臺灣博碩士論文加值系統

高溫燒結高嶺土而生成富鋁紅柱石 (mullite) 的過程裡，有許多反應發生；高嶺土經由固相分解生成鋁矽比例為富鋁的~2:1第一型 mullite (primary mullite, M(I))，而經由玻璃化 (vitrification) 後再成核、成長的第二型 mullite (secondary mullite, M(II) 或 M(III))，其鋁矽比例為~3:2。第二型富鋁紅柱石的成長機制，進而陶瓷體的組織結構 (texture)，均受到生胚製程的影響文獻裡早有報導，但是除了結晶成長方向曾經被分析過，在刮刀成型的高嶺土生胚，燒結後所衍生的組織結構卻經常無法複製，而再現性輒遭非議。
實驗中利用不同的生胚製程條件，以玻璃化燒結方式製作陶瓷試樣、來觀察燒結完成後富鋁紅柱石的顯微結構與組織結構，進而瞭解影響生成富鋁紅柱石組織結構的主因。其中使用不同的儀器進行顯微結構的鑑定及分析，由X-ray diffraction (XRD) 的巨觀方式與掃描式電子顯微鏡 (SEM)及穿透式電子顯微鏡 (TEM) 等微觀的方法來完成整體的研究結果。

There are lots of reactions in formation of mullite during sintering of kaolinite powder at high temperature. Primary mullite (M(I), 2Al2O3·SiO2) is the result of a solid state reaction of kaolinite. And secondary mullite (M(II) or M(III), 3Al2O3·2SiO2) is formed by vitrification after nucleation and grain growth. It has been investigated that the growth mechanism of secondary mullite and the texture of ceramics are affected by the process of green tape. Expect that the growth direction of crystal has been analyzed, the texture of kaolinite green tape formed by tape casting after sintered can not be reproduced.
In order to realize the mechanism in formation of mullite we study different green tape process by vitrification and observe the microstructure of mullite after sintering.. The microstructure is analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM).

Abstract .…………………………………………………………..……Ⅰ
摘要………………………………………………………………..……Ⅱ
目錄………………………………………………………………..……Ⅲ
圖索引………………………………………………………………..…Ⅵ
表索引…………………………………………………………...……. Ⅸ
第一章 前言………………………………………………..……………1
第二章 文獻回顧……………………………………………..…………3
2.1 高嶺土的結構與特性………………………………….……………3
2.2 富鋁紅柱石的結構與特性………………………….………………7
2.3 Mullite的結晶成長方向………………………………………...…..9
2.4 燒結高嶺土生成 mullite 的反應………………………………….9
2.5 刮刀成型製程對富鋁紅柱石組織結構的影響…………...………12
第三章 實驗步驟………………………………………………………15
3.1 實驗藥品………………………………………………...…………15
3.1.1 高嶺土…………………………………………………………15
3.1.2 Darvan C……………………………………………..…………15
3.1.3 聚乙烯醇 (polyvinyl alcohol, PVA)………………...………...16
3.1.4 聚乙二醇 (polyethylene glycol, PEG)………………………..16
3.1.5 BYK-340……………………………………………...………..17
3.2 試片製作…………………………………………..……………….17
3.2.1 刮刀成型法……………………………………………………17
3.2.1.1 高嶺土細粉末的懸浮液製備…………………………….17
3.2.1.2 泥漿的製備與厚膜的刮刀成型………………………….18
3.2.2 單向冲壓法……………………………………………………19
3.2.2.1高嶺土原始粉末壓餅……………………………………..19
3.2.2.2 高嶺土細粉末壓餅……………………………………….19
3.2.3 樣品燒結條件…………………………………………………24
3.3 X-ray 繞射…………………………………………………...……..24
3.4 掃描式電子顯微鏡…………………………...……………………24
3.5 穿透式電子顯微鏡………………………………………..……….25
第四章 結果……………………………………………………………27
4.1 X-ray 繞射分析…………………………………………...….…….27
4.1.1 粉末與薄膜生胚X-ray分析……………………………….…27
4.1.2 冲壓粉末與薄膜熟胚(as-sintered) X-ray分析…………….…29
4.1.2.1 燒結條件為樣品包埋高嶺土粉末……………………….29
4.1.2.2 燒結條件為樣品置放於氧化鋁基板…………………….31
4.2 掃描式電子顯微鏡觀察…………………………………………...33
4.2.1 厚膜生胚觀察………………………………………………....33
4.2.2 燒結條件為包埋原始高嶺土粉末且以1500oC燒結4小時…37
4.2.2.1 單軸向冲壓法製作的原始粉末熟胚…………………….37
4.2.2.2 單軸向冲壓法製作的高嶺土細粉末熟胚………....…….39
4.2.2.3 刮刀成型法製作的高嶺土細粉末熟胚…………….……41
4.2.3 燒結條件為置於氧化鋁基板上且以1500oC燒結4小時..…43
4.2.4 燒結條件為置於氧化鋁基板上且以1600oC燒結1小時..…46
4.2.4.1 刮刀成型法製作的高嶺土細粉末熟胚………………….46
4.2.4.2 單軸向冲壓法製作的高嶺土細粉末熟胚……………….49
4.3 穿透式電子顯微鏡觀察…………………………………………...50
4.3.1 原始粉末與高嶺土細粉末觀察…………………………...….50
4.3.2 Mullite 相與玻璃相周圍未知相的觀察……………………...52
4.3.3 樣品與氧化鋁基板貼合介面的觀察…………………………54
第五章 結果與討論……………………………………………………57
第六章 結論……………………………………………………………59
第七章 未來工作………………………………………………………60
參考文獻……………………………….……………………………….61

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