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Studies on the Growth and Characterization of Some Optical Crystals

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Studies on the Growth and Characterization of Some Optical Crystals STUDIES ON THE GROWTH AND CHARACTERIZATION OF SOME OPTICAL CRYSTALS Thesis of the research work submitted to Bharathidasan University, Thiruchirappalli in partial fulfillment of the requirements for the award of the degree of DOCTOR OF PHILOSOPHY IN PHYSICS Submitted by P.PARAMASIVAM Under the Supervision of Dr. C. RAMACHANDRA RAJA, Ph.D., Associate Professor in Physics POSTGRADUATE & RESEARCH DEPARTMENT OF PHYSICS GOVERNMENT ARTS COLLEGE (AUTONOMOUS) KUMBAKONAM - 612001 TAMIL NADU, INDIA FEBRUARY – 2012 Dr. C. Ramachandra Raja, Ph.D., Associate Professor in Physics, Department of Physics, Government Arts College (Autonomous), Phone : +91 4364221751 Kumbakonam – 612001, CelL: +91 9976696277 Tamil Nadu, India. Email: [email protected] CERTIFICATE This is to certify that the thesis entitled “STUDIES ON THE GROWTH AND CHARACTERIZATION OF SOME OPTICAL CRYSTALS” submitted by Mr. P.PARAMASIVAM is a bonafide record of the research work done by him during the period of study from 2004 to 2011 under my supervision in the Department of Physics, Government Arts College (Autonomous), Kumbakonam and that the thesis has not previously formed the basis for the award of any Degree, Diploma, Associateship, Fellowship or any other similar title. This thesis represents an independent work on the part of candidate. Kumbakonam C. Ramachandra Raja (Research Supervisor) Mr. P.Paramasivam, Research Scholar (Part - Time), Department of Physics, Government Arts College (Autonomous), Kumbakonam – 612001, Tamil Nadu, India. DECLARATION I hereby declare that the work presented in this thesis entitled “STUDIES ON THE GROWTH AND CHARACTERISATION OF SOME OPTICAL CRYSTALS” has been originally carried out by me under the guidance and supervision of Dr.C.Ramachandra Raja, Associate Professor, Department of Physics, Government Arts College (Autonomous), Kumbakonam. This work has not been submitted either in whole or in part for any other Degree or Diploma at any Universities or Research Institutes. Kumbakonam P.Paramasivam ACKNOWLEDGEMENT The author deeply expresses his wholehearted gratitude to his respectful guide and supervisor Dr. C. RAMACHANDRA RAJA, Associate Professor, Department of Physics, Government Arts College (Autonomous), Kumbakonam, India for his effective guidance, continuous encouragement, and who has had a profound influence to complete the research and thesis work. This thesis shall always bear testimony to my respect and gratitude towards my mentor. The author expresses his sincere gratitude to Dr.J.Govindhadas, Principal, Government Arts College, Kumbakonam, India and extends his profound thanks to Dr.K.C.Srinivasan, Head of the Department of Physics, Government Arts College, Kumbakonam, India for providing this opportunity. The author is deeply thankful to Dr.R.Jayavel, Director, Department of Nano Technology, Anna University, Chennai, India, Dr.R.Mohan Kumar, Professor, Presidency College, Chennai, India, Dr.N.Vijayan, Scientist, NPL, New Delhi, India, Dr.V.Manivannan, Addl. Director (CRD), PRIST University, Thanjavur, Prof.R.S.Sundararajan, Department