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系統識別號 U0026-0812200912052958
論文名稱(中文) 鹼土矽酸鹽類螢光粉體之製備及其光性質研究
論文名稱(英文) Synthesis and Luminescence Properties of Alkaline Silicate Phosphors
校院名稱 成功大學
系所名稱(中) 材料科學及工程學系碩博士班
系所名稱(英) Department of Materials Science and Engineering
學年度 94
學期 2
出版年 95
研究生(中文) 游國彰
研究生(英文) Kuo-Chang Yu
電子信箱 hooker@mail.mse.ncku.edu.tw
學號 n5690108
學位類別 碩士
語文別 中文
論文頁數 85頁
口試委員 口試委員-張炎輝
指導教授-黃啟祥
口試委員-陳引幹
口試委員-朱聖緣
口試委員-丁志明
中文關鍵字 發光性質  螢光粉  矽酸鹽 
英文關鍵字 phosphors  luminescence  silicate 
學科別分類
中文摘要 與UV-LED 搭配的紅色螢光粉,是近來深受注目的研究方向。為獲得相對發射光強度較強之紅色螢光粉體,本研究以溶膠-凝膠法合成MSiO3:Eu3+ X mole% ( M=Mg, Ca, Sr, Ba;X=0~20 ) 螢光粉體,檢討煆燒溫度、Eu3+離子之添加量、二次熱處理、TEOS 水解條件之控制及增感劑Bi3+離子之添加等實驗參數,對合成粉體發光性質之影響。
M=Mg, Ca, Sr 及Ba 之四系列MSiO3:Eu3+螢光粉,其發射光光譜之形態均相似,於383nm 波長激發時,其發射光波長皆位於613nm 及590nm處,在CIE 座標圖中落於紅色光區域裏。其發射光強度是隨著活化劑添加量的提高而增強,其中MgSiO3:Eu3+對其他三種螢光粉而言,有相對較高之發光強度。各系列螢光粉,其煆燒溫度分別為,MgSiO3:Eu3+ 12mole%於800 oC、CaSiO3:Eu3+ 12mole%於1200 oC、SrSiO3:Eu3+ 12mole%於900oC、BaSiO3:Eu3+ 12mole%於900 oC 煆燒且恆溫2h 具有相對較高發射光強度。粉體在煆燒過程中,於表面所產生之孔洞,對其發光性質有損害的現象。
對MgSiO3:Eu3+ 12 mole%螢光粉體而言,其發射光強度是隨著二次熱處理溫度的提高而增強,於1000 oC 時有較佳之發射光強度。控制TEOS水解溫度為80 oC,pH 值為0.85 時,所得粉體有較佳之發光強度;而藉6mole%增感劑Bi3+的添加,其粉體之發光強度有明顯增加之現象。


英文摘要 Red phosphors applied in UV-LED is the one of the significant topicsrecently. In order to obtain the efficient phosphors, MSiO3:Eu3+ X mole%
( M=Mg, Ca, Sr, Ba;X=0~20 ) were synthesized via sol-gel method. Theeffects of calcination temperature, contents of Eu3+and Bi3+, conditions of re-heat treatment and hydrolysis of TEOS on the relative emission intensity of the phosphors were investigated.
It had similar form for the emission spectra of MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ). The emission intensity peaks are at 613 and 590nm while the
MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ) phosphors were excited by UV-LED ( λem=383nm ). However, it had higher emission intensity of MgSiO3:0.12Eu3+calcined at 800 oC, CaSiO3:0.12Eu3+ calcined at 1200 oC,
SrSiO3:0.12Eu3+ calcined at 900 oC and BaSiO3:0.12Eu3+ calcined at 900 oC
for 2h.
In the study, the emission intensity of MgSiO3:0.12Eu3+ powders increased with raising the temperature of re-heat treatment。The phosphors had the highest emission intensity while controlling the re-heat treatment at
1000 oC、the condition of TEOS at 40 oC, pH=0.85。Doping 6mol% Bi3+ for the phosphors is also increasing the emission intensity.


