臺灣博碩士論文加值系統

本實驗利用固態反應法(solid-state reaction)進行螢光粉的製備，第一系列是以Ba2YNbO6作為螢光粉主體材料，藉由摻雜不同濃度Sm3+稀土離子，並觀察於不同摻雜濃度情況下螢光粉之結晶結構、表面型態與發光特性之影響。第二系列是藉由共摻雜La3+離子取代Y3+離子之晶格位置以改善螢光粉體之發光性質。第三則是以Ba2LaNbO6作為螢光粉主體材料，摻雜不同濃度的稀土離子Sm3+，並分析於不同摻雜濃度對螢光粉之晶體結構、表面型態及發光特性之影響。第四系列是以Ba2YNbO6固定摻雜2 mol% Sm3+稀土離子並且共摻雜Bi3+助熔劑，觀察於不同共摻雜濃度支助熔劑情況下螢光粉之結晶結構、表面型態與發光特性之影響。
系列一是以Ba2YNbO6作為螢光粉主體材料，藉由摻雜不同濃度Sm3+稀土離子及共摻雜Bi3+稀土離子，由X-Ray diffraction分析結果顯示，在煆燒溫度1250 oC煆燒6小時的情況下，表明Ba2YNbO6為立方體系結構，並沒有二次相的產生。在284 nm激發波長激發下，四個放射峰波長分別坐落於550~585 nm、651~682 nm、602~636 nm以及713~752 nm，分別為4G5/2→6H5/2磁偶極躍遷、4G5/2→6H9/2電偶極躍遷以及4G5/2→6H7/2、4G5/2→6H11/2電子躍遷。當Sm3+離子濃度為2 mol%時有最強的放射強度，之後發生濃度淬滅效應。CIE色度座標隨著Sm3+摻雜濃度變化由淺藍光區偏移至橘紅光區。
系列二為在Ba2(Y0.98Sm0.02)NbO6螢光粉體中，以La3+離子取代Y3+離子之晶格位置，製備成Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉。由XRD分析結果顯示，在煆燒溫度1250 oC，煆燒6小時的情況下，隨著La3+離子摻雜濃度的遞增，螢光粉體之結晶結構由立方體系之Ba2YNbO6結構轉變為單斜晶系之Ba2LaNbO6結構。在SEM分析中得知，可以觀察到螢光粉體之表面型態並不會隨著La3+離子摻雜濃度之多寡而有太大的變化，皆為不規則狀且具有顆粒團聚之現象。透過Williamson-Hall方程式計算，摻雜不同濃度La3+離子之晶格應變均為壓應變狀態，且壓應變值變大，證實La3+離子成功取代Y3+離子之晶格位置。
第三系列則是以Ba2LaNbO6作為螢光粉主體材料，摻雜不同濃度之Sm3+稀土離子，由X-Ray diffraction分析結果顯示，在煆燒溫度1250 °C下持續溫度6小時，可以觀察到螢光粉體為單斜晶系之Ba2LaNbO6結構，並無二次相產生。在284 nm激發波長下，其放射光譜有四個Sm3+離子特性放射峰出現，波長坐落於550~585 nm、651~682 nm、602~636 nm以及713~752 nm，分別為Sm3+離子之4G5/2→6H5/2磁偶極躍遷、4G5/2→6H9/2電偶極躍遷以及4G5/2→6H7/2、4G5/2→6H11/2電子躍遷。當Sm3+離子濃度為2 mol%時有最強的放射強度，之後發生濃度淬滅效應，CIE色度座標隨著摻雜濃度變化由淺藍光區偏移至橘紅光區。
第四系列是以Ba2YNbO6固定摻雜2 mol% Sm3+稀土離子並且共摻雜不同濃度之Bi3+助熔劑，由X-Ray diffraction分析結果顯示，在煆燒溫度1250 oC，煆燒6小時的情況下，可以觀察到螢光粉體為立方體系結構，並沒有二次相的產生。在Bi3+離子共摻下可以觀察到，螢光粉體之發光強度提高，可說明Bi3+離子發揮助熔劑之效果。CIE色度座標隨著Bi3+共摻雜濃度變化由橘紅光區偏移至橘黃光區。

The solid-state reaction method was used to prepare phosphors in this study. In the first part, Ba2YNbO6 was used to be the host, and co-doped with different concentrations of Sm3+ ions. The influences of doping ion concentrations on the structure, surface morphologies and luminescence properties of phosphors were examined. In the second part, in order to improve the luminescence properties of phosphors, La3+ ions were used to replace the Y3+ ions in the lattice of Ba2YNbO6 system. The third part, the Ba2LaNbO6, is used to be the host of phosphor material and doped with different concentrations of Sm3+ ion to explore the effects of different doped concentrations on the crystal structure, surface morphology and luminescence properties of the phosphors.The fourth part, Ba2YNbO6 fixed doping Sm3+ concentration 2 mol% phosphor powder and using co-doping method as Bi3+ flux to synthesize powder. Observe the influence of phosphor crystal structure, surface morphology and luminescence characteristics under different co-doping concentrations to support flux.
