臺灣博碩士論文加值系統

本研究主要是以溶膠凝膠法製備BaY2ZnO5作為螢光粉主體，並摻雜不同Tm3+離子濃度作為發光中心，以及添加不同重量百分比之尿素與PEG2000，來探討其添加濃度對於螢光粉的晶體結構、表面型態與光致發光特性之影響。
第一部分以BaY2ZnO5作為螢光粉主體，摻雜不同濃度之Tm3+離子，由XRD結果顯示，在煆燒1200 ℃持溫8小時條件下，摻雜濃度由0.5 mol% 增加至5 mol% 結果顯示有少數的二次相的生成，據推測可能是因為秤重的藥品縮比較小，使量測時的精準度會有誤差而導致二次相產生，但整體仍維持斜方晶系BaY2ZnO5之結構。而從SEM分析得知摻雜不同濃度的Tm3+離子之條件下，可發現螢光粉體之表面型態大多為不規則狀，且顆粒尺寸不一。而在光致發光特性方面，於365 nm波長激發下，由放射光譜得知主要由Tm3+離子特性放射峰所組成，來自於1D2→3F4、1G4→3H6、1D2→3H5、1G4→3F4、1G4→3H5之電子躍遷為主，當Tm3+離子濃度為2 mol%時具有最強之放射強度。CIE色度座標則是隨著Tm3+離子摻雜濃度增加，從藍綠色光區移至深藍色光區。
第二部分則是以BaY2ZnO5作為螢光粉主體，固定Tm3+離子摻雜濃度2 mol%，並添加不同重量百分比之尿素來改善其螢光粉之發光特性。在煆燒1200 ℃持溫8小時條件下，添加濃度從0.5 wt%增加至50 wt%，由XRD結果顯示還是有少數二次相的生成，但整體仍維持斜方晶系BaY2ZnO5之結構。SEM分析方面得知添加不同重量百分比之尿素條件下，可以發現螢光粉體之表面多為不規則狀團聚現象。而在光致發光特性方面，於365 nm波長激發下，由放射光譜得知主要的放射波段457nm為Tm3+離子1D2→3F4之電子躍遷，當尿素離子添加濃度為1 wt.%時能夠增加放射強度。CIE色度座標隨著添加尿素濃度的增加皆位於深藍色光區。
在第三部分仍以BaY2ZnO5作為螢光粉主體，固定Tm3+離子摻雜濃度2 mol%，並添加不同重量百分比之PEG2000，在煆燒1200 ℃持溫8小時條件下，添加濃度從1 wt.%增加至50 wt.%。由XRD結果顯示仍有二次相生成，但仍可維持斜方晶系BaY2ZnO5之結構。SEM分析方面得知添加不同重量百分比之PEG2000條件下，可以發現螢光粉體的表面型態隨著添加濃度的增加，顆粒從不規則狀轉變為球型顆粒，故添加PEG2000確實可以改變螢光粉體之表面顆粒型態。而在光致發光特性方面，於365 nm波長激發下，主要的放射波段457nm (1D2→3F4)為Tm3+離子4f-4f內層軌域之電子躍遷，當PEG 2000離子添加濃度為2 wt.%時能夠增加放射峰的強度。CIE色度座標隨著PEG2000添加量的增加皆位於深藍色光區。
在第四部分是以Ba(Y0.98Tm0.02)2ZnO5添加固定尿素添加量為1 wt.%，在煆燒1200 ℃持溫8小時條件下，改變PEG2000添加量從1 wt.%增加至5 wt.%。由XRD結果顯示還是有少數二次相的生成，但整體仍維持斜方晶系BaY2ZnO5之結構。SEM分析方面得知Ba(Y0.98Tm0.02)2ZnO5:1wt.%尿素螢光粉體的表面型態為隨著PEG 2000添加量的增加，會有較顯著的顆粒但仍有團聚之現象，且顆粒尺寸不一。而在光致發光特性方面，於激發波長365nm的激發下，主要的放射波段457nm為Tm3+離子1D2→3F4之電子躍遷，當固定尿素添加量1wt.%與PEG2000 3 wt.%時能夠增加放射峰的強度。CIE色度座標結果顯示Ba(Y0.98Tm0.02)2ZnO5:1wt.%尿素添加不同PEG2000濃度座標皆位於深藍色光區。

在第五部分是以Ba(Y0.98Tm0.02)2ZnO5添加固定PEG2000添加量為2 wt.%，在煆燒1200℃持溫8小時條件下，尿素離子添加量從1 wt.%增加至5 wt.%。由XRD結果顯示還是有少數二次相的生成，但整體仍維持斜方晶系BaY2ZnO5之結構。SEM分析方面得知添加不同重量百分比之尿素，Ba(Y0.98Tm0.02)2ZnO5:2 wt.%PEG2000螢光粉體的表面型態會由顯著的顆粒狀轉變為不規則狀，且顆粒尺寸會隨著尿素的添加而明顯變大。而在光致發光特性方面，於365 nm波長激發下，添加尿素不影響其發光特性。由放射光譜得知主要仍由Tm3+離子特性放射峰所組成，來自於1D2→3F4、1G4→3H6、1D2→3H5、1G4→3F4、1G4→3H5之電子躍遷為主，當Ba(Y0.98Tm0.02)2ZnO5:2 wt.%PEG2000添加尿素1 wt.%時，位於440 ~ 470 nm範圍之Tm3+離子1D2→3F4電子躍遷強度最強，因此可得知尿素1 wt.%時為最佳添加量。CIE色度座標結果顯示Ba(Y0.98Tm0.02)2ZnO5:2 wt.%PEG2000添加不同尿素濃度座標皆位於深藍色光區。

In this study, BaY2ZnO5 was used to be the host material of phosphor and doped with different concentrations of Tm3+ ion as the luminescent centers prepared using the sol-gel method at 1200 oC for 8 h. In addition, in order to enhance the photoluminescence properties, adding different weight percentages of urea and PEG2000 in the Ba(Y0.98Tm0.02)2ZnO5 phosphor was performed. The effects of addition concentrations on the crystal structure, surface morphology and luminescence properties of the phosphor powder were also examined.
