Synthesis and Luminescence Properties of Oxide Nanophosphors by Solvothermal Method
- Abstract
- This thesis reports the correlation between the synthesis, crystallization and luminescence properties of GdVO4:Eu3+, Y1-xGdxVO4:Eu3+, Gd2O3:Eu3+, Y2O3:Eu3+, La2O3:Eu3+, CaTiO3:Pr3+ and Li doped CaTiO3:Pr3+ nanophosphors, respectively.
The oxide nanophosphors were prepared by solvothermal method. The compared to the solid state reaction method, the most important advantage of the solvothermal process is simple and fast at room temperature with a grain size on the nanometer scale.
In the phosphors, the optimization of chemical composition, particle size distribution, and morphology are required for the more efficient luminescence of phosphor materials. Among them, the spherical morphology is an important factor for lower light scattering at the surface as well as higher packing densities. The enhancement in photoluminescence performance of oxide phosphors may result not only from the improved crystallinity leading to higher oscillating strengths for the optical transitions, but also from the reduced internal reflections of the emitted light due to the rougher surface. The nanophosphors crystalline, surface morphology and luminescence properties are highly dependent on sintering temperature, grain size, host lattice and sensitizer.
The luminescence properties were enhanced by the improved crystallinity and surface morphology. Also, the nanophosphor with efficient luminescence properties can be obtained by the control of synthesizing conditions. In this study reported the luminescence properties on synthesis conditions. The crystallinity, grain size and luminescence properties of nanophosphors are dependent on the sintering temperature. Sintering temperature was found to effectively enhance not only the morphology but also luminescence properties of the nanophosphors. For the Li-doped phosphors, the improvement in photoluminescence intensity with the Li-doping may results from the improved crystalline. For the enhanced PL intensity, it can also be suggested that the incorporation of Li+ ions creates the oxygen vacancies, which might act as a sensitizer for the effective energy transfer due to the strong mixing of charge transfer state.
This thesis have been discussed the synthesis of nanophosphors by solvothermal method and oxide phosphors properties. So, the oxide phosphors can give a promise for fluorescence lamp and display technologies.
- Issued Date
- 2013
- Awarded Date
- 2013. 2
- Type
- Dissertation
- Publisher
- 부경대학교
- Affiliation
- 부경대학교 대학원
- Department
- 대학원 물리학과
- Advisor
- 정중현
- Table Of Contents
- Abstract ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ i
1. Introduction ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 1
1.1 History of phosphor technology ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 1
1.2 Application of phosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 2
1.2.1 LCD (liquid crystal display) ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 4
1.2.2 PDP (plasma display panel) ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 5
1.2.3 FED (field emission display) ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 8
1.2.4 VFD (vacuum fluorescent display) ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 9
1.3 Nanophosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 11
1.4 Research purpose․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 12
2. Theoretical background ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 14
2.1 A general introduction to luminescent materials ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 14
2.2 Luminescence mechanism ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 16
2.2.1 Excitation mechanism ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 16
2.2.2 Emission mechanism ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 20
2.2.3 Activator ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 21
2.3 Energy transfer ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 22
2.4 Energy level of rare earth ions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 24
2.4.1 Luminescence properties of Eu3+ ion ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 24
2.4.2 Luminescence properties of Pr3+ ion ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 29
2.5 CIE 1931 ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 30
3. Experimental ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 35
3.1 Synthesis of nanophosphor ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 35
3.1.1 Solvothermal synthesis ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 37
3.1.2 Sintering ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 39
3.2 Nanophosphor powders synthesis by solvothermal method ․ ․ ․ ․ ․ ․ ․ ․ ․ 43
3.2.1 Precursor preparation ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 44
3.2.2 Precursor solvothermal reactions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 45
3.3 Characterization of the phosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 46
3.3.1 XRD ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 46
3.3.2 FE-SEM ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 48
3.3.3 PL and PLE spectra ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 49
4. Results and discussion ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 53
4.1 Luminescence characteristics of GdVO4:Eu3+ nanophosphors ․ ․ ․ ․ ․ ․ ․ 53
4.1.1 Synthesis conditions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 55
4.1.2 XRD patterns ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 57
4.1.3 FE-SEM images ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 59
4.1.4 PL and PLE spectras ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 59
4.1.5 Summary ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 64
4.2 Luminescence characteristics of Y1-xGdxVO4:Eu3+ nanopowder ․ ․ ․ ․ ․ ․ 66
4.2.1 Synthesis conditions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 66
4.2.2 XRD patterns ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 67
4.2.3 FE-SEM images ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 68
4.2.4 PL and PLE spectras ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 70
4.2.5 Summary ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 75
4.3 Luminescence characteristics of RE2O3:Eu3+ (RE = Gd, Y and La) nanophosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 76
4.3.1 Synthesis conditions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 78
4.3.2 XRD patterns ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 79
4.3.3 FE-SEM images ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 79
4.3.4 PL and PLE spectras ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 81
4.3.5 Summary ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 84
4.4 Luminescence characteristics of CaTiO3:Pr3+ and Li-doped CaTiO3:Pr3+ nanophosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 85
4.4.1 CaTiO3:Pr3+ nanophosphor ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 88
4.4.1.1 Synthesis conditions ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 88
4.4.1.2 XRD patterns ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 89
4.4.1.3 FE-SEM images ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 90
4.4.1.4 PL and PLE spectras ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 92
4.4.2 Li-doped CaTiO3:Pr3+ nanophosphors ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 98
4.4.2.1 XRD patterns ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 98
4.4.2.2 FE-SEM images ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 99
4.4.2.3 PL and PLE spectras ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 101
4.4.4 Summary ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 105
5. Conclusion ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 109
6. References ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 112
7. ACKNOWLEDGEMENT ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ ․ 118
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