In the first part, Sm3+ ions doped Ba2YNbO6 phosphors were synthesized using the solid-state reaction. The XRD analysis results show that all of the phosphors are the cubic structure of the Ba2YNbO6, and there is no secondary phase under the calcination temperature of 1250 oC for 6 h in the air. The results show that Sm3+ ions incorporate into the Ba2YNbO6 cubic structure and replace the Y3+ ion lattice to form a solid solution. Under the excitation wavelength of 284 nm, there are four emission peaks appear in the wavelength region of 550 ~ 585 nm, 651 ~ 682 nm, 602 ~ 636 nm and 713 ~ 752 nm, which are corresponding to the magnetic dipole transition of 4G5/2
→6H5/2, electric dipole transition of 4G5/2→6H9/2, and electronic transition of 4G5/2→6H7/2, 4G5/2→6H11/2, respectively. There is the strongest emission intensity for the Sm3+ ion concentration is 2 mol%, and a concentration quenching effect is observed when the Sm3+ ion concentration is larger than 2 mol%. The CIE chromaticity coordinate shifts from the light blue region to the orange-red light region with increasing the Sm3+ ion concentrations.
In the second part of this study, the Y3+ ions are replaced by La3+ ions in the Ba2(Y0.98Sm0.02)NbO6 phosphor system. The XRD analysis results show that the crystal structure of the phosphor changes from the cubic structure of Ba2YNbO6 to the monoclinic structure of Ba2LaNbO6, without the formation of second phases under the calcination temperature of 1250 oC for 6 h in the air. The SEM micrographs were observed that the surface morphologies of phosphors do not be changed much, and the surface morphology is irregular and the particle agglomeration was occurred as the La3+ ion concentration increasing. The compressive strain exists when the Y3+ ions are replaced by La3+ ions calculated using the Williamson-Hall equations which is due to a large ion of La3+ ions to replace a small ion of Y3+ ions successful in the lattices of Ba2(Y0.98Sm0.02)NbO6 system.
In the third part, the Ba2LaNbO6 is the host of phosphor, and is doped with different concentrations of Sm3+ ions. The XRD results show that it has a monoclinic structure, and no secondary phase is observed under the calcination temperature of 1250oC for 6 h in the air. At the excitation wavelength of 284 nm, four of the emission peaks appear of Sm3+ 4f-f characteristic transition in the emission spectra of the wavelengths located at 550 ~ 585 nm, 651 ~ 682 nm, 602 ~ 636 nm and 713 ~ 752 nm, respectively, which corresponds to the magnetic dipole transition of the 4G5/2→6H5/2, the electric dipole transition of the 4G5/2→6H9/2, and the electronic transition of the 4G5/2→6H7/2, 4G5/2→6H11/2, respectively. There is the strongest emission intensity of the Sm3+ ion concentration is 2 mol%,and the concentration quenching effect occur when the Sm3+ ion concentration is higher than 2 mol%. The CIE chromaticity coordinates shift from the light blue area to the orange-red light area as the different concentrations of the Sm3+ ion increased.
In the fourth part, the Ba2YNbO6 fixed doping Sm3+ concentration 2 mol% phosphor powder and using co-doping method as Bi3+ flux to synthesize powder. The XRD results show that it has a cubic structure, and no secondary phase is observed under the calcination temperature of 1250oC for 6 h in the air.Meanwhile, the emission intensity was enhanced as the Bi3+ ion doped-Ba2(Y0.98Sm0.02)NbO6 phosphor, indicating that the Bi3+ ion can act as a sensitizer in this study.The CIE chromaticity coordinate shifts from the light orange-red region to the orange-yellow light region with increasing the Bi3+ ion concentrations.