of Physics, Govt. Arts College, Kumbakonam, India, Mr.B.Vijayabhaskaran, Assistant Professor of Physics, Anjalai Ammal- Mahalingam Engineering College, Kovilvenni, Tiruvarur, India and Dr.A.Antony Joseph, Assistant Professor of Physics, Annai Enggineering college, Kumbakonam, India for their valuable suggestions, fruitful discussions and immense help at various phases of the research. iv The author records his immense gratitude to Dr.P.K.Das, Professor, IPC, IISc, Bangalore, India for providing the opportunity to do the NLO study. The author also gratefully acknowledges the valuable help extended by the authorities of SAIF, IIT, Chennai, India, ICP, CECRI, Karaikudi, India and ACIC, St. Joseph’s College, Tiruchirappalli, India to carryout the desired studies. The author expresses his deep sense of gratitude to Dr.M.Arivazhagan, Assistant Professor of Physics, A.A. Government Arts College, Musiri, India, Dr.I.Vethapothakar, Assistant Professor of Physics, Anna University of Technology, Thiruchirappalli, Mr.M.Chitravel, Assistant Professor of Chemistry, T.R.P. Engg. College, Thiruchirappalli, India, Ms.D.Trixy Nimmy Priscilla, Lecturer, Department of Physics, Anjalai Ammal-Mahalingam Engineering College, Kovilvenni, Tiruvarur, India for their consistent support throughout this work. The author is also thankful to Prof. M.Arulanandasamy Department of English, Anjalai Ammal-Mahalingam Engineering College, Kovilvenni, Tiruvarur and Dr.P.Arangamsamy, Head of the Department of English, periyar Maniammai University, Thanjavur for their careful revision and proof- reading of the text at every stage of its preparation. The author extends his sincere thanks to all the teaching and non teaching staff members of the Department of Physics, Government Arts College, Kumbakonam for their continued support. v Lastly, and most importantly, the author wants to thank his parents, wife and sons without whom this work could not have been accomplished successfully. Their support, even at the cost of their personal comfort and needs, is worth the whole world. The author also thanks his entire extended family and friends for having provided a loving environment for him during the whole course of his research work. The Author vi TABLE OF CONTENTS Chapter No Title Page No Preface xii List of Publications xvi Conferences / Seminars xvii List of Tables xviii List of Figures xix List of Symbols xxi List of Abbreviations xxii 1 INTRODUCTION TO CRYSTAL GROWTH – AN OVERVIEW 1.1 INTRODUCTION 1 1.2. NUCLEATION 3 1.2.1. Kinds of Nucleation 4 1.2.2. Classical Theory of Nucleation 5 1.2.3. Kinetic Theory of Nucleation 5 1.3. STABILITY OF NUCLEUS 6 1.4. ENERGY FORMATION OF SPHERICAL 7 NUCLEUS 1.5. SUPERSATURATION AND ITS EXPRESSION 10 1.6. CLASSIFICATION OF CRYSTAL GROWTH 11 1.6.1. Growth from Melt 12 1.6.2. Growth from Vapour 15 1.6.3. Growth from Solution 17 1.7. GEL GROWTH 18 vii Chapter No Title Page No 1.8. HYDROTHERMAL GROWTH 19 1.9. FLUX GROWTH 19 1.10. LOW TEMPERATURE SOLUTION GROWTH 20 1.10.1. Slow Cooling Method 21 1.10.2. Temperature Gradient Method 22 1.10.3. Slow Evaporation Method 22 1.11. CRITERIA FOR OPTIMIZING SOLUTION 23 GROWTH 1.11.1. Material Purification 23 1.11.2. Solvent Selection 24 1.11.3. Solubility 24 1.11.4. Solution Preparation and Crystal Growth 25 1.11.5. Crystal Habit 25 1.12 ADVANTAGES