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研究生：	韋亞曼 Wijaya, Arman Kusuma
論文名稱：	熔鹽法應用於白光LED之綠光螢光粉Ca3(ScZn)2Si3O12:Ce3+效果研究 Effects of Fluxes on Luminescence Properties of Ca3(ScZn)2Si3O12:Ce3+ Green Phosphor for White LEDs
指導教授：	陳引幹 Chen, In-Gann
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2014
畢業學年度：	102
語文別：	英文
論文頁數：	107
外文關鍵詞：	Carbothermal reduction method, flux, PL intensity, Quantum efficiency, Thermal stability
相關次數：	點閱：88 下載：2
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Carbothermal reduction (CTR) method was used to synthesize several samples series; flux added into Ca2.955Sc1.8Zn0.3Si3O12:0.03Ce3+ (CSZS:Ce), Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu2+, Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu3+, and Ca2.955Ga2Si3O12:0.03Ce3+ (CGS:Ce). Different kind of fluxes; LiF, NaF, LiF-NaF and NH4Cl fluxes were added into Ca2.955Sc1.8Zn0.3Si3O12:0.03Ce3+ (CSZS:Ce) separately. We used Eu2O3 as an activator source and NaF flux in solid state reaction and carbothermal reduction method to form Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu3+ and Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu2+, respectively. Another sample series were prepared by substituted Sc3+ ions by Ga3+ ions to form Ca2.955Ga2Si3O12:0.03Ce3+. Doped Zn2+ and NaF flux also were used to form Ca2.955Ga1.8Zn0.3Si3O12:0.03Ce3+ series.
By adding 2 wt% of NaF flux into CSZS:Ce, can enhance the PL intensity and quantum efficiency as high as CSZS:Ce without flux. Besides, can reduce the sintering temperature up to 300 oC compared to former CSZS:Ce without flux. However, the thermal quench tend to decrease more for CSZS:Ce with flux. In addition, NH4Cl flux has a negative effect at low temperature of sintering process due to many impurities can be detected from XRD. LiF-NaF compound flux exhibit a single phase at relative low sintering temperature 1150 oC only by using 1 wt% of compound flux.
From XRD pattern, both Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu2+ and Ca2.955Sc1.8Zn0.3Si3O12:0.03Eu3+ with 2 wt% of NaF showed a good crystallinity at 1150 oC. Replacing activator Ce3+ ions by Eu2+ or Eu3+ ions has significant effect specially on emission wavelength of phosphor. According UV/Visible spectra, CSZS:Eu2+ can be excited by UV light and visible light (green). A weak emission can be observed from UV light excitation but no emission detected in visible light region from green light excitation (520 nm). CSZS:Eu3+ show weak emission between 580-640 nm.
Compared with Ca2.955Sc1.8Zn0.3Si3O12:0.03Ce3+ (CSZS:Ce) series, Ca2.955Ga2Si3O12:0.03Ce3+ (CGS:Ce) series were not matched well with XRD database pattern Ca3Ga2Si3O12 JCDPS# 74-1576. However, many impurities detected such Ca2Ga2SiO7 and Ca2SiO4.

Abstract	I
Acknowledgement	III
Table of Contents	IV
List of Tables	VII
List of Figures	VIII
Chapter 1 Introduction	1
1–1	Background	1
1–2	Motivation and Purpose	2
1–3 Architecture of Thesis	3
Chapter 2 Fundamentals and Literature Reviews	5
2–1 Concept and Definitions of Luminescent Materials	5
2–1–1 Phosphors	5
2–1–2 Mechanism of Luminescence	7
2–2 Design of Phosphor Powder	9
2–2–1 Body Structure Effect	9
2–2–2 Selection for the Activator	10
2–2–2–1 Transition Metal Ions	10
2–2–2–2 Rare-Earth Ions	11
2–2–2–3 Structural Defects	12
2–2–3 Poisoners and Inhibitors	13
2–3 Factors Affecting the Emission Wavelength	13
2–3–1 Configurational Coordinate Diagram	13