論文目次 目錄
中文摘要……………………………………………………………………Ⅰ
英文摘要……………………………………………………………………Ⅱ
目錄…………………………………………………………………………Ⅲ
表目錄………………………………………………………………………Ⅵ
圖目錄………………………………………………………………………Ⅶ
第一章緒論………………………………………………………………1
1-1 前言……………………………………………………………………1
1-2 研究動機與目的………………………………………………………2
第二章 理論基礎與文獻回顧………………………………………………5
2-1 螢光材料簡介…………………………………………………………5
2-2 螢光材料分類…………………………………………………………5
2-3 螢光材料激發源種類及其應用………………………………………8
2-4 發光原理簡介…………………………………………………………9
2-5 活化劑與抑制劑的介紹……………………………………………11
2-6 稀土離子的發光特性………………………………………………11
2-8 色彩簡介……………………………………………………………13
2-8-1 視覺敏感度……………………………………………………13
2-8-2 CIE 色度座標 ( CIE x,y chromaticity ) ………………………13
2-8-3 演色性 ( Color rendering index;CRI ) ………………………15
2-9 溶膠-凝膠法…………………………………………………………15
2-9-1 溶膠-凝膠法反應機構…………………………………………15
2-9-2 TEOS 之水解縮合反應…………………………………………16
2-10 文獻回顧……………………………………………………………17
第三章 實驗方法及步驟…………………………………………………30
3-1 實驗用起始原料……………………………………………………30
3-2 實驗流程……………………………………………………………31
3-2-1 以溶膠凝膠法製備MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ) 螢光
粉體…....……………………………………………….…….......31
3-2-1-1 煆燒處理…………………………………………………31
3-2-2 MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ) 螢光粉體之改質…………32
3-2-2-1 TEOS 水解條件之控制……………………………………32
3-2-2-2 煆燒粉體之後續熱處理…………………………………32
3-2-2-3 增感劑Bi3+離子之摻雜……………………………………32
3-3 成分與結構分析………………………………………………..……33
3-3-1 X-RAY 繞射( X-Ray Diffractometer,XRD )分析………………33
3-3-2 熱重熱差 ( DTA/TG ) 分析……………………………...……33
3-3-3 傅立葉轉換紅外線吸收光譜儀(FT-IR)………………………33
3-3-4 場發射型掃瞄式電子顯微鏡( FE-SEM )分析…………...……33
3-3-5 高解析穿透式電子顯微鏡 ( HR-TEM ) 分析………………34
3-4 光性質量測…………………………………………………………34
3-4-1 光譜儀(Photoluminescence Spectrometer)分析……………34
3-4-2 相對發射強度量測……………………………………………..34
3-4-3 色度座標分析 ( Analysis of C.I.E. chromaticity diagrams ) ….34
第四章 結果與討論……………………………………………………...…40
4-1 MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ) 螢光粉體之性質研究……….…40
4-1-1 熱差-熱重 ( DTA/TGA ) 分析……………………………...…40
4-1-2 粉體之FT-IR 分析………………………………………………40
4-1-3 粉體之相鑑定及微結構分析………………………..…………41
4-1-3-1 X 光繞射( XRD )及穿透式電子顯微鏡( TEM )分析…..…41
4-1-3-2 掃描式電子顯微鏡 ( SEM ) 分析…………..……………43
4-1-4 螢光光譜分析……………………………………………..……44
4-1-4-1 粉體之激發光譜量測…………………………………...…44
4-1-4-2 煆燒溫度對發射光強度之影響………………………...…45
4-1-4-3 活化劑添加量對發射光強度之影響………………...……46
4-2 MSiO3:Eu3+ ( M=Mg, Ca, Sr, Ba ) 螢光粉體之改質…………….…46
4-2-1 二次熱處理對粉體發光性質之影響………………………..…46
4-2-2 TEOS 水解條件控制對粉體發光性質之影響…………….……47
4-2-3 添加增感劑Bi3+對粉體發光性質之影響……………………...48
第五章 結論……………………………………………………………...…80
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