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研究生: 朱霆恩
Chu, Ting-En
論文名稱: 氮化鋁燃燒合成技術製程開發
Process Development on Combustion Synthesis of Aluminum Nitride
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: 2021
畢業學年度: 109
語文別: 中文
論文頁數: 139
中文關鍵詞: 氮化鋁燃燒合成法
外文關鍵詞: aluminum nitride, combustion synthesis method
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  • 本實驗室研究以自蔓延高溫燃燒合成法製備氮化鋁已有相當長的時間。此方法之可行性與鋁粉形態有密切相關,先前實驗室所用之鋁粉主要為片狀鋁粉,經過實驗室過去多年開發後,目前已可以使用片狀鋁粉進行燃燒合成並且能穩定生產產物量級至少5 kg級且轉化率達99.9%的氮化鋁。然而,由於此種鋁粉價格較高,不利於工業化生產,為使開發出來的氮化鋁合成技術能夠應用於工業化生產,必須使用低價位鋁粉開發氮化鋁合成技術,以達到降低成本之目的。緣此,本論文研究係以開發低成本鋁粉燃燒合成氮化鋁為目標。吾人選用低價位球形鋁粉進行燃燒合成製程開發,且參考過先前學長們的實驗結果,探討先前本實驗量產開發所遭遇的問題並提出解決方案而能達到6 kg級量產開發。在使用球形鋁粉合成氮化鋁之實驗中發現,要能進行燃燒合成反應,不僅引燃能量必須提升且需穩定供應熱源,另一關鍵的問題是鋁粉本身的堆積密度。基於此,本論文研究使用兩種鋁粉相混以有效地改善球形鋁粉本身高堆積密度的特性,本論文研究因而解決了球形鋁粉本身難以引燃且反應容易中斷的問題,並提升產物量級至6 kg級,產物之整體轉化率為99.08%,產率為99.17%。在本論文研究中,吾人也另外找尋了一種價格低廉且較低堆積密度的球形鋁粉,並進行量產製程開發,已可穩定將產物量級提升至6 kg級,且藉由改變壓力、加入添加劑等方法,提高量產級產物之轉化率,在8 atm下6 kg級產物整體轉化率99.29%,產率為99.01%。

    In our laboratory, we have studied the preparation of aluminum nitride by self-propagating high-temperature combustion synthesis for a long time. The feasibility of this method is closely related to the shape of the aluminum powder. The aluminum powder used in the past was mainly flake aluminum powder. After few years of development in the laboratory, the flake aluminum powder can now be used for SHS combustion synthesis and stably produce aluminum nitride with a product level of at least 5 kg and a product conversion rate of 99.9%. However, due to the high price of such aluminum powder, it is not advantageous for industrial production. In order to make the aluminum nitride synthesized by combustion be used to industrial production, it is necessary to use low-priced aluminum powder to develop aluminum nitride synthesis technology to reduce costs. For this reason, the research of this thesis aims to develop for using low-cost aluminum powder to synthesized aluminum nitride. We use low-cost spherical aluminum powder for combustion synthesis process development, and refer to the experimental results of seniors, and discuss the problems in the previous mass production development, and propose solution, then we can achieve 6kg mass production development. In the experiment of using spherical aluminum powder to synthesize aluminum nitride, it was found that the combustion synthesis reaction is able to carry out, not only the ignition energy must be increased and the heat source must be stably supplied but the key is the bulk density of the aluminum powder itself. Based on this conclusion, the research uses two types of aluminum powder to mix together, then can effectively decrease the high bulk density of the spherical aluminum powder itself. This method solves the problem that I have mentioned above and also improves the product level of 6 kg, and the overall conversion rate of the product is 99.08%, and the yield rate is 99.17%. In this study, I also searched for a low-cost and low bulk density spherical aluminum powder, and developed the mass production process, which can stably achieve the product level of 6kg. Changing the pressure, adding additives and other methods in the combustion synthesis process can improve the conversion rate of mass-produced products. The overall conversion rate of 6 kg-level products at 8 atm is 99.29%, and the yield of the product is 99.01%.

    第一章 緒論 1 1-1簡述陶瓷材料 1 1-2氮化鋁性質與應用 2 1-3目前氮化鋁主要的製備方法 5 第二章 原理及文獻回顧 8 2-1燃燒合成法(COMBUSTION SYNTHESIS) 8 2-2 燃燒反應熱力學之分析 10 2-3 燃燒反應動力學之分析 13 2-4 燃燒合成氮化物 14 2-5 反應物孔隙度及壓力對燃燒合成反應的影響 18 2-6 氣相反應成核 20 2-7研究動機 23 第三章 實驗裝置儀器與藥品 25 3-1小型反應器裝置 25 3-2 大型反應器裝置 27 3-3 量產反應器裝置 28 3-4 分析儀器 29 3-5 其他儀器設備 31 3-6 藥品 32 第四章 實驗方法 34 4-1 反應錠製備流程 36 4-1-1 小型反應錠(小型坩堝) 36 4-1-2 大型反應錠(中形坩堝) 36 4-1-3 試量產反應錠(大型坩堝) 36 4-2 燃燒合成的反應步驟 37 4-3 氮化鋁產物之轉化率分析 39 4-4 氮化鋁產物之後處理 41 第五章 結果與討論 42 5-1 以遠洋20μm球形鋁粉進行氮化鋁燃燒合成 42 5-1-1以遠洋20μm球形鋁粉燃燒合成 42 5-1-2量產製程失敗原因及改善 45 5-1-3遠洋20μm球形鋁粉上層鋪Ecka不規則鋁粉量產製程 46 5-1-4 引燃能量問題-鎢絲 52 5-1-5氮化鋁量產製程改善-改變堆積密度 62 5-1-6氮化鋁量產製程改善-使用混粉改變堆積密度(彤杉32μm片狀鋁粉) 67 5-1-7氮化鋁量產製程改善-使用混粉改變堆積密度(宏泰30μm片狀鋁粉) 76 5-2 以金昊1-2μm球形鋁粉進行氮化鋁燃燒合成 83 5-2-1金昊1-2μm球形鋁粉燃燒合成製程-添加劑對產物影響 83 5-2-2金昊1-2μm球形鋁粉-均混疊氮化鈉 84 5-2-3金昊1-2μm球形鋁粉-均混氯化銨 87 5-2-4金昊1-2μm球形鋁粉-均混尿素 89 5-2-5氮化鋁量產製程開發-金昊1-2μm球形鋁粉 92 5-2-6金昊1-2μm球形鋁粉-嘗試改變壓力 98 5-2-7探討未加添加劑金昊1-2μm球形鋁粉然情況 104 5-2-8金昊1-2μm球形鋁粉-嘗試加入添加劑 105 5-2-9改善堆積密度-金昊1-2μm球形鋁粉與彤杉32μm片狀鋁粉 116 5-2-10改善堆積密度-金昊1-2μm球形鋁粉與宏泰30μm片狀鋁粉 120 5-3 比較產物形貌差異 124 5-4 目前不同球形鋁粉生成氮化鋁最大量級燃燒條件及最佳燃燒條件 129 5-4-1不同球形鋁粉生成氮化鋁之最大量級燃燒條件 129 5-4-2不同球形鋁粉生成氮化鋁之最佳燃燒條件 129 第六章 結論 132 第七章 參考文獻 136

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