smaller phonon energies [1]. Moreover, they also exhibit low optical

attenuation between 0.4 and 5 μm range, broad infrared transmission (as low from 4

um to 6 um range), high refractive index and excellence rare earth (RE) solubility,

which promoted better radiative transitions mechanism in the RE ions. Erbium ion

(Er3+

) has been identified as an ideal and excellence existing candidate RE ions as it

emits both in visible (upconversion) and infrared by excitation of 800 and 980 nm

laser diodes (LD) [2-3]. Due to the above factors, much efforts has been focused to

exploit them as prospect photonic materials for the applications of optical fiber

amplifiers and upconversion lasers, nonlinear optical devices, optical data storage

and sensors [4-6]. Today with the intensive computer networks development

especially in data transmission services of the wavelength division multiplexing

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(WDM) system has prompted much investigation into extending the bandwidth

which can be addressed by optical amplification [7-9].

1.2 Problem Statement

The searching for novel glass composition for this low phonon oxides is a challenge

for both material and optical glass designer due to the current demand for low loss

broadband and flat gain amplifiers applications. Due to rapid development of

broadband erbium-doped fiber amplifiers (EDFA) in recent years, broader bandwidth

above 50 nm than silica-based EDFA at the 1.5 μm optical telecommunication

window for erbium-doped tellurite oxide glasses are expected could be obtained.

Several proposed oxide glass components such as ZnO, TiO2, Bi2O3, PbO, and WO3

are among potential candidates for this purpose. Thus selection of appropriate

composition is very crucial task since it will affect the physical, chemistry and

optical properties of the glass host. ZnO has been known an excellent glass modifier

which facilitate easy glass formation in parent TeO2 glass matrix [10]. The addition

of TiO2 on the other hand will enhance both linear and nonlinear optical properties

of the glass [11]. Recently Bi2O3, PbO, and WO3 which are also referred as heavy

metal oxides (HMO) form an important class of glass materials for photonic

devices. These oxides would contribute significant structural and optical glass

properties since they comprise of heavy, low field strength and high polarizability

behaviour [12]. In this study differentxxcompositions of ternary and

multicomposition tellurite based glasses were fabricated. It is to note that in the

realization of the desired end glass host properties, selection of the right glass

formulation or batching procedure and glass fabrication parameter: melting

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temperature, time and surrounding ambient condition (open/closed-circulated gasses

feeding) are seriously taken into consideration. It is to ensure glassy, transparency,

homogeneity and contamination-free of the fabricated glass samples are fulfilled.

1.3 Objectives

The features exhibited by rare-earth ions especially Er3+

-doped tellurite oxide based

glasses as mentioned above have been recognised as factors that triggered the

motivation to exploit the potential of this materials in the area of telecommunication

technology. The main goals of this study are to formulate and fabricate a new

tellurite based multicomponent (ternary and above) glass compositions which posses

better glass stability and optical performance. The roles of each glass constituent in

this complex amorphous structure, expected to provide an interesting physical and

optical characteristic are to be explored.

In order to obtain high performance broad and intense 1.5 m emission due to

transition of 4I13/2

4I15/2 of Er

3+ in tellurite based glasses, nature of the dopant site of

the glass matrix need to be well understood. Both theoretical and experimental

techniques are adopted in this work to explore the fascinating Er3+

behaviour in the

amorphous nature of glass. The theoretical Judd-Ofelt (JO) approach is a

comprehensively spectroscopic analysis attribute to the intensity of RE ions. The

analytical calculation procedure of the intensity parameters which also referred to JO

intensity parameters, t(t=2,4.6) involve tedious multiple equation solving has

allowed for the calculation of manifold to manifold transition probabilities, from

which the radiative lifetimes and branching ratios of emission can be determined

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[13]. In addition the absorption-emission probabilities or cross section relationship

due to 4I13/2

4I15/2 of Er

3+ may also be predicted through the reciprocity relation of

the McCumber theory. Furthermore the optical performance of Er3+

-doped tellurite

based glasses are often compromise with luminescence quenching factors attributed

to nature of the glass host, rare-earth doping concentration and existing hydroxyl

(OH-) groups. All these factors are commonly referred to the contribution from non-

radiative processes which compete with the radiative counterpart and reflected by the

quantum efficiency of studied glass. Finally through the fluorescence spectra

observation an optical transition mechanism could be proposed in explaining the

physical mechanism processes that probably involved in the corresponding glass.

