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研究生: 劉依婷
Liu, I-Ting
論文名稱: 添加θ-Al2O3粉末製得之透光氧化鋁的特徵研究
Characteristics of translucent alumina fabricated by adding theta alumina powders
指導教授: 郭明錦
Kuo, M.C.Tom
共同指導: 顏富士
Yen, Fu-Su
學位類別: 碩士
Master
系所名稱: 工學院 - 資源工程學系
Department of Resources Engineering
論文出版年: 2018
畢業學年度: 106
語文別: 中文
論文頁數: 69
中文關鍵詞: 真空燒結Theta alumina透光氧化鋁注漿成形
外文關鍵詞: Translucent alumina, Theta Alumina, Vacuum sintering, Slip casting
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  • 本研究在d50 = 240 nm的高純度α-Al2O3中,添加d50 = 18 nm 的θ- Al2O3,配置成含θ- Al2O3 0–30 wt%的θ/α- Al2O3的漿料。利用注漿成形法製成生坯,並於生坯中添加500 ppm的Mg2+,在真空條件下以1530-1700°C持溫1小時進行燒結。以BET、XRD、DTA觀察起始粉末平均粒徑、礦物相以及生坯於較低溫的相變熱反應。進行真空燒結後量測相對視密度、以SEM觀察微結構並計算平均晶粒大小以及量測光穿透率來比較添加θ-Al2O3細粒成分對粗粒α-Al2O3於高溫燒結的影響。
    結果顯示全部的生坯相對密度都可以達到68%以上,最高的生坯密度76%出現在θ添加量為15 wt%的樣品。而從真空燒結試驗可以發現,添加θ-Al2O3對透光氧化鋁燒結體密度、晶粒尺寸,及光穿透率均有影響。由θ-Al2O3相轉換得之的細粒α-Al2O3會與原存在的粗粒α-Al2O3形成兩個燒結系統。粗細兩種粒體間的相互熱反應顯然較缺乏,因此添加θ-Al2O3確實會抑制原α-Al2O3的晶粒成長,但其抑制效果止於15-20 wt% θ添加量間,出現晶粒約9.0 μm(燒結條件:1700°C持溫1小時)。
    研究結果也說明燒結體的透光率,於1530-1600°C間由燒結體密度主導,於1650°C-1700°C間則是燒結體之晶粒大小為影響關鍵。前者,15 wt% θ的樣品可以獲得最高的全穿透率64%以及直線穿透率6.52%,晶粒大小約7 μm。後者因抑制晶粒成長的結果,添加θ-Al2O3者存在較多的晶界影響,透光率相對較低。隨添加量減少,樣品晶粒尺寸達15 μm(0% θ添加量),獲得最高的全穿透率85%,直線穿透率22%。根據本研究計算與綜合實驗結果推知,θ/α-Al2O3混合的最佳比例應介於15-20 wt%間。此時全穿透率78%以及直線穿透率15%,晶粒大小約11 μm。

    The characteristics of processing green body and the followed sintering behavior during fabricating the translucent alumina using mixtures of α-Al2O3 powders (crystallite size 240 nm and chemical purity: Al2O3 99.9%) and θ-Al2O3 powders (18 nm and 99.9% ) were examined. Slurries prepared by mixing α-Al2O3 powders with 5, 10, 15, 20 and 30 wt % of θ-Al2O3 were used to produce green bodies by slip casting techniques. After dried, the green body was doped with 500 ppm Mg2+ and then sintered at 1530-1700°C for 1hr under vacuum status. It is found that the relative density of all green bodies can reach over 69%. The green with highest density of 76% was obtained when 15 wt % of θ-Al2O3 was added. The vacuum sintering results reveal that the slurries with θ-Al2O3 powders would affect the sintered density, grain size, and light transmittance properties of the translucent alumina. It is worthwhile to note that the finer-grained α-Al2O3 particles which transformed from θ-Al2O3 will experience a second sintering system coexisting with that of the original coarser-grained α-Al2O3. Although we didn't thoroughly observe the sintering phenomena of the two systems, the result shows the addition of θ-Al2O3 obviously slows down the grain growth of α-Al2O3. According to the calculations and experimental results, the optimal ratio of θ/α-Al2O3 mixtures should be between 15~20/85~80. In this case the alumina will show 78% total transmission, 15% in-line transmission, and its mean sintered grain size can be 11 μm.

    摘要 I Extended Abstract II 致謝 IX 目錄 X 表目錄 XII 圖目錄 XIII 第一章 緒論 1 1.1 前言 1 1.2 研究動機 2 1.3 研究設計 2 第二章 相關文獻回顧與整理 3 2.1 氧化鋁及其過渡相 3 2.1.1 氧化鋁的相變 3 2.1.2 氧化鋁的結晶相 5 2.1.3 θ-Al2O3相轉換的臨界粒徑與基礎晶徑 10 2.1.4 α-Al2O3的存在對於θ-相轉換的影響 10 2.2 多晶透光氧化鋁 12 2.2.1 製作透光氧化鋁的要點 12 2.2.1.1 粉體特性 12 2.2.2.2 助燒結劑 19 2.2.2.3 成形方法 21 2.2.2 陶瓷體的透光機制 24 2.2.3 燒結機制 26 第三章 研究方法及步驟 29 3.1 實驗原料 29 3.2 實驗方法 31 3.2.1 漿料與生坯製備 31 3.2.2 燒結條件 31 3.3 特性分析 34 3.3.1 粉末結晶相分析 34 3.3.2 粉末熱差分析 34 3.3.3 漿料粒徑分佈分析 34 3.3.4 粉末比表面積分析 35 3.3.5 顯微結構分析 35 3.3.6 生坯及燒結體密度量測 36 3.3.7 燒結體透光率量測 37 第四章 結果與討論 38 4.1 生坯性質分析 38 4.2 燒結體性質分析 42 4.2.1 燒結體密度 42 4.2.2 燒結體微結構變化 42 4.2.3 燒結體平均晶粒尺寸 43 4.2.3 燒結體光穿透率 43 4.3 θ-Al2O3的功能 54 4.3.1 θ-Al2O3的添加量與透光主導因素 54 4.3.2 θ-Al2O3與雙燒結系統 55 第五章 結論 62 參考文獻 63 附錄 68

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