In the Ba(Y1-xTmx)2ZnO5 system, XRD results show that there were some secondary phases for Tm3+ ion concentration doped from 0.5 to 5 mol% but the overall structures of the orthorhombic BaY2ZnO5 was still maintained. The secondary phases were speculated that may be generated due to the proportion of weighed medicines was too small, which will cause errors in the accuracy of the measurement. According to SEM analysis, the surface morphologies of these phosphor powder was irregular mostly with different particle sizes. Under an excitation wavelength of 365 nm, the emission spectrum consists of the 1D2→3F4, 1G4→3H6, 1D2→3H5, 1G4→3F4, and 1G4→3H5 electronic transition of Tm3+ ions. The CIE chromaticity coordinates shifts from the blue-green region to the deep blue region with increasing the Tm3+ ion concentrations.
In the Ba(Y0.98Tm0.02)2ZnO5 added with various contents of urea system, XRD results show that the structure keeps orthorhombic BaY2ZnO5 crystal structure under the calcination temperature of 1200 °C for 8 h. With an increase of the urea contents, there were some secondary phases was observed. According to SEM analysis, the surface morphology of the phosphor powder was mostly irregular with the particles agglomeration. Under an excitation wavelength of 365 nm, the emission spectrum that the main emission band 457 nm was the electronic transition of Tm3+ ion 1D2→3F4.When the conontents of urea was 1 wt.%, the emission intensity would be enhanced.The CIE chromaticity coordinates are located in the deep blue region with the increase of the contents of urea.
Furthermore, in the Ba(Y0.98Tm0.02)2ZnO5 added with various contents of PEG2000 system, XRD results show that the structure is belong to the orthorhombic BaY2ZnO5 crystal structure, but with some secondary phases under the calcination temperature of 1200 °C for 8 h. According to SEM analysis, the surface morphologies of the phosphor powder changed from irregular to granular shape indicating that the PEG2000 additions can indeed change the particle shape of the phosphor powder. Under an excitation wavelength of 365 nm, the main emission band 457 nm(1D2→3F4), which was the 4f-4f inner orbital of Tm3+ ion. When the conntents of PEG2000 was 2 wt.%, the emission intensity would be enhanced. The CIE chromaticity coordinates are still located in the deep blue region with the increase of the PEG2000 contents.
