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研究生:陳宏嘉
研究生(外文):Hung-Chia Chen
論文名稱:燃燒合成法氮化鋁材料之傳統燒結與微波燒結研究
論文名稱(外文):Study of conventional sintering and microwave sintering with AlN material made by SHS method
指導教授:鍾賢龍
指導教授(外文):Shyan-Lung Chung
學位類別:碩士
校院名稱:國立成功大學
系所名稱:化學工程學系碩博士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
畢業學年度:90
語文別:中文
論文頁數:95
中文關鍵詞:微波燒結氮化鋁
外文關鍵詞:Microwave sinteringAlN
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  • 被引用被引用:7
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摘要
本研究採用燃燒合成法所得之氮化鋁粉體以微波及傳統高溫爐方式進行燒結,主要分為兩大部分:第一部分各以微波加熱及傳統加熱方式對添加碳酸鈣助劑之氮化鋁(SHS法合成)粉體進行燒結,並對此兩種不同燒結方式所得之燒結體作進一步分析、探討、比較;第二部分以微波加熱方式對添加氧化釔助劑之氮化鋁粉體進行燒結,並探討氧化釔添加量、燒結溫度、燒結時間及氮化鋁純度等對微波燒結體之影響。
以上兩部分研究除了對燒結體之密度、線性收縮率作初步分析外,另以X-ray繞射儀(XRD)、掃瞄式電子顯微鏡(SEM)、Holometrix Laser Flash Instrument熱傳導儀、穿透式電子顯微鏡(TEM)等儀器,對燒結體之顯微結構、晶相、熱傳導性等性質作進一步之分析、探討。實驗證實,微波燒結較傳統燒結有較快的燒結速率、較高的線性收縮率、較小的晶粒及較均勻顯微結構;而添加氧化釔5wt%於1800℃微波燒結30分鐘之燒結體線收縮率可達17.9%。此外原料粉體中之雜質含量多寡,為影響熱傳導值高低之主要因素。
Abstract
In this study, SHS-produced AlN powder was sintered by microwave heating method and conventional heating method. This study includes tow parts : The first part presents the comparison of AlN samples with CaCO3 as additives between sintered by microwave heating method and conventional heating method. The second part study the effect of additives, sintering times, temperature and purity of powder on AlN samples sintered by microwave heating method.
The density and linear shrinkage of the sintered bodies in two parts stated above were analyzed, then microstructure and second phase were characterized by XRD, SEM, TEM and HRAEM respectively. The thermal conductivity was measured by laser flash method.
The results of the experiments showed that the sintering rate and linear shrinkage of the sintered samples in microwave sintering are higher than ones in conventional sintering. And bodies by microwave sintering also possess relatively finer grain size and more uniform microstructure than ones in conventional sintering. Besides, AlN sample with 5wt% Y2O3 as additives and sintered at 1800℃for 30 minutes could reach a value of 17.9% of linear shrinkage, and the main factor influenced the thermal conductivity value was purity of raw powder.
總目錄

摘要 ………………………………………………… Ⅰ
Abstract …………………………………………… Ⅱ
誌謝 ………………………………………………… Ⅲ
總目錄 ……………………………………………… Ⅳ
表目錄 ……………………………………………… Ⅷ
圖目錄 ……………………………………………… Ⅸ
第一章 緒論
1-1引言 …………………………………………… 1
1-2 SHS簡介 ……………………………………… 2
1-3 氮化鋁的合成 ……………………………… 6
1-4 基版材料介紹 ……………………………… 9
1-5 前人研究 …………………………………… 10
1-6 研究目的及重點 …………………………… 11
第二章 理論基礎
2-1 微波加熱概論 ………………………… 13
2-1-1 何謂微波 ……………………… 13
2-1-2 微波爐的組成 …………………………… 14
2-1-3 微波加熱原理 …………………………… 14
2-1-4 微波加熱與傳統加熱的區別 …………… 15
2-1-5 微波加熱的特點 ………………………… 16
2-2 氮化鋁的特性 ……………………………… 17
2-3 熱傳導機構 ………………………………… 17
2-4 液相燒結 …………………………………… 20
2-5 液相燒結助劑選擇 ………………………… 22
第三章 實驗裝置和藥品
3-1 粉碎裝置 ……………………………… 27
3-2 研磨裝置 ……………………………… 27
3-3 常壓燒結裝置 ………………………… 27
3-4 微波燒結設備 ………………………… 27
3-5 其他設備 ……………………………… 28
3-6 藥品和氣體 …………………………… 29
第四章 實驗方法
4-1實驗原料與研磨 ……………………… 35
4-2 實驗流程 …………………………… 38
4-3 粉體性質分析 ………………………… 39
4-3-1 粒徑分析 ……………………… 39
4-3-2 氮含量與氧含量分析 ………… 39
4-3-3 比表面積分析 ………………… 39
4-3-4 不純物分析 …………………… 39
4-4 燒結生胚製作 ………………………… 40
4-4-1 燒結原料粉末 ………………… 40
4-4-2 原料調配 ……………………… 40
4-4-3 乾壓 …………………………… 40
4-5 鍛燒 …………………………………… 40
4-6 燒結 …………………………………… 41
4-6-1 常壓1850℃燒結 ……………… 41
4-6-2 微波燒結 ……………………… 42
4-7 燒結性質分析 ………………………… 43
4-7-1 微分熱分析(DTA) …………… 43
4-7-2 試片密度測量 ………………… 43
4-7-3 線收縮率(Linear Shrinkage) … 43
4-7-4 燒結收縮曲線 ………………… 44
4-7-5 熱傳導性………………………… 44
4-8晶相及微結構分析 …………………………… 44
4-8-1 XRD分析 …………………………………… 44
4-8-2 SEM分析 …………………………………… 45
4-8-3 EDS分析 …………………………………… 45
4-8-4 WDS分析 …………………………………… 45
4-8-5 TEM分析 …………………………………… 45
第五章 傳統常壓燒結與微波燒結之比較
5-1 添加碳酸鈣之微分熱分析(DTA) …… 47
5-2 密度比較 ……………………………… 48
5-3 線性收縮率比較 ……………………… 48
5-4 熱傳導值比較 ………………………… 51
5-5 XRD分析 ……………………………… 51
5-6微結構分析 ……………………………… 54
5-7 結論 …………………………………… 60
第六章 微波燒結實驗
6-1 燒結溫度、持溫時間與線性收縮率 …… 63
6-2 熱傳導值 ……………………………… 71
6-3 XRD分析 ……………………………… 73
6-4 微結構分析 …………………………… 73
6-5 結論 …………………………………… 92
參考文獻 ………………………………………… 93
自述 ……………………………………………… 98
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