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研究生：	張豐勝 Chang, Feng-Sheng
論文名稱：	Mg-alpha-SiAlON氮氧化物螢光粉之合成製程開發與螢光效能之研究 Process Development for Synthesis of Mg-alpha-SiAlON Oxynitride Phosphor and on its Phosphor Performance
指導教授：	鍾賢龍 Chung, Shyan-Lung
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2010
畢業學年度：	98
語文別：	中文
論文頁數：	142
中文關鍵詞：	螢光粉、氮氧化物、燃燒合成法、SiAlON 、引燃劑、螢光粉後處理
外文關鍵詞：	Phosphor, Oxynitride, Combustion synthesis, Igniter, SiAlON, Post-synthesis treatment
相關次數：	點閱：95 下載：0
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白光LED被當作新世代之固態照明設備，其具有高功率、省電、散熱佳、長壽命化、無汙染等之優點，而目前工業上使用之氧化物螢光粉(如YAG：Ce3+)並不符合這些要求，特別是運用於高功率的白光LED之氧化物螢光粉熱穩定性較差，操作溫度上升後易造成光色的改變，高性能螢光粉之開發因而成為白光LED發展上之重要課題。近來文獻研究顯示氮氧化物螢光粉，其具有高發光效率、高化學穩定性、熱穩定性佳、無環境汙染並且可在藍光或紫外光下激發，因而被應用在具有潛能白光LED固態照明中，現今由於氮氧化物螢光粉在合成製程一般是需要高溫、高壓或長時間反應且設備造價昂貴，因而限制了其應用。在過去研究文獻中，極少對於Mg-α-SiAlON 螢光粉之螢光性質研究，因此本論文將引用本實驗室過去建立之合成氮化物陶瓷粉體與Ca-α-SiAlON螢光粉之燃燒合成法，並成功地開發出能夠在低壓下以及在短時間內可大量製造Mg-α-SiAlON 螢光粉之方法。本論文探討反應物的組成、螢光粉後處理如酸洗、熱處理等對產物之影響，最後找出發光強度較佳之條件並與市售作比較，實驗結果發現，改變反應物間的組成與比例，可合成出不同螢光強度及波長之範圍之Mg-α-SiAlON螢光粉體，此螢光粉的激發波長範圍為220~500nm，若利用380nm之紫外光激發此螢光粉可得到一主峰波長位置位於555nm 及發光範圍介於400~650nm 之放射光譜，而螢光粉體後處理程序中發現酸洗與再次燃燒合成皆可以有效提升螢光強度，但並不影響產物之激發、放射光譜與晶相組成，其最佳螢光強度已超越市售螢光粉強度，約為市售1.12倍。

White light-emitting diodes (white LEDs) are considered as next-generation solid-state lighting systems because of their promising advantages such as low power consumption, lower heat generation, high efficiency, high reliability, long lifetime, and the lack of mercury. The presently used oxide phosphors (e.g.,YAG:Ce3+) can not meet the requirements of high efficiency and high thermal stability by the high power white LED applications. It causes the color shift when operation temperature increased. It is thus an important research subject to develop phosphors materials with desirable properties such as high efficiency, high thermal stability, chemical resistance and high brightness. Recently, oxynitride phosphors which has high luminescence intensity, high chemical stability, thermal stability properties under UV or blue light irradiation, have received considerable attention due to their potential applications in solid-state lightings and displays. The literatures didn’t indicated that oxynitride phosphor (Mg-α-SiAlON) had luminescence properties. However, the conditions for producing this kind of oxynitride phosphor by using nowadays synthesis methods are such as high temperature, high pressure, long duration time, and expensive equipments. For the reason the production costs of oxynitride phosphor are too high to limit its applications. In our laboratory had been developed on nitride ceramic materials and oxynitride phosphors (Ca-α-SiAlON) by self-propagating high temperature synthesis (SHS) reactions for this thesis. The Mg-α-SiAlON phosphor was produced in large scale, low pressure, and short duration time. It discussed the effects on the properties of the product including reactant composition ,and post-synthesis treatments. The results showed that the phosphor with different luminescence intensity and wavelength by using different condition and parameters. There was a product which excitation spectrum was covered the range of 220-500nm and a broad emission band in the range of 400-650nm and centered at 555nm was observed upon 380nm excitation. The phosphor increases luminescence intensity by post-synthesis treatment, but it doesn’t have negative effect on the properties of the product including excitation spectrum, emission spectrum and crystalline phase. The luminescence intensity can exceed commercial phosphor and the intensity is 1.12 times compared with commercial phosphor.

中文摘要...................................................I
英文摘要.................................................III
誌謝.......................................................V
總目錄...................................................VII
表目錄....................................................XI
圖目錄...................................................XII
第一章 緒論.................................................1
1-1 前言...................................................1
1-2 研究動機及目的..........................................3
第二章 理論基礎及文獻回顧....................................4
2-1 螢光材料...............................................4
2-1-1 螢光材料之發展........................................4
2-1-2 螢光材料之分類........................................5
2-2 螢光材料之理論基礎.......................................8
2-2-1 發光機制及種類........................................8
2-2-2 發光原理............................................10
2-2-3 影響螢光發光特性之因素................................14
2-2-4 稀土離子的發光特性....................................19
2-3 螢光材料之應用........................................ 22
2-4 α-SiAlON 與α-SiAlON 螢光粉之介紹及文獻回顧..............24
2-4-1 α-SiAlON之介紹..................................... 24
2-4-2 α-SiAlON 螢光粉之文獻回顧............................25
2-4-3 α-SiAlON 之文獻回顧..................................35
2-5 合成α-SiAlON 螢光粉之方法及比較.........................41
第三章 實驗方法及設備...................................... 47
3-1 實驗藥品............................................. 47
3-2 實驗設備..............................................48
3-2-1 壓模成形設備及模具....................................48
3-2-2 燃燒合成反應器.......................................49
3-2-3 保溫裝置............................................51
3-2-4 分析儀器............................................52
3-3 儀器原理及量測方法.....................................52
3-3-1 晶相分析............................................53
3-3-2 光學特性分析.........................................53
3-3-3 微結構及元素分析.....................................54
3-3-4 熱電偶溫度之測量.....................................55
3-4 實驗方法及流程.........................................56
3-4-1 反應物製作.......................................... 56
3-4-2 引燃劑包覆.......................................... 56
3-4-3 燃燒合成反應........................................ 57
3-4-4 反應物參數.......................................... 59
3-4-5 產物後處理.......................................... 59
3-4-5-1 產物酸洗......................................... 59
3-4-5-2 產物熱處理.........................................61
3-4-5-3 產物熱處理與酸洗.................................. 62
3-4-6 產物之分析...........................................62
3-4-7 反應溫度之測量...................................... 63
第四章 結果與論............................................64
4-1 反應物的組成對產物之影響................................66
4-1-1 氮化矽對產物之影響....................................66
4-1-2 疊氮化鈉對產物之影響..................................75
4-1-3 氯化銨對產物之影響....................................82
4-1-4 銪離子摻雜量對產物之影響..............................92
4-2 最佳參數之探討........................................101
4-3 產物後處理之影響..................................... 108
4-3-1 產物酸洗之影響......................................108
4-3-2 產物熱處理之影響....................................117
4-3-3 產物熱處理後酸洗之影響...............................125
第五章 結論...............................................134
參考文獻.................................................137
自述.....................................................142

                                    

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校內：2015-07-29公開
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