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MINISTRY OF EDUCATION AND TRAINING HANOI UNIVERSITY OF SCIENCE AND TECHNOLOGY LE THI THAO VIEN Synthesis and properties of undoped and transition metal (Mn2+, Cr3+) doped Zn2SiO4 and Zn2SnO4 phosphors DOCTORAL DISSERTATION ON MATERIAL SCIENCES HANOI – 2020 MINISTRY OF EDUCATION AND TRAINING HANOI UNIVERSITY OF SCIENCE AND TECHNOLOGY LE THI THAO VIEN Synthesis and properties of undoped and transition metal (Mn2+, Cr3+) doped Zn2SiO4 and Zn2SnO4 phosphors Majors: Material Sciences Code: 9440122 DOCTORAL DISSERTATION ON MATERIAL SCIENCES ADVISORS: Prof Dr PHAM THANH HUY Dr NGUYEN THI KHOI HANOI – 2020 COPYRIGHT DECLARATION This thesis compresses only my research results It does not contain any previous data submitted by any people or organizations except that have been marked in the references Hanoi, 15/9/2020 Advisors PhD Student Prof Dr Pham Thanh Huy Le Thi Thao Vien i ACKNOWLEDGEMENTS Although my name is on the cover of this dissertation, many people were of great importance to this research I want to take a moment to extend my gratitude to the involved The first, I would like to express my sincerest thanks to my supervisor, Prof Pham Thanh Huy, excellence and estimable teacher, for all of his supports His dedication to science has been encouraging me so much, protected me from the confusion since I started studying and researching at the Advanced Institute for Science Technology (AIST) This dissertation was carried out at AIST, together with several research groups researches I had garnered variable information from these seminars with free discussions coming from all of our group members Possibly just as important as the practical aid was the friendly, cooperative atmosphere at AIST; it made me enjoy virtually every second of working on my dissertation I wish to thank Associate prof Dao Xuan Viet; Dr Nguyen Tu; Dr Nguyen Duy Hung, and all of my teammates for their friendships with kind-hearts and unconditional assistance The last few months weren’t easy, and I want to thank all my dearest friends, who helped me get back on track when I lost my laptop and found many difficulties in life Without your care, understanding, and motivational speeches, this thesis would no doubt look different and not for the better Your friendship makes me realize what a lucky person I am For the last, more than I can say, I would like to express manifest thanks to my husband and two children for always being by my side, putting their truth in me during my duration at AIST Lastly, I want to mention my father, mother, my parents-in-law, and two sisters, and thank them for making me the person that I have become Le Thi Thao Vien ii CONTENTS LIST OF FIGURES viii LIST OF TABLES xiv BRIEF INTRODUCTION Chapter INTRODUCTION 1.1 Background of Luminescence 1.1.1 Luminescence 1.1.2 Optical quenching 1.1.3 Electroluminescence 1.1.4 Thermoluminescence 10 1.2 Background of Transition Metal (TM) ions in the crystal field………10 1.2.1 Transition metals………………………………………………………10 1.2.2 The effect of crystal fields on the separation of TM ions…………… 11 1.2.3 Tanabe-Sugano diagrams 15 1.2.4 Energy levels of Mn 1.2.5 Energy levels of Cr 2+ 3+ ion in a crystal field 18 ion in a crystal field 20 2+ 3+ 1.3 Literature review of transition metal (Mn , Cr ) doped Zn2SiO4 and Zn2SnO4 phosphors 22 2+ 1.3.1 Structure and optical properties of Zn2SiO4: Mn ………………… 22 1.3.2 Structure and optical properties of Zn2SnO4, Zn2SnO4:Mn2+ ………………………………………………………………………………………………………………………… 24 1.4 Phosphor-based LEDs 26 1.4.1 LED 26 1.4.2 Phosphor-based LEDs 27 1.4.3 LED application in agricultural lighting 30 Chapter EXPERIMENTAL TECHNICS 