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研究生：	劉益嘉 Liu, Yi-Chia
論文名稱：	燃燒合成氮化鋁粉體之量產製程開發 Process Development for Scale-Up Production of Aluminum Nitride Based on Combustion Synthesis
指導教授：	鍾賢龍 Chung, Shyan-Lung
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2011
畢業學年度：	99
語文別：	中文
論文頁數：	94
中文關鍵詞：	氮化鋁、燃燒合成法
外文關鍵詞：	Aluminum Nitride, Combustion synthesis
相關次數：	點閱：81 下載：0
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本實驗室研究以燃燒合成法製備氮化鋁粉體已相當久的時間，而其技術也相當純熟。而本論文研究為氮化鋁粉體之量產製程開發，自原本之每批次350g放大至1.4kg，再放大至3.5kg，探討製程方法與最佳操作條件。於每批次反應鋁粉為1.4kg之放大生產研究中，在最佳操作條件下，經鄂碎後小於100mesh之氮化鋁粉體其轉化率達99.5%以上，氧含量達0.40wt%以下。於每批次反應鋁粉為3.5kg之放大生產研究中，在最佳操作條件下，經鄂碎後小於100mesh之氮化鋁粉體其轉化率達99.7%以上，氧含量達0.45wt%以下。在市場的需求上，大多數氮化鋁粉體所需粒徑較小，因此本實驗研究亦探討將合成之粉體使用濕式研磨，磨至所需粒徑(D50=3~4μm、D50=1~2μm)，並依不同需求使用不同表面改質，使粉體擁有較好的抗濕效果，並使用恆溫恆濕測試、pH值測試氮化鋁粉體改質結果。

Conbustion synthesis methods for aluminum nitride powder have been developed in our labortary for many years, and several methods have been applicable for commercial production. In this thesis research, the author develops the process for scale-up production of AlN based on the combustion synthesis methods established in our labortary. In the case of using 1.4kg of Al powder for a batch, the conversion of the AlN powder which is under 100 mesh after crushing is higher than 99.5%, and the oxygen content is below 0.45wt% under the optimum operation condition. The particle size of AlN powder is usually required to be small in the current market. In this thesis research, the author also studies the milling of AlN so as to obtain the powder in the size range of D50=3~4μm and D50=1~2μm. In addition, surface treatment of the AlN powder to prevent hydrolysis was also performed during ball-milling process. Finally, the results of anti-hydrolysis is analysed by a constant temperature and humidity test and pH test.

摘要 ............................................ I
Abstract............................................... II
誌謝 ............................................ III
總目錄 .................................................. IV
表目錄 ................................................ VII
圖目錄 .......................................... IX
第一章 緒論 ............................................ 1
1-1 簡介陶瓷材料 ................................... 1
1-2 氮化鋁性質與應用 ................................. 1
1-3 氮化鋁合成方法 ................................... 4
1-4 簡介燃燒合成法 ...................................... 6
1-5 燃燒反應熱力學 ....................................... 8
1-6 燃燒反應動力學 ....................................... 11
1-7 燃燒合成氮化物 ...................................... 12
1-8 氣相反應成核 ....................................... 15
1-8-1 均勻相成核(Homogeneous nucleation) ................. 15
1-8-2 異質相成核(Heterogeneous nucleation) ............... 16
1-9 研究動機 ........................................... 18
第二章 實驗室裝置與藥品 ................................... 20
2-1 大型反應器裝置 ....................................... 20
2-2 大型研磨機裝置 ....................................... 20
2-3 分析儀器 ........................................... 21
2-4 其他儀器設備 ........................................ 22
2-5 藥品 ............................................. 23
第三章 實驗方法 .......................................... 26
3-1 氮化鋁量產製程開發 .............................. 26
3-1-1 製備反應錠 ............................. 26
3-1-1-1 1.4kg 級反應錠 ............................ 26
3-1-1-2 3.5kg 級反應錠 ........................... 26
3-1-2 燃燒合成反應之進行 .............................. 27
3-1-2-1 1.4kg 級反應錠燃燒合成反應之進行 .................. 27
3-1-2-2 3.5kg 級反應錠燃燒合成反應之進行 ................... 28
3-1-3 產物轉化率測詴 ........................... 30
3-1-3-1 原理 ................................ 30
3-1-3-2 實驗步驟 ................................ 30
3-1-3-3 轉化率計算 ........................... 30
3-2 氮化鋁細磨技術建立以及抗濕處理 ...................... 32
3-2-1 研磨前準備 ......................... 32
3-2-2 研磨流程 ............................ 32
3-2-3 研磨後粉體性質測詴 ................................ 33
3-2-3-1 粒徑分析 ........................... 33
3-2-3-2 氮氧分析 .............................. 33
3-2-3-3 恆溫恆濕測詴 ............................ 33
3-2-3-4 純水中pH 值測詴 .............................. 34
第四章 結果與討論 .................................. 35
4-1 實驗結果與討論 .................................. 35
4-2 氮化鋁量產製程開發 .............................. 35
4-2-1 1.4kg 級反應錠 ................................. 38
4-2-1-1 改變反應時氮氣錶壓 ................................ 38
4-2-1-2 改變雙層反應碇外層添加劑量 ...................... 43
4-2-1-3 改變雙層反應碇外層稀釋劑 ........................... 47
4-2-1-4 雙層反應碇外層添加劑與稀釋劑綜合效應 ......... 50
4-2-1-5 1.4kg 級反應錠最佳條件 ....................... 53
4-2-2 3.5kg 級反應錠與最佳條件 ............................ 55
4-3 氮化鋁細磨技術建立以及抗濕處理 ........................ 60
4-3-1 探討氧含量上升原因 .................................. 61
4-3-2 氮化鋁抗濕處理 ............................... 63
4-3-3 氮化鋁細磨技術結果以及抗濕結果 ..................... 64
4-3-3-1 粒徑D50=3~4μm、ABS 改質 ...................... 64
4-3-3-2 粒徑D50=3~4μm、硬酯酸改質....................... 69
4-3-3-3 粒徑D50=1~2μm、ABS 改質 ....................... 75
4-3-3-4 粒徑D50=1~2μm、硬酯酸改質..................... 79
4-4 成本估算 ......................................... 84
第五章 結論 ........................................... 87
參考文獻 ........................... 89
自述 .................................................. 94
                                    

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