臺灣博碩士論文加值系統

一般硫酸鋁銨法採用直接煅燒製程，雖可製備高純度氧化鋁粉末，但是不易獲得奈米級氧化鋁粉末。本研究採用改良式硫酸鋁銨法，先以硫酸鋁銨法製備高純度硫酸鋁銨，按配比調製成溶液後，再以噴霧熱解製程製作奈米級氧化鋁粉末，其中以硫酸鋁銨溶液流量3.0 ml/min、載氣流量4L/min有較佳的類球型實心顆粒，且氧化鋁粉體粒徑在0.3~0.5μm之間，其性能雖佳，但生產效率低，不利於工業化量產。
因此本研究另以添加PEG及氣氛煅燒的方式製備氧化鋁粉末，以避免氧化鋁在¬θ-Al2O3 →α-Al2O3相轉換時的指狀成長及團聚現象，獲得晶粒細微的氧化鋁粉末。本研究先將高純度硫酸鋁銨煅燒成δ-Al2O3，再加入PEG作為阻隔氧化鋁團聚的介質，來抑制氧化鋁煅燒時產生的指狀生長及團聚現象；但是PEG在高溫環境下會氧化燒失，故本研究特別以氮氣氣氛進行高溫煅燒，避免PEG的燒失；添加PEG的δ-Al2O3是在氮氣氛下升溫至1250℃煅燒2hr，再將溫度降至900℃，通入空氣進行有氧煅燒，燒除PEG介質，獲得兼具高純度且易燒結之氧化鋁微粉，其平均粒徑約0.3μm，團聚現象大幅減少；TEM微觀結構顯示，α-Al2O3周邊有微量θ-Al2O3殘留，未完全轉換為α-Al2O3，由此推斷添加PEG分散劑會阻隔Al2O3的團聚並抑制其晶粒成長，使θ-Al2O3 →α-Al2O3的相轉換延遲。

Aluminum ammonium sulfate method is conventionally applied to direct heating. It can obtain high purity of alumina powder, but it is not easy to obtain nanoscale alumina powders. In this study, we used modified aluminum ammonium sulfate method. Firstly, we prepared high-purity aluminum ammonium sulfate, and then dissolve it into solution with a specific ratio. Next, we used spray pyrolysis process making nanoscale alumina powders. The flow rate of a solution of aluminum ammonium sulfate is 3.0 ml/min and the flow rate of a carrier gas is 4L/min for obtaining better spherical solid particles. The size of alumina powder particles is between 0.3~0.5μm. Although it shows good performance, its productivity is pretty low, which is not suitable for industrialization.
Therefore, in this study, we added PEG and nitrogen gas to prepare alumina powders in a manner to avoid finger growth and agglomeration at θ-Al2O3 → α-Al2O3 phase transformation. We first heated high-purity aluminum ammonium sulfate into δ-Al2O3, then added PEG as a medium to block agglomeration of alumina powder, in order to suppress finger growth and agglomeration. However, PEG suffers oxidizing loss at a high temperature. Thus, we added in nitrogen gas to prevent the loss of PEG. δ-Al2O3 with PEG is heated at 1250 ℃ for 2hr under nitrogen gas. Then the temperature was lowered to 900 ℃ with air to remove the entire PEG medium. Using this method, we can obtain high purity of alumina powder with an average particle size of about 0.3μm, reducing agglomeration significantly. The TEM microstructures display that α-Al2O3 is surrounded by trace θ-Al2O3 residue, which is not completely converted into α-Al2O3. We concluded that adding PEG will block agglomeration of Al2O3, inhibit particle growth, and delay θ-Al2O3 → α-Al2O3 phase transition.

誌謝 i
摘要 ii
Abstract iii
目錄 v
表目錄 viii

圖目錄 ix
第一章 緒論 1
1-1 研究背景 1

1-2 研究動機 3

1-3 研究目的 5
第二章 理論基礎與文獻回顧 7
2-1 文獻探討 7
2-1-1高純度氧化鋁粉體的製備方法 7
2-2 噴霧熱解法的特性 11
2-2-1噴霧熱解法的製程 11
2-2-2噴霧熱解法的影響因素 12
2-3噴霧熱解中形成的各種顆粒和外觀 15
2-3-1實心球形顆粒 15
2-3-2 方形顆粒 16
2-3-3環形顆粒 17
2-3-4 蜂巢狀顆粒和高爾夫球狀顆粒 18
2-3-5 泡沫狀顆粒 19
2-3-6 針狀顆粒和塊狀顆粒 20
2-3-7 多孔球形顆粒 21
2-3-8 空心球狀顆粒 22
2-3-9 破損的球殼形顆粒 22
2-3-10 碎片狀顆粒 23
2-3-11 瓶子狀顆粒 24
2-4燒結方式與燒結理論 25
2-4-1真空與氣氛燒結 25
2-5-2真空燒結原理 26
2-5-3氣氛燒結原理 26
2-5-4燒結理論 27
第三章 實驗方法 31
3-1 硫酸鋁銨暨噴霧熱解法實驗 31
3-1-1硫酸鋁銨暨噴霧熱解法實驗流程 31
3-1-2無塵手套箱之建置 33
3-1-3硫酸鋁銨暨噴霧熱解法實驗步驟 37
3-2 改良式硫酸鋁銨法實驗 44
3-2-1改良式硫酸鋁銨法實驗流程 44
第四章 結果與討論 46
4-1 參數條件對硫酸鋁銨性質之影響 46
4-1-1硫酸鋁銨溶解再結晶之產率 46
4-2 噴霧製成對粉粒型態的影響 49
4-2-1氧化鋁粉粒之型態 49
4-2-2 不同硫酸鋁銨溶液流量的影響 50
4-2-3不同載氣流量 51
4-3 熱處理條件對高純度氧化鋁微粉的性質影響 52
4-3-1硫酸鋁銨之熱行為與礦物相 52
4-3-2高純度氧化鋁粉末之微結構與化學組成分析 53
4-3-3 不同煅燒溫度之高純度氧化鋁的性質差異 56
4-4 添加PEG對高純度氧化鋁微粉性質影響 60
4-4-1 添加不同比例之PEG對高純度氧化鋁的影響 60
4-5 影響奈米氧化鋁粉末凝聚的因素 66
4-5-1 凝聚現象 66
4-5-2 純度 66
4-5-3 表面能 67
第五章 結論 69
參考文獻 70

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