摘要................................................................................................................................. i
Abstract ........................................................................................................................ iii
誌謝............................................................................................................................... vi
目錄.............................................................................................................................. vii
表目錄........................................................................................................................... xi
圖目錄.......................................................................................................................... xii
第一章 緒論 ................................................................................................................. 1
1-1 前言 ................................................................................................................ 1
1-2 Ba2YNbO6主體晶體介紹 ............................................................................... 2
1-3 Ba2LaNbO6主體晶體介紹 ............................................................................. 2
1-4 研究動機與目的 ............................................................................................ 3
第二章 理論基礎與文獻回顧 ..................................................................................... 8
2-1 發光之定義 .................................................................................................... 8
2-1-1 螢光與磷光之關係 ............................................................................. 8
2-1-2 依激發源的種類與其應用 ................................................................. 8
2-1-3 螢光材料簡介 ..................................................................................... 9
2-2 螢光材料種類 ................................................................................................ 9
2-2-1 有機螢光材料 ..................................................................................... 9
2-2-2 無機發光材料 ..................................................................................... 9
2-2-3 半導體發光材料 ............................................................................... 11
2-3 固態材料中的光致發光現象 ...................................................................... 11
2-3-1 本質型發光(Intrinsic Luminescence) ............................................... 11
2-3-1-1 能帶發光(band-to-band luminescence) ......................................... 11
2-3-1-2 激子發光(exciton luminescence) .................................................. 11
2-3-1-3 交叉發光(cross-luminescence)...................................................... 12
2-3-2 外質型發光(extrinsic luminescence) ................................................ 12
2-3-2-1 侷限型(localized type) ................................................................... 12
2-3-2-2 非侷限型(unlocalized type) ........................................................... 13
2-4 螢光粉體發光機制簡介 .............................................................................. 13
2-4-1 發光原理與發光過程 ....................................................................... 13
2-4-2 組態座標(configuration coordination) ............................................. 13
2-4-3 史托克位移(stokes shift) .................................................................. 14
2-4-4 能量轉移(energy transfer) ................................................................ 14
2-4-5 電子-聲子交互作用(electron-phonon interaction)........................... 15
2-4-6 交叉緩解(cross relaxation) ............................................................... 15
2-4-7 非輻射躍遷(non-radiative transition) ............................................... 15
2-5 影響發光效率及性質的主要因素 .............................................................. 15
2-5-1 主體晶格效應 ................................................................................... 16
2-5-2 毒劑效應(poisoning effect) .............................................................. 16
2-5-3 熱淬滅效應(thermal quenching) ...................................................... 16
2-5-4 濃度淬滅效應(concentration quenching effect) ............................... 16
2-5-5 光游離效應(photoionization effect) ................................................. 16
2-5-6 補償效應(offset effect) ..................................................................... 17
2-6 螢光體的組成與選擇 .................................................................................. 17
2-7 螢光粉體之合成技術 .................................................................................. 18
2-7-1 固態反應法(solid-state reaction) ...................................................... 18
2-7-2 水熱合成法(hydrothermal method) .................................................. 19
2-7-3 溶膠-凝膠法(sol-gel method) ........................................................... 19
第三章 實驗方法與步驟 ........................................................................................... 34
3-1 實驗流程 ...................................................................................................... 34
3-2 實驗材料 ...................................................................................................... 34
3-3 成分與結構分析 .......................................................................................... 35
