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研究生:陳郡甫
論文名稱:添加氧化鈦於鋰鋁矽酸鹽玻璃陶瓷在失透過程中顯微結構的變化
論文名稱(外文):Effect of adding TiO2 on the microstructure of lithium aluminosilicate glass ceramics during devitrification processes
指導教授:李志浩李志浩引用關係
學位類別:碩士
校院名稱:國立清華大學
系所名稱:工程與系統科學系
學門:工程學門
學類:核子工程學類
論文種類:學術論文
論文出版年:2007
畢業學年度:95
語文別:中文
論文頁數:64
中文關鍵詞:鋰鋁矽酸鹽玻璃陶瓷低熱膨脹係數
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本論文主要探討鋰鋁矽酸鹽玻璃陶瓷,在氧化鈦成分比例(共有
0 wt%、1 wt%、2 wt%、4 wt%共四種比例)的試樣,經過不同的熱處理條件下,使用X光粉末繞射、X光吸收光譜術和紅外光吸收光譜術分析其內部微結構與相改變之間的關係。由X光粉末繞射我們發現主晶相(β-石英固溶體、β-鋰輝石固溶體)的相轉變熱處理溫度會隨氧化鈦添加量的增加而降低,而且熱處理溫度的上升有助於次要相(金紅石、鈦酸鋯、矽酸鋯、鋅或鎂尖晶石)晶體的成長。從X光近吸收邊緣的光譜特徵可知鈦、鋯元素週遭原子結構隨熱處理條件的變化。當試樣從非晶質玻璃相轉變為高度結晶相時,這兩種元素的配位數會從低的配位數轉變為高的配位數(鈦從4配位變為6配位,鋯從6變成8配位)。不過添加氧化鈦4 wt%的試樣就沒有配位數變化的趨勢,但由鈦K層的X光近吸收邊緣光譜相當類似六配位鈦的金紅石結構;而鋯K層的X光近吸收邊緣光譜類則近似於八配位鋯的矽酸鋯結構。紅外光吸收光譜術不能夠直接推測主晶相或是次要相的種類,不過可以間接由吸收波段的變化,判斷參與相變化的元素週邊原子的鍵結與鍵結的振動形式,進一步證實X光粉末繞射中主晶相的變化。
In the thesis, we changed the titanium dioxide contents under different heat treatment conditions to observe the variations of the inner microstructure while the phase transform. X-ray powder diffraction, X-ray absorption spectroscopy and infrared spectroscopy were used. According to the XRD results, while the titanium dioxide contents were increased, the phase transformation temperatures of the main phases (β-quartz solid solutions and β-spodumene solid solutions) were decreased. And then various secondary phases were usually precipitated at higher temperatures. XAS showed that the local environment of Ti and Zr were changed by different thermal treatment conditions. According to the XANES of Ti (Zr) K-edge studies, the coordination numbers changed from lower to higher coordination number while the sample transforms from an amorphous glass to a highly crystalline glass ceramics (Ti from 4 to 6, Zr from 6 to 8). But these phenomena would not be observed at the samples of the 4 wt% TiO2. More information about the materials fine structure can be obtained from infrared spectroscopy data. We could utilize the variations of the IR spectral feature to decide that the bond of the inner atoms, the kinds of bonding vibration and the phase type.
摘要…………………………………………………………Ⅰ
Abstract……………………………………………………Ⅱ
致謝…………………………………………………………Ⅲ
目錄…………………………………………………………Ⅳ
圖目錄………………………………………………………Ⅵ
表目錄………………………………………………………Ⅸ
第一章 序論
1-1 前言……………………………………………………1
1-2 研究動機………………………………………………1
1-3 研究內容………………………………………………2

第二章 文獻回顧
2-1 玻璃陶瓷………………………………………………3
2-2 璃陶瓷形成的基本原理………………………………3
2-2-1 導論……………………………………………3
2-2-2 玻璃的相分離…………………………………5
2-2-3 玻璃結晶化的控制……………………………6
2-2-4 成核劑…………………………………………7
2-2-5 玻璃陶瓷的特性與應用………………………8
2-3 鋰鋁矽酸鹽系玻璃陶瓷………………………………10
2-3-1 鋰鋁矽酸鹽玻璃陶瓷的簡介………………………10
2-3-2 LAS玻璃陶瓷主晶相的晶體結構與其性質…………12
2-3-3 添加氧化鈦對於鋰鋁矽酸鹽玻璃陶瓷的影響…16

第三章 實驗設計
3-1 試片製備………………………………………………19
3-2 試片分析………………………………………………20
3-2-1 熱差分析………………………………………20
3-2-2 X光粉末繞射……………………………………21
3-2-3 X光吸收光譜術…………………………………21
3-2-4 紅外線吸收光譜術……………………………22
3-3 儀器原理………………………………………………24
3-3-1 熱差分析法……………………………………24
3-3-2 X光粉末繞射……………………………………25
3-3-3 X光吸收光譜術…………………………………25
3-3-4 紅外線吸收光譜術………………………………28

第四章 實驗結果與討論
4-1 XRD數據及分析…………………………………………………30
4-2 XAS數據及分析…………………………………………………42
4-2-1 鋯的K層X光吸收光譜…………………………………42
4-2-2 鈦的K層X光吸收光譜…………………………………46
4-4 實驗結果綜論…………………………………………………57

第五章 結論…………………………………………………………59
參考文獻……………………………………………………………61
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