For the various contents of PEG2000 from 1 to 5 wt.% added in the Ba(Y0.98Tm0.02)2ZnO5:1 wt.% urea system, the XRD results show that the structure is orthorhombic BaY2ZnO5 crystal structure, but there are some secondary phases observed under the calcination temperature of 1200 °C for 8 h. According to SEM analysis results, the surface morphologies of the phosphor powders are obvious granular and with agglomerations, but the size of particles are various. Under an excitation wavelength of 365 nm, the emission spectra consist of the 1D2→3F4, 1G4→3H6, 1D2→3H5, 1G4→3F4, and 1G4→3H5 electronic transitions of Tm3+ ions, respectively. Therefore, it can be seen that when the addition of PEG2000 content is 2wt.%, it will have the effect of enhancing emission behavior. The CIE chromaticity coordinates are all located in the deep blue region for various contents of PEG2000 added in the Ba(Y0.98Tm0.02)2ZnO5:1 wt.% urea system.

For the various contents of urea from 1 to 5 wt.% added in the Ba(Y0.98Tm0.02)2ZnO5:2 wt.% PEG2000 system, XRD results show that the structure keeps the orthorhombic BaY2ZnO5 crystal structure but some secondary phases were still observed under the calcination temperature of 1200 °C for 8 h. According to SEM analysis, the surface morphologies of the phosphor powder was obvious granular change to irregular, and the particles size will increase significantly with the addition of urea. Under an excitation wavelength of 365 nm, the emission spectra consists of the 1D2→3F4, 1G4→3H6, 1D2→3H5, 1G4→3F4, and 1G4→3H5 electronic transitions of Tm3+ ions, respectively. Therefore, it can be seen that when the addition of urea content is 3 wt.% which will have the effect of enhancing emission behavior. The CIE chromaticity coordinates are all located in the deep blue region for the the various contents of urea added in the Ba(Y0.98Tm0.02)2ZnO5:2 wt.% PEG2000 system.

摘要...i
Abstract...iv
誌謝...vii
目錄...viii
表目錄...xii
圖目錄...xiii
第一章 緒論...1
1-1前言...1
1-2 BaY2ZnO5主體介紹...2
1-3尿素...2
1-4聚乙二醇...2
1-5研究動機與目的...3
第二章 理論基礎與文獻回顧...8
2-1發光的定義...9
2-1-1螢光與磷光之關係...9
2-1-2激發源的種類與應用...9
2-1-3 螢光材料簡介...10
2-2 螢光材料種類...10
2-2-1有機螢光材料...11
2-2-2無機發光材料...11
2-2-3 半導體發光材料...12
2-3 固態材料中的光致發光現象...12
2-3-1 本質型發光(Intrinsic Luminescence)...13
2-3-2 外質型發光(extrinsic luminescence)...14
2-4 發光機制簡介...15
2-4-1 發光原理與發光過程...15
2-4-2 組態座標(configuration coordination)...15
2-4-3 史托克位移(stokes shift)...15
2-4-4 能量轉移(energy transfer)...16
2-4-5 電子-聲子交互作用(electron-phonon interaction)...17
2-4-6 交叉緩解(cross relaxation) 17
2-4-7 非輻射躍遷(non-radiative transition)...17
2-5 影響發光性質的主要因素...17
2-5-1 主體晶格效應(host lattice effect)...18
2-5-2 熱淬滅效應(thermal quenching)...18
2-5-3毒劑效應(poisoning effect)...18
2-5-4 濃度淬滅效應(concentration quenching effect)...18
