臺灣博碩士論文加值系統

本研究以高嶺石(Kaolinite、平均粒徑3.1μm)、滑石(Talc、平均粒徑 6.4μm)及氧化鋁(Alumina、平均粒徑100nm)為原料合成堇青石，並且添加不同粒徑之堇青石粉末作為晶種，藉此降低堇青石的生成溫度。使用之晶種為平均粒徑1.2μm、18.2μm及40.8μm。生料與熟料二者之配比為1:1，經壓碇成型後進行熱處理以取得堇青石相。研究主要透過DTA及XRD技術完成。前者瞭解其熱反應發生溫度範圍，後者對熱處理過程特定溫度所得煆燒粉末的礦物進行相分析。結果發現，相較於未添加晶種之系統，添加晶種可使反應中間相鎂鋁尖晶石(Spinel)與β-堇青石之生成量下降，合成反應路徑改變，使得頑火輝石(Protoenstatite)與富鋁紅柱石(Mullite)及頑火輝石(Protoenstatite)與Al2O3 略過生成Spinel及β-堇青石，而直接生成α-堇青石(α1a，α1m)。藉由計算原料粒體與晶種粉末粒徑差異之配位數關係推知，細化晶種粒體可使系統中受其影響的程度提高，並於1300oC前開始生成α-堇青石。添加平均粒徑1.2μm晶種之樣品，可於1175oC開始生成α-堇青石，並於1250oC持溫30min得到高純相堇青石。

關鍵詞:堇青石，固態反應，晶種，粒徑

In this study, cordierite was synthesized by raw materials kaolinite (mean particle size 3.1μm), talc (mean particle size 6.4μm) and alumina (mean particle diameter 100nm). To lower the formation temperature of cordierite, this research added cordierite powders that differs in particle size as seeds. An mean particle size of the cordierite seeds is 1.2μm, 18.2μm and 40.8μm and the ratio of raw material and seed is 1:1. This research was completed by DTA and XRD techniques. The former is to understand the temperature range of thermal behaviors, the latter is to analyze the mineral phase of a certain calcined powder. Comparing to the system without seed adding, the result of the study showed that, seeding could reduce the intermediate phase Spinel and β-cordierite in the generation and change the synthesis routes.Rather than formed Spinel and β-cordierite, Protoenstatite + Mullite and Proenstatite +Al2O3 directly formed α-cordierite(α1a，α1m).By calculating the particle coordination number of raw material with seeds, the extent of seeding effect in the system would increase with fine seed and result in forming α-cordierite early before 1300oC. It is found that the addition of seed size of 1.2μm begins to synthesize α-cordierite at 1175oC and eventually to get high purity phase cordierite for holding 30min at 1250oC.

Keywords:cordierite,solid-state reation,seeding effect

目錄
中文摘要 I
Abstract II
致謝 III
目錄 V
表目錄 IX
圖目錄 X
第一章 緒論 1
1.1 前言 1
1.2 研究動機 2
1.3 研究目的 3
第二章 理論基礎與前人研究 4
2.1 堇青石介紹 4
2.1.1堇青石結構 5
2.1.2 堇青石熱膨脹特性 6
2.2 堇青石的合成方式 6
2.2.1固態反應(Solid State Reaction)法 6
2.2.2溶膠-凝膠反應(Sol-gel Reaction)法 7
2.2.3玻璃-陶瓷合成法 7
2.2.4加熟料合成堇青石文獻回顧 8
2.3 晶種效應 8
2.3.1成核成長 8
2.3.2 晶種效應的文獻 9
第三章 研究方法及步驟 16
3.1 實驗原料 16
3.1.1 原料性質 16
3.1.2晶種製作 16
3.2 實驗設計與方法 18
3.2.1 原料粉末製備 18
3.2.2 晶種粒徑對合成堇青石之影響 18
3.2.3 粉末熱處理 18
3.2.4 堇青石開始生成溫度 19
3.3 特性分析 19
3.3.1粒徑分佈 (Particle size distribution) 19
3.3.2粉末結晶相分析 (Phase Identification) 19
3.3.3熱差分析 (Differential thermal analysis) 19
3.3.4顯微結構分析 20
3.3.5各結晶相生成量之定量分析 20
第四章 結果與討論 24
4.1 由DTA比較晶種粒徑改變對合成堇青石影響 24
4.1.1高嶺石與滑石粉末之熱差分析 24
4.1.2 堇青石原料系統粉末熱差分析 24
4.1.3 原料系統與添加晶種後之熱差分析比較 25
4.1.4 高嶺石與滑石粉混合樣品(3K1T)及α-氧化鋁與滑石混合樣品(3A1T)添加晶種後之熱差分析 28
4.2 由XRD結晶相分析比較晶種粒徑改變對合成堇青石影響 36
4.2.1原料系統與添加晶種之結晶相分析 36
4.3 堇青石晶種影響能力分析 42
4.3.1 晶種與原料混合後粒體間的關係 42
4.3.2 堇青石開始生成溫度 44
4.3.3 高純相堇青石 46
第五章 結論 49
參考文獻 50
附錄A Raw material powder characteristcs 56
附錄B 高嶺石與滑石相關反應 62
附錄C 原料粒體間之計算 63

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