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研究生: 陳文儀
論文名稱: 陰離子型共聚物的合成及應用於鈦酸鋇漿體的分散
指導教授: 許貫中
學位類別: 碩士
Master
系所名稱: 化學系
Department of Chemistry
論文出版年: 2008
畢業學年度: 96
語文別: 中文
中文關鍵詞: 鈦酸鋇分散劑合成
論文種類: 學術論文
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  • 鈦酸鋇是一種高介電常數的陶瓷粉體,為積層陶瓷電容器的關鍵原料。在鈦酸鋇電子陶瓷的製程中,要得到穩定性高且分散良好的漿體,必須添加分散劑。本篇論文合成一種陰離子型共聚物,並探討其對於鈦酸鋇水系漿體分散性質的影響。首先,在鹼性環境下,利用自由基聚合反應,合成出相同分子量,不同單體比例的共聚物poly(methacrylic acid-co-methacrylamide-co-(b-carboxylate(hydroxyl acrylic polyethylester))) (PMAMC),並以1H-NMR及FT-IR確認聚合物的結構,以GPC測定其分子量,使用電位滴定儀測量共聚物含羧基比例及其解離率。其次,探討這兩種共聚物對鈦酸鋇水系漿體分散性的影響,研究方法有流變行為、沈降體積及粒徑分佈的測試,並利用界達電位及吸附量等實驗結果來解釋,另外,利用ICP-MS來測量鈦酸鋇漿體中鋇離子的溶出量。研究結果顯示添加這兩種共聚物皆能使鈦酸鋇漿體穩定,而其中又以添加PMAMC 1分散效果最佳。相對於PMAMC 0,添加PMAMC 1對於漿體中電解質濃度的變化較無影響,因為PMAMC 1帶有長側鏈CHAP。最後,添加共聚物PMAMC皆能抑制鋇離子溶出。
    關鍵字:鈦酸鋇、共聚物、合成、分散、鋇離子溶出

    摘 要 I ABSTRACT II 目錄 III 圖目錄 VI 表目錄 IX 第一章 緒論 1 1-1 研究背景 1 1-2 研究目的 2 第二章 文獻回顧 3 2-1 鈦酸鋇粉末之簡介 3 2-1-1 鈦酸鋇之基本性質 3 2-1-2鈦酸鋇粉末之相圖及結構 3 2-2 粒子的特性 4 2-3 粒子之聚沉 (AGGLOMERATION)與絮凝 (FLOCCULATION) 4 2-4 粒子間的作用力 5 2-5 分散機制 7 2-5-1 靜電排斥穩定 (Electrostatic stabilization) 7 2-5-2 立體阻障穩定 (Steric stabilization) 8 2-6 漿體系統的流變性質 9 2-6-1 漿體系統之流變學模型 9 2-6-2 粒子間作用力對漿體系統流變行為之影響 10 2-7 分散劑在粉體表面的吸附行為 11 2-7-1 Langmuir吸附等溫式 11 2-7-2 分散劑的吸附構形及厚度 12 2-8 粉體的表面電荷與界達電位 (-POTENTIAL) 14 2-8-1 粒子表面電荷的來源 14 2-8-2界達電位 (-potential) 14 2-9 鋇離子溶出 15 2-10分散劑應用於陶瓷材料之文獻探討 16 2-10-1黏度與沉降實驗 16 2-10-2 吸附實驗 19 2-10-3 分散劑種類 23 2-11 漿體分散效果的評估 24 2-11-1 流變性質 24 2-11-2吸附行為 25 2-11-3 界達電位 25 2-11-4 粒徑分佈 25 2-11-5 沉降體積 26 第三章 實驗流程與測量原理分析 42 3-1 實驗流程 42 3-2 實驗方法 42 3-2-1 陰離子型共聚物PMAMC之合成 42 3-2-2 陰離子型共聚物PAAMA之合成 42 3-2-3 共聚物之結構鑑定與性質分析 43 3-2-4 鈦酸鋇材料之晶相分析 43 3-2-5 共聚物對鈦酸鋇漿體之分散效果分析 43 3-3 實驗材料與實驗設備 43 3-3-1 鈦酸鋇 (BT)粉末: 43 3-3-2 藥品: 44 3-3-3 實驗設備 45 3-4 共聚物之合成 46 3-4-1 單體CHAP (β-carboxylate(hydroxyl acrylic polyethylester )) 之合成 46 3-4-2 共聚物PMAMC (Poly Methacrylic acid-co-Methacrylamide-co-(β-carboxylate(hydroxyl acrylic polyethylester)))及PAAMA (Poly Methacrylic acid-co-Methacrylamide) 之合成 47 3-5 鈦酸鋇粉末晶相分析 48 3-6 高分子結構鑑定及性質分析 49 3-6-1 共聚物固含量測量 49 3-6-2 凝膠滲透層析 (GPC)分析 49 3-6-3 紅外線 (IR)光譜分析 50 3-6-4 核磁共振 (NMR)光譜分析 51 3-6-5 共聚物解離率的量測 52 3-7 共聚物對鈦酸鋇漿體之分散性質分析 52 3-7-1 鈦酸鋇漿體的配製 52 3-7-2 鈦酸鋇漿體之流變性質的量測 52 3-7-3 共聚物之吸附量的量測 53 3-7-4 粒子界達電位的量測 53 3-7-5 粒子粒徑分佈的量測 53 3-7-6 沉降體積的量測 54 3-7-7 胚體密度的量測 54 3-7-7.1 生胚密度 54 3-7-7.2 燒結密度 55 3-7-8 鋇離子溶出量 55 3-7-9 微結構分析 56 第四章 共聚物之性質分析 60 4-1 聚合物之結構分析 60 4-1-1 PMAMC單體CHAP之結構鑑定 60 4-1-2 共聚物PMAMC以及PAAMA之結構鑑定 60 4-2 共聚物之分子量 61 4-3 共聚物之羧基比例與解離率 62 4-3-1 共聚物之解離率 62 4-3-2 共聚物之羧基比例 62 第五章 結果與討論 71 5-1 鈦酸鋇粒子在水中的解離 71 5-2 共聚物對鈦酸鋇漿體吸附行為之影響 71 5-3 共聚物對鈦酸鋇漿體流變行為之影響 75 5-4 共聚物對鈦酸鋇漿體界達電位 (-POTENTIAL)之影響 77 5-4-1各共聚物對鈦酸鋇漿體界達電位的影響 78 5-4-2 pH值對鈦酸鋇粒子界達電位的影響 78 5-5 共聚物對鈦酸鋇漿體粒徑大小及分佈之影響 79 5-5-1 共聚物對鈦酸鋇漿體粒徑大小的影響 80 5-5-2 共聚物對鈦酸鋇漿體粒徑分佈的影響 80 5-6 共聚物對鈦酸鋇漿體沉降體積之影響 81 5-6-1 PMAMC及PAAMA對鈦酸鋇漿體沉降體積的影響 81 5-6-2 PMAAN對鈦酸鋇漿體沉降體積的影響 82 5-7 共聚物對鈦酸鋇胚體密度之影響 82 5-7-1 共聚物對鈦酸鋇生胚密度的影響 83 5-7-2 共聚物對鈦酸鋇燒結密度的影響 84 5-8 共聚物對鈦酸鋇微結構之影響 84 5-9 共聚物對鈦酸鋇漿體鋇離子溶出之影響 85 第六章 結論 109 參考文獻 111

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