2-5-5 光游離效應(photoionization effect)...19
2-5-6 補償效應(offset effect)...19
2-6 螢光體的組成與選擇...19
2-7 螢光粉體之合成技術...20
第三章 實驗方法與步驟...36
3-1 實驗流程...36
3-2 實驗材料...36
3-3 成分與結構分析...37
3-3-1 X光繞射 (X-ray diffraction analysis, XRD)分析...37
3-3-2 場發射掃描式電子顯微鏡 (field emission scanning electron microscopy, FE-SEM)分析...37
3-4 螢光粉體之光學特性分析...37
3-4-1 吸收光譜 (absorption spectrum)...37
3-4-2 螢光光譜儀 (photoluminescence, PL)特性量測...37
3-4-3 衰減時間(Decay time)分析...38
3-4-4 CIE色度座標分析 (analysis of C.I.E chromaticity diagram)...38
第四章 結果與討論...46
4-1 以溶膠-凝膠法製備 Ba(Y1-xTmx)2ZnO5 (x = 0 ~ 0.05) 螢光粉...46
4-1-1 Ba(Y1-xTmx)2ZnO5 螢光粉之XRD結構分析...46
4-1-2 場發射掃描式電子顯微鏡(FE-SEM)表面形態分析...46
4-1-3 Ba(Y1-xTmx) 2ZnO5螢光粉之吸收光譜分析...46
4-1-4 Ba(Y1-xTmx) 2ZnO5螢光粉之激發光譜分析...47
4-1-5 Ba(Y1-xTmx) 2ZnO5螢光粉之放射光譜分析...47
4-1-6 Ba(Y1-xTmx) 2ZnO5螢光粉之衰減曲線...48
4-1-7 CIE色度座標...48
4-1-8 Ba(Y1-xTmx) 2ZnO5螢光粉之熱淬滅分析...48
4-1-9 結論...49
4-2 以溶膠-凝膠法製備Ba(Y0.98Tm0.02) 2ZnO5添加尿素之螢光粉...63
4-2-1 Ba(Y0.98Tm0.02) 2ZnO5添加尿素螢光粉之XRD結構分析...63
4-2-2 FE-SEM表面形態分析...63
4-2-3 Ba(Y0.98Tm0.02) 2ZnO5添加尿素螢光粉之吸收光譜分析...63
4-2-4 Ba(Y0.98Tm0.02) 2ZnO5添加尿素螢光粉之激發光譜分析...64
4-2-5 Ba(Y0.98Tm0.02) 2ZnO5添加尿素螢光粉之放射光譜分析...64
4-2-6 CIE色度座標...64
4-2-7 Ba(Y0.98Tm0.02) 2ZnO5添加尿素螢光粉之熱淬滅分析...64
4-2-8 結論...65
4-3 以溶膠-凝膠法製備Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000之螢光粉...77
4-3-1 Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000螢光粉之XRD結構分析...77
4-3-2 FE-SEM表面形態分析...77
4-3-3 Ba(Y0.98Tm0.02) 2ZnO5添加PEG 2000螢光粉之吸收光譜分析...77
4-3-4 Ba(Y0.98Tm0.02) 2ZnO5添加PEG 2000螢光粉之激發光譜分析...77
4-3-5 Ba(Y0.98Tm0.02) 2ZnO5添加PEG 2000螢光粉之放射光譜分析...78
4-3-6 CIE色度座標...78
4-3-7 Ba(Y0.98Tm0.02) 2ZnO5添加PEG 2000螢光粉之熱淬滅分析...78
4-3-8 結論...79
4-4 以溶膠-凝膠法製備Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG2000之螢光粉...91
4-4-1 Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG2000螢光粉之XRD結構分析...91
4-4-2 FE-SEM表面形態分析...91
4-4-3 Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG 2000螢光粉之吸收光譜分析...91
4-4-4 Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG 2000螢光粉之激發光譜分析...92
4-4-5 Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG 2000螢光粉之放射光譜分析...92
4-4-6 CIE色度座標...92
4-4-7 Ba(Y0.98Tm0.02)2ZnO5固定尿素1wt%並添加不同濃度PEG 2000螢光粉之熱淬滅分析...92
4-4-8 結論...93
4-5 以溶膠-凝膠法製備Ba(Y0.98Tm0.02)2ZnO5添加PEG2000 2wt%與不同尿素含量之螢光粉...105
4-5-1 Ba(Y0.98Tm0.02)2ZnO5添加PEG2000 2wt%與不同尿素含量螢光粉之XRD結構分析...105
4-5-2 FE-SEM表面形態分析...105
4-5-3 Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000 2wt%與不同尿素含量螢光粉之吸收光譜分析...105
4-5-4 Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000 2wt%與不同尿素含量螢光粉之激發光譜分析...106
4-5-5 Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000 2wt%與不同尿素含量螢光粉之放射光譜分析...106
4-5-6 CIE色度座標...106
4-5-7 Ba(Y0.98Tm0.02)2ZnO5添加PEG 2000 2wt%與不同尿素含量螢光粉之熱淬滅分析...106
4-5-8 結論...107
第五章 總結論...119
參考文獻...122

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