OF LOW TEMPERATURE 26 SOLUTION GROWTH TECHNIQUE 2 AN OVERVIEW OF OPTICAL MATERIALS 2.1. INTRODUCTION 28 2.2 IMPORTANCE OF CRYSTALS AS OPTICAL 30 MATERIALS 2.3 NONLINEAR OPTICAL MATERIALS 31 2.4. THEORETICAL EXPLANATION OF 33 NONLINEAR OPTICS 2.5. VARIOUS TYPES OF NLO EFFECTS 36 2.5.1. Second Harmonic Generation 37 2.5.2. Sum Frequency Generation 38 2.5.3. Difference Frequency Generation 39 viii Chapter No Title Page No 2.5.4. Optical Parametric Generation 39 2.5.5. Linear Electro Optic Effect 40 2.5.6. Optical Rectification 40 2.6. NONLINEAR OPTICAL MATERIALS 40 2.7. DEVELOPMENT OF NLO MATERIALS 41 2.7.1. Organic Crystals 42 2.7.2. Semi-Organic Crystals 44 2.7.3. Inorganic Crystals 45 2.8. SQUARIC ACID, L-PROLINE, GLYCINE AND 46 THIOCYANATE BASED OPTICAL CRYSTALS 2.9. SCOPE OF THE RESEARCH WORK 50 3 CHARACTERIZATION TECHNIQUES 3.1. INTRODUCTION 52 3.2. SINGLE CRYSTAL XRD STUDIES 53 3.2.1. Principle of X-ray diffraction 53 3.2.2. Sample Selection and Preparation 55 3.2.3. Sample Mounting 55 3.2.4. Sample Centering 55 3.3 POWDER X-RAY DIFFRACTION STUDIES 57 3.3.1. X-ray Powder Diffractometer 58 3.4. FT-IR SPECTRAL ANALYSIS 60 3.4.1. Preparation of Liquid Sample 64 3.4.2. Preparation of Solid Sample 64 3.5 NUCLEAR MAGNETIC RESONANCE ANALYSIS 65 ix Chapter No Title Page No 3.5.1 Introduction 65 3.5.2 NMR Spectroscopy - Principle 66 3.5.3 Nuclear spins 66 3.5.4 NMR Spectrometer - Construction 68 3.5.5 NMR Spectrometer - Working 69 3.5.6 Applications of NMR Spectroscopy 69 3.6. UV-Vis-NIR SPECTROSCOPY 70 3.7. THERMAL STUDIES 72 3.7.1. Differential Thermal Analysis 74 3.7.2. Thermogravimetry Analysis 75 3.8. KURTZ POWDER METHOD 77 3.8.1. Introduction 77 3.8.2. Experimental Procedure 77 4 SYNTHESIS, GROWTH AND CHARACTERIZATION OF A NEW NONLINEAR OPTICAL MATERIAL: 4-PHENYLPYRIDINIUM HYDROGEN SQUARATE (4PHS) 4.1. INTRODUCTION 80 4.2. EXPERIMENTAL PROCEDURE 81 4.3. CHARACTERIZATION STUDIES 4.3.1. Single Crystal X-RD Analysis 82 4.3.2. FT-IR Spectral Analysis 83 4.3.3. Nuclear magnetic resonance 86 4.3.4 Optical transmission spectrum analysis 88 4.3.5. Second Harmonic Generation Analysis 89 x Chapter No Title Page No 4.3.6. Thermal Analysis 90 4.4. CONCLUSION 91 5 GROWTH AND CHARACTERIZATION OF A NEW NONLINEAR OPTICAL CRYSTAL: GHS 5.1. INTRODUCTION 93 5.2. EXPERIMENTAL PROCEDURE 94 5.3. CHARACTERIZATION STUDIES 96 5.3.1. Single Crystal X-RD Analysis 97 5.3.2. Powder XRD Analysis 97 5.3.3. FT-IR Spectral Analysis 100 5.3.4. Optical Transmission Spectrum Analysis 101 5.3.5. Nuclear magnetic resonance 102 5.3.6. Second Harmonic Generation Analysis 105 5.3.7 Thermal Analysis 106 5.4. CONCLUSION 107 6 CRYSTALLIZATION AND CHARACTERIZATION OF A NEW NONLINEAR OPTICAL CRYSTAL: LPS 6.1. INTRODUCTION 109 6.2. EXPERIMENTAL PROCEDURE 110 6.3. CHARACTERIZATION STUDIES 111 6.3.1. Single Crystal X-RD Analysis 112 6.3.2. FT-IR Spectral Analysis 112 6.3.3. Optical Transmission Spectrum Analysis 114 6.3.4. Second Harmonic Generation Analysis 115 6.3.5. Thermal Analysis 116 6.4. CONCLUSION 117 xi Chapter No Title Page No 7 GROWTH AND CHARACTERIZATION OF CADMIUM MANGANESE THIOCYANATE (CMTC) CRYSTAL 7.1. INTRODUCTION 119 7.2. EXPERIMENTAL PROCEDURE 120 7.3. CHARACTERIZATION 121 7.3.1. Single Crystal X-RD Analysis 122 7.3.2. FT-IR Spectral Analysis 122 7.3.3.
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