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研究生： 吳杏旋
論文名稱： 添加陰離子型分散劑之鈦酸鋇漿體在不同pH值下的分散行為
指導教授： 許貫中
Hsu, Kung-Chung
學位類別： 碩士
Master
系所名稱： 化學系
Department of Chemistry
論文出版年： 2004
畢業學年度： 92
語文別： 中文
論文頁數： 165
中文關鍵詞： 鈦酸鋇 、分散劑 、pH 、分散性質
英文關鍵詞： BaTiO3, dispersant, pH, properties
論文種類： 學術論文
相關次數： 點閱：423  下載：18 
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    • 本研究主要是延續實驗室所研發出來的陰離子型分散劑PCOB poly〔(4-carboxyamino-4-oxo-2-butenate)-acrylamide〕，與商用型之甲基丙烯酸鈉鹽PMAA-Na〔sodium salt of poly(methacrylic acid)〕應用於鈦酸鋇粉末探討在不同pH值之分散效果，其中PCOB係以馬來酸