32 2.1 Introduction 32 2+ 2+ 2.2 Synthesis of Zn2SiO4, Zn2SiO4:Mn , Zn2SnO4, Zn2SnO4:Mn , 3+ 3+ 3+ Zn2SnO4:Cr , Zn2SnO4:Cr , Al 33 2.2.1 Materials 33 2.2.2 Synthesis of Zn2SiO4 33 2+ 2.2.3 Synthesis of Zn2SiO4: Mn 34 2.2.4 Synthesis of Zn2SnO4 34 2+ 34 3+ 3+ 3+ Zn2SnO4:Cr and Zn2SnO4:Cr , Al 34 2.2.5 Synthesis of Zn2SnO4:Mn 2.2.6 Synthesis of 2.2.7 Mechanical milling 35 iii 2.3 Techincal methods 35 2.3.1 Structural characterisation 35 2.3.2 Photoluminescent characterization 30 2.4 LED package process 43 2.4.1 Die bonding 44 2.4.2 Wire Bonding 45 2.4.3 Phosphor Dosing 45 2.4.4 Dispensing 46 2.4.5 Curing 47 2.4.6 Testing 47 Chapter STRUCTURE AND OPTICAL PROPERTIES OF Zn2SiO4 AND 2+ Zn2SiO4:Mn PHOSPHORS 48 3.1 Introduction 48 3.2 Structure and optical properties of Zn2SiO4 phosphors 49 3.2.1 X-ray diffraction of Zn2SiO4 49 3.2.2 Phosphor morphology of Zn2SiO4 50 3.2.3 Vibrational analysis: Raman spectra of Zn 2SiO4 51 3.3 Structure and optical properties of Zn2SiO4:Mn 3.3.1 3.3.2 3.3.3 3.3.4 2+ phosphors 55 2+ X-ray diffraction of Zn2SiO4:Mn 55 2+ Phosphor morphology of Zn2SiO4:Mn 57 2+ Vibrational analysis of Zn2SiO4:Mn 58 2+ Optical properties of Zn2SiO4:Mn 61 2+ 3.3.5 Thermoluminescence (TL) properties and Decay time of Mn doped Zn2SiO4 64 2+ 3.3.6 Application of Mn doped Zn2SiO4 on UV LED 66 3.4 Conclusion 67 Chapter STRUCTURE AND OPTICAL PROPERTIES OF Zn2SnO4 AND 2+ Zn2SnO4:Mn PHOSPHORS 68 4.1 Introduction 68 4.2 Structural and optical properties of Zn2SnO4 phosphors 69 4.2.1 X-ray diffraction of Zn2SnO4 69 4.2.2 Optical properties of Zn2SnO4 74 4.3 Structural and optical properties of Zn2SnO4:Mn 2+ 80 2+ Phosphor morphology of Zn2SnO4:Mn 84 2+ Optical properties of Zn2SnO4:Mn 84 4.3.1 X-ray diffraction of Zn2SnO4:Mn 4.3.2 4.3.3 2+ 80 iv 2+ 4.3.4 Decay time of 5%Mn doped Zn2SnO4 89 4.3.5 Temperature-dependent PL and internal quantum efficiency of Zn2SnO4:5%Mn 2+ phosphors 91 2+ 4.3.6 Application of un-doped and Mn doped Zn2SnO4 on LED 92 4.4 Conclusion 93 3+ 3+ 3+ Chapter OPTICAL PROPERTIES OF Zn2SnO4:Cr AND Zn2SnO4:Cr , Al FOR PLANT CULTIVATION LED 95 5.1 Introduction 95 5.2 Structural and optical properties of Zn2SnO4:Cr 5.2.1 3+ phosphors 97 3+ X-ray diffraction of Zn2SnO4:Cr 97 3+ Phosphor morphology of Zn2SnO4:Cr 100 3+ Optical properties of Zn2SnO4:Cr 101 5.2.2 5.2.3 5.2.4 Application of the prepared phosphor for fabricating infrared LEDs 105 3+ 5.3 Structural and optical properties of Zn2SnO4:Cr , Al 3+ 3+ phosphors 106 3+ ,Al 106 5.3.1 X-ray diffraction and FESEM of Zn2SnO4:Cr 5.3.2 Crystal field analysis 109 3+ 3+ 5.3.3 The effect of Al on optical properties of ZTO: Cr 111 5.3.4 Application of the prepared phosphor 116 5.4 Conclusion 117 CONCLUSIONS AND FUTURE WORKS 120 PUBLICATIONS 123 RELATED PUBLICATIONS 124 REFERENCES 125 v LIST OF ACRONYMS Acronyms Full name EDX/EDS: Energy-Dispersive X-ray spectroscopy LED: Light Emitting Diode NIR: Near-infrared PL: Photoluminescence SEM: Scanning Electron Microscope XRD: X-Ray Diffraction FESEM: Field emission scanning electron Microscope PLE: Photoluminescence excitation UV: Ultraviolet HWHM: Half-Width at half-maximum IR: Infra-red TM: Transition Metal EL: Electroluminescence NBOH: Non – bridging oxygen hole centers RGB: Red, Green and Blue FTIR: Fourier – transform infrared spectroscopy HEBM: High – energy planetary ball mill AIST: Advanced 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often exist... Zno-SnO2 ZnO/SnO2 composite SnO2 /Zn2 SnO4 Zn2 SnO4 Zn2 SnO4 1.3.2.3 Optical properties of Zn2 SnO4: Cr 3+ Table 1.8 Summary of some color emissions of Zn2 SnO4: Cr 3+ Phosphors ZTO: Cr 3+ 4+ 3+ Like Mn ions,
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