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研究生： 吳孟倫
Wu, Meng-Lun
論文名稱： 在真空及氮氣氣氛下之氧化鋁初階段燒結研究
Early-stage Sintering of Alumina in Vacuum and Nitrogen Atmosphere
指導教授： 黃啓原
Huang, Chi-Yuen
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： 2019
畢業學年度： 108
語文別： 中文
論文頁數： 56
中文關鍵詞： 多晶氧化鋁 、注漿成型 、燒結動力學 、氣氛燒結
外文關鍵詞： alumina, slip casting, atmosphere sintering, activation energy, nitrogen, vacuum
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    • 本研究探討在不同燒結環境下，對於多晶氧化鋁燒結行為的影響，有別於以往探討在添加不同助燒結劑、升溫速率等因素，觀察在真空和氮氣氣氛下燒結之微結構變化。先以注漿成型法製備相對密度可達61%之生胚，使用助燒結劑以硝酸鎂作為前驅物利用滲透法添加500 ppm Mg2+至生胚中，分別以真空、氮氣和傳統常壓燒結，並分析其微結構、晶粒尺寸、密度及燒結活化能。
    由實驗結果得知，於真空和氮氣氣氛下燒結之密度，皆可在1400℃不持溫的燒結條件下達到98%以上的相對密度，在1450℃持溫4 h 之條件下相對密度甚至可以達到99.7%。晶粒尺寸方面，真空和氮氣氣氛之燒結樣品在不持溫的情況下可使晶粒限縮在1 μm 以下，根據燒結末期之晶粒成
    長公式計算，並和數據進行擬合，以0-4 h 的持溫條件下，真空與氮氣氣氛之晶粒成長指數為2，傳統常壓燒結則為3。微結構方面，於氮氣氣氛與傳統常壓燒結下之燒結體有明顯較大的孔隙，這是由於形成封閉型孔隙時，孔隙內部氣壓上升且內部氣體不易透過晶界擴散至表面，而在真空環境下則無觀察到上述情況。最後再以Arrhenius 方程式計算在不同燒結環境下的活化能，並進行比較。

    The initial sintering kinetic of alumina have been studied in different heating rate and doped with metallic oxide (TiO2 or MgO). However, sintering in atmosphere is barely discussed. In this study, green compacts of alumina were produced by slip casting and doped with 500 ppm Mg2+ by infiltration. The α-alumina powder dispersed in deionized water by PAA-NH4. After pre-heated at 800℃ for 12 h, the compacts sintered in air, vacuum and nitrogen atmosphere at 1300-1450℃ and held for 0-4 h. The samples sintered in vacuum and in nitrogen could reach high density (~98%) at 1400℃ and grain size could be ~1 μm. The activation energy of sintering during densification is analyzed by Arrehnius equation. The results of densification activation energy in vacuum, nitrogen and air are 67.4 kJ/mol, 46.8 kJ/mol and 194.7 kJ/mol respectively. After fitting the form with various sintering atmosphere, grain growth exponent n of vacuum and nitrogen sintering are 2, and conventional sintering is 3. The activation energy of grain growth in different atmosphere can be analyzed. It is 268.4 kJ/mol for vacuum sintering and 269.3 kJ/mol, 512.5 kJ/mol for nitrogen and conventional sintering respectively.

    摘要 ................................................. I 致謝 .................................................. X 目錄 ................................................ XI 圖目錄 ..................................... XIII 表目錄 ....................................... XVI 第一章 緒論 .................................... 1 1-1 前言 ............................................ 1 1-2 研究目的 .................................... 1 第二章 文獻回顧 ............................. 2 2-1 氧化鋁的特性與應用 .................................. 2 2-2 成型技術 ........................................ 3 2-3 助燒結劑 .................................. 4 2-4 滲透理論 ..................................... 5 2-5 預燒結 ......................................... 6 2-6 燒結理論 ...................................... 7 2-7 燒結動力學 ................................. 10 2-7-1 擴散機制 ................................ 10 2-7-2 活化能計算 ............................................................................................. 12 2-8 氣氛燒結 .................................................................................................... 17 第三章實驗流程 ............................................................................................... 20 3-1 實驗流程 .................................................................................................... 20 3-2 漿料製備與分析 ........................................................................................ 21 3-2-1 起始粉末分析 ......................................................................................... 21 3-2-2 助燒結劑與分散劑 ................................................................................. 22 3-2-3 漿料黏度分析 ......................................................................................... 23 3-3 注漿成形 .................................................................................................... 23 3-3-1 石膏模製作 ............................................................................................. 23 3-3-2 注漿成形製程 ......................................................................................... 23 3-4 生胚分析 .................................................................................................... 24 3-4-1 預燒結 ..................................................................................................... 24 3-4-2 生胚密度測量 ......................................................................................... 25 3-4-3 生胚微結構 ............................................................................................. 25 3-4-4 修胚 ......................................................................................................... 25 3-5 燒結體分析 ................................................................................................ 26 3-5-1 燒結條件 ................................................................................................. 26 3-5-2 燒結體密度分析 ..................................................................................... 26 3-5-3 燒結體微結構 ......................................................................................... 27 第四章 結果與討論 ......................................................................................... 28 4-1 初始粉末分析 ............................................................................................ 28 4-2 漿料分析 ................................................................................................... 29 4-3 生胚分析 ................................................................................................... 30 4-4 燒結體分析 ............................................................................................... 32 4-4-1 不同燒結溫度 ........................................................................................ 32 4-4-2 不同持溫時間 ........................................................................................ 37 4-5 氣氛燒結活化能 ....................................................................................... 46 第五章 結論 ..................................................................................................... 51 參考文獻 ........................................................................................................... 52

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