3-3-1 X光繞射 (X-ray diffraction analysis, XRD) 分析 .......................... 35
3-3-2 場發射掃描式電子顯微鏡 (Field emission scanning electron microscopy, FE-SEM) 分析 ........................................................................ 35
3-4 螢光粉體之光學特性分析 .......................................................................... 35
3-4-1 吸收光譜(Absorption spectrum)....................................................... 35
3-4-2 螢光光譜儀(Photoluminescence, PL)特性量測 .............................. 35
3-4-3 衰減時間(Decay time)分析 .............................................................. 35
3-4-4 化學分析電子能譜儀(Electron spectroscope for chemical analysis, ESCA) .......................................................................................................... 36
3-4-5 CIE色度座標分析(analysis of C.I.E chromaticity diagram) ............ 36
第四章 結果與討論 ................................................................................................... 42
4-1 以固態反應法製備Ba2YNbO6 : Sm3+螢光粉 ............................................ 42
4-1-1 Ba2YNbO6 : Sm3+ 螢光粉之X-ray結構性質分析 ......................... 42
4-1-2 場發射掃描式電子顯微鏡(FE-SEM)表面形態分析 ...................... 42
4-1-3 Ba2YNbO6 : Sm3+螢光粉之吸收光譜分析 ....................................... 43
4-1-4 Ba2YNbO6 : Sm3+螢光粉之激發光譜分析 ....................................... 43
4-1-5 Ba2YNbO6 : Sm3+螢光粉之放射光譜分析 ....................................... 43
4-1-6 Ba2YNbO6 : Sm3+螢光粉之衰減曲線 ............................................... 44
4-1-7 Ba2YNbO6 : Sm3+螢光粉之ESCA分析 ........................................... 45
4-1-8 CIE色度座標 .................................................................................... 45
4-1-9 Ba2YNbO6 : Sm3+螢光粉之熱淬滅分析 ........................................... 45
4-1-10結論 .................................................................................................. 46
4-2以固態反應法製備Ba2(Y0.98-xLaxSm0.02)NbO6 (x = 0 ~ 0.98)之螢光粉 .... 65
4-2-1 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之X-ray結晶結構分析 ............. 65
4-2-2 場發射掃描式電子顯微鏡(FE-SEM)表面形態分析 ...................... 65
4-2-3 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之吸收光譜分析 ........................ 65
4-2-4 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之激發光譜分析 ........................ 65
4-2-5 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之放射光譜分析 ........................ 66
4-2-6 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之衰減曲線 ................................ 66
4-2-7 Ba2(Y0.98-xLaxSm0.02)NbO6螢光粉之ESCA分析 ............................ 66
4-2-8 CIE色度座標 .................................................................................... 67
4-2-9結論 .................................................................................................... 67
4-3以固態反應法製備Ba2LaNbO6 : Sm3+之螢光粉 ........................................ 80
4-3-1 Ba2LaNbO6 : Sm3+螢光粉之X-ray結構性質分析 .......................... 80
4-3-2 場發射掃描式電子顯微鏡(FE-SEM)表面形態分析 ...................... 80
4-3-3 Ba2LaNbO6 : Sm3+螢光粉之吸收光譜分析 ..................................... 80
4-3-4 Ba2LaNbO6 : Sm3+螢光粉之激發光譜分析 ..................................... 81
4-3-5 Ba2LaNbO6 : Sm3+螢光粉之放射光譜分析 ..................................... 81
4-3-6 Ba2LaNbO6 : Sm3+螢光粉之衰減曲線 ............................................. 82
4-3-7 Ba2LaNbO6 : Sm3+螢光粉之ESCA分析 ......................................... 82
4-3-8 CIE色度座標 .................................................................................... 82
4-3-9 Ba2LaNbO6 : Sm3+螢光粉之熱淬滅分析 ......................................... 83
4-3-10結論 .................................................................................................. 83
4-4 以固態反應法製備Ba2(Y0.98Sm0.02)NbO6螢光粉共摻Bi2O3助熔劑 .... 101
4-4-1 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之X-ray結構性質分析 101
4-4-2 場發射掃描式電子顯微鏡(FE-SEM)表面形態分析 .................... 101
4-4-3 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之吸收光譜分析 ........... 101
4-4-4 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之激發光譜分析 ........... 102
4-4-5 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之放射光譜分析 ........... 102
4-4-6 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之衰減曲線 ................... 103
4-4-7 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之ESCA分析 ............... 103
4-4-8 CIE色度座標 .................................................................................. 103
4-4-9 Ba2(Y0.98Sm0.02)NbO6共摻Bi2O3螢光粉之熱淬滅分析 ............... 104
4-4-10結論 ................................................................................................ 104
第五章 總結論 ......................................................................................................... 121
5-1 第一部份： ................................................................................................ 121
5-2 第二部份： ................................................................................................ 122
5-3 第三部分 : ................................................................................................. 122
5-4 第四部分 : ................................................................................................. 123
參考文獻.................................................................................................................... 124
Extended Abstract .................................................................................................... 129

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