1.4 Thesis Outlines

Chapter 2 of this thesis presents a review on the principle of glass formation which

defines and explains some basic structural and kinetic theories of glass. The model of

glass theories and its formation mechanisms are fundamental elements to understand

glasses behaviour even more better. It then followed by a detail review specifically

on tellurite glasses which describe some of its special physical and optical features

as compared to other glasses.

The rare-earth ions in glasses phenomena and some of its fundamental

characteristics are very important resources in this study especially the role of Er3+

ions in the tellurite glass host are presented in Chapter 3. It begins with the basic rare

earth spectroscopic theory which account for the observed intensity absorption

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spectra of the rare-earth ions in solids. This is followed by the theory of Judd-Ofelt

where the related absorption intensity parameters t(t=2,4.6) are obtained through a

comprehensive numerical calculation procedure. Also included in this chapter some

of the nonradiative factors that may affect glass optical performance. A special topic

on upconversion process is given at the end of the chapter, attribute to anti-Stokes

emission phenomenon which known strongly exhibited in most Er3+

doped glasses.

The glass sample preparation and method of characterizations shall be highlighted in

Chapter 4. The steps of important procedure together with details of preparation

conditions are described here. Beginning with glass sample formulation, then the

batching procedure and glass fabrication are mentioned in lengthy. Both structural

and optical characterization techniques that utilized in the present study are

illustrated in detail. The particulars of the material characterization and

instrumentation are also specified in this chapter.

Chapter 5 presents the experimental data and result analysis of the measurements

described in Chapter 4. Section 5.1 describes the amorphous nature and thermal

properties of glass are investigated. The glass refractive index is determined in

Section 5.2. Details of the analytical techniques involved in the determining of

water (OH-) content and TeO2 structural units ([TeO4] tbp, [TeO3] tp, [TeO3+1]

polyhedral) are presented clearly in section 5.3 and 5.4 respectively. Section 5.5

is describing the optical energy gap (Eopt) behaviour in the present glass and its

variation upon different compositions. This is follows by comprehensive JO

result analysis in Section 5.6 describing the nature of the Er3+

ions inside the glass

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host where related intensity parameters are obtained. The upconversion spectra at

different excitation laser diode (LD) power of wavelength 980 nm are analyzed in

Section 5.7. Finally the near infrared (NIR) 1.5 m emission due to the transition of

4I13/2

4I15/2 of Er

3+ for selected glasses are presented in Section 5.8.

In Chapter 6 the nature of the Er3+

ions vicinity in the glass matrix corresponding to

interaction with surrounding ligands are interpreted in details through the obtained

t(t=2,4,6) values which are strongly related to structural modification of the

constituent glass composition. Details proposed optical transition mechanisms of

Er3+

ions which possibly involved in the present glasses are also elaborated in length

based on both fluorescence upconversion and NIR spectra. Further discussion

specifically focused on the NIR 1.5 m emission due to the transition of 4I13/2

4I15/2

of Er3+

for selected glasses are presented here. The prospect for photonic device

materials and its potential are explored through the obtained t(t=2,4,6) values,

electric dipole line strength (Sed), spontaneous transition probabilities (AT),

absorption and emission cross section (a and e), emission width (FWHM), lifetime

and quantum efficiency ().

Finally, Chapter 7 summarizes the results obtained in the present studies and

explores the possibility of further works in this area of research.

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http://www.sciencedirect.com/science/article/pii/002230939390742G

http://www.sciencedirect.com/science/article/pii/002230939390742G



http://www.ingentaconnect.com/content/sgt/pcg/1999/00000040/00000005/4005257

http://www.ingentaconnect.com/content/sgt/pcg/1999/00000040/00000005/4005257

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