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研究生： 唐筱婷
Tang, Hsiao-Ting
論文名稱： 真空氣氛下燒結透光氧化鋁陶瓷
Preparation of Translucent Polycrystalline Alumina by Vacuum Sintering
指導教授： 黃啟原
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： 2017
畢業學年度： 105
語文別： 中文
論文頁數： 82
中文關鍵詞： 真空燒結 、多晶氧化鋁 、注漿成形 、透光 、機械性質
外文關鍵詞： vacuum sintering, polycrystalline alumina, slip casting, translucent, mechanical properties
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    • 　　本研究利用注漿成形法製備Mg2+ 添加量0-2000 ppm之多晶氧化鋁生胚，真空氣氛下以不同條件燒結，探討其微結構、透光率、硬度及破裂韌性。漿料以去離子水當作溶劑混合氧化鋁粉末，分別添加0-2000 ppm Mg2+，並加入分散劑聚丙烯酸銨改善漿料黏度，利用釔安定氧化鋯磨球球磨，提高氧化鋁粉末分散性並降低顆粒凝聚情形，得到流動性佳之漿料，注入石膏模製成生胚，經過 800oC/12 h 預燒結，去除分散劑並消除細小氧化鋁顆粒，生胚相對密度約62-66%。
    　　所得生胚在高溫爐A、B真空氣氛下以不同條件進行燒結，A、B高溫爐皆為中度真空範圍 (1-10-3 mbar)，但因爐體大小差異，高溫爐A之爐體較大，真空度較差，高溫爐B之爐體較小，真空度較好，因此生胚燒結後結果不同。
    實驗結果顯示，添加1000 ppm Mg2+ 之樣品以高溫爐A 1700oC 燒結能達到相對密度99.4%，高溫伴隨晶粒粗化，晶粒尺寸17.3 μm，本實驗所得最佳之直線透光率6.93%，硬度值16.26 GPa、破裂韌性3.25 MPa/m1/2。　　
    　　高溫爐B之樣品經過1700oC燒結，純氧化鋁燒結體密度僅96.7%，添加Mg2+ 的燒結體密度提高至98.8%，純氧化鋁樣品晶粒尺寸為33.5 μm，添加Mg2+ 能夠抑制晶粒成長，晶粒縮減至10-12 μm，但當添加量由500 ppm增加至 2000 ppm抑制晶粒成長的效果並沒有明顯增加，因此添加Mg2+ 於結構當中，可同時抑制晶粒成長並在較低燒結溫度得到較緻密的燒結體，而樣品直線透光率因孔隙過多而低至2%，硬度值17-18 GPa、破裂韌性3.5-4 MPa/m1/2。

    The transmittance and mechanical properties of polycrystalline alumina ceramic are related to its density, porosity, and grain size. Green bodies with high relative density and high uniformity are required for polycrystalline alumina ceramic. In this study, polycrystalline alumina green bodies doped with 0–2000 ppm Mg2+ were produced by slip casting. A dispersant, PAA-NH4, was added in order to achieve low viscosity. Pre-heating at 800C for 12 h eliminated fine particles and decomposed magnesium nitrate and the dispersant. The relative density of the green bodies was 62–66%. Sintering was done in vacuum at various temperatures, holding times, and heating rates in furnaces A and B. The results show that the bodies with 1000 ppm Mg2+ has high transmittance after sintering at 1700C for 1 h in furnace A. The relative density reached 99.4% and the real in-line transmission was 6.93%. The hardness and fracture toughness were 16.26 GPa and 3.25 MPa × m1/2, respectively. Sintering in vacuum at 1700°C for 1 h was done in furnace B. Doping of alumina with Mg2+ raised its density to 98.8% (the density of pure alumina is only 96.7%). Doping alumina with Mg2+ inhibited its grain growth, resulting in its densification at low temperature and its improvement of mechanical properties. The real in-line transmission was 2% because of its numerous pores, and its hardness and fracture toughness were 17–18 GPa and 3.25 MPa × m1/2, respectively.

    摘要 I Abstract II 致謝 XII 目錄 XIII 表目錄 XVI 圖目錄 XVII 第一章 緒論 1 1-1 前言 1 1-2 研究動機 1 1-3 研究目的 2 第二章 文獻回顧 3 2-1 氧化鋁基本性質與應用 3 2-2 多晶氧化鋁 5 2-2-1 透光機制 5 2-2-2 機械性質 8 2-3 透光多晶氧化鋁之原料 10 2-3-1 氧化鋁粉末特性 10 2-3-2 助燒結劑 10 2-4 透光多晶氧化鋁之成形技術 12 2-4-1 成形技術介紹 12 2-4-2 注漿成形 14 2-5 透光多晶氧化鋁燒結 15 2-5-1 燒結理論 15 2-5-2預燒結 18 2-5-3特殊設備燒結及燒結氣氛控制 20 第三章 實驗方法與流程 23 3-1 漿料製備與性質分析 23 3-1-1 起始粉末 23 3-1-2 助燒結劑與分散劑 24 3-1-3 X光繞射分析 24 3-1-4 漿料黏度分析 25 3-2 注漿成形 25 3-2-1 石膏模製程 25 3-2-2 注漿成形流程 25 3-3生胚分析 27 3-3-1 生胚密度 27 3-3-2 生胚微結構 27 3-4 燒結體分析 28 3-4-1燒結條件 28 3-4-2 燒結體密度 29 3-4-3 燒結體微結構 29 3-4-4 透光率 30 3-4-5 硬度與破裂韌性 30 第四章 結果與討論 33 4-1 起始粉末分析 33 4-2 漿料分析 35 4-3 生胚分析 37 4-4 透光多晶氧化鋁之觀察 41 4-4-1 高溫爐 A 之燒結體分析 41 4-4-2 高溫爐 B 之燒結體分析 50 4-5 高溫爐A及高溫爐B燒結結果比較 61 4-6 透光率分析 64 4-7 硬度與破裂韌性量測 68 4-8 真空環境下1700oC樣品比較 74 第五章 結論 78 參考文獻 79

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