2–3–2 Stokes Shift	14
2–3–3 Nephelauxetic Effect	15
2–3–4 Lattice Field Effect	16
2–4 Factors Affecting the Emission Intensity	19
2–4–1 Concentration Quenching	19
2–4–2 Toxic Effect	20
2–4–3 Sensitizer	20
2–4–4 Thermal Quenching	21
2–4–4–1 Quenching Mechanism	21
2–4–5 The Main High-Huang-Rhys Coupling Constants	22
2–4–6 Surface Defects	23
2–4–7 Residual Impurity	23
2–5 Principles and Applications of Material Characterization Instruments	24
2–5–1 Differential Thermal Analysis/Thermogravimetric (DTA/TG)	24
2–5–2 X-Ray Diffractometer (XRD)	25
2–5–3 Scanning Electron Microscopy (SEM)	25
2–5–4 Fluorescence Spectrometer	26
2–6–1 Crystal Structure	28
2–6–2 Luminescence	29
2–7 Phosphor Research on Chen, In-Gann’ s Laboratory	30
2–7–1 Research YAG:Ce Yellow Phosphor	30
2–7–1–1 Synthesis of Nano YAG:Ce by Co-precipitation Method with HMDS	30
2–7–1–2 Prepared YAG:Ce Nano Powder by Adding Different Concentrations of HMDS	30
2–7–1–3  Study of YAG:Ce Phosphor Coated by SiO2	30
2–7–1–4 Doped Si Into YAG:Ce Phosphor	31
2–7–2 Study of Ca3Sc2Si3O12:Ce3+ Green Phosphors	31
2–7–2–1	Preparation of Ca2.955Sc2-yAlySi3O12:0.03Ce3+ (y=0–0.4)	31
2–7–2–2	Preparation of Ca2.955Sc2-(2x/3)ZnxSi3O12:0.03Ce3+ (x=0–0.5)			32
2–7–3	Study of CaTiO3:Eu3+, Li+ Red Phosphor	32
2–7–4 Study of Ca3Y2Si3O12:RE3+ Phosphor	33
2–7–4–1 Study of Ca3Y2Si3O12:Eu3+ Red Phosphor	33
2–7–4–2 Study of Ca3Y2Si3O12:Tb3+, Ce3+ Green Phosphor	33
2–7–4–3 Study of Ca3Y2Si3O12:Dy3+, Ce3+ Phosphor	33
2–8 Literature Reviews of Ca3Sc2Si3O12:Ce3+	33
2–8 Literature Reviews of Ca3Ga2Si3O12:RE3+	38
Chapter 3 Experimental Methods and Procedures	49
3–1 Raw Materials	49
3–2 Experimental Procedures	52
3–2–1 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+ (CSZS:Ce) Green Phosphor With Different Fluxes		52
3–2–2 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+:RE (RE=Eu2+ and Eu3+) With NaF Flux	54
3–2–3 Investigating the Structure and Luminescence Properties of Ca2.955Sc2Si3O12:Ce3+ (CGS:Ce) Series	54
3–3 Equipments	55
3–3–1 High Temperature Box Furnace	55
3–3–2 X-Ray Diffraction Spectrometer (XRD)	55
3–3–3 Fluorescence Spectrophotometer	55
3–3–4 UV/Visible Spectrometer	56
3–3–5 Scanning Electron Microscope (SEM)	56
3–3–6 Differential Thermal Analysis/Thermal Gravimetric (DTA/TG)	56
Chapter 4 Results and Discussions	60
4–1 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+ (CSZS:Ce) Green Phosphor With Different Fluxes	60
4-1-1 Differential Thermal Analysis/Thermogravimetric (DTA/TG)	60
4-1-2 X-Ray Diffraction (XRD)	61
4-1-3 Scanning Electron Microscopy (SEM)	62
4-1-4 Luminescence Properties	63
4–2 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+:RE (RE=Eu2+ and Eu3+) With NaF Flux	85
4–2–1 Structure Analysis of Ca2.955Sc1.8Zn0.3Si3O12:Eu2+ and Ca2.955Sc1.8Zn0.3Si3O12:Eu3+	85
4–2–2 Photoluminescence Spectra of Ca2.955Sc1.8Zn0.3Si3O12:Eu2+ and Ca2.955Sc1.8Zn0.3Si3O12:Eu3+	85
4–3 Investigating the Structure and Luminescence Properties of Ca2.955Sc2Si3O12:Ce3+ (CGS:Ce) Series	92
Chapter 5 Conclusion	101
5–1 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+ (CSZS:Ce) Green Phosphor With Different Fluxes	101
5–2 Investigating the Structure and Luminescence Properties of Ca2.955Sc1.8Zn0.3Si3O12:Ce3+:RE (RE=Eu2+ and Eu3+) With NaF Flux	102
5–3 Investigating the Structure and Luminescence Properties of Ca2.955Sc2Si3O12:Ce3+ (CGS:Ce) Series	102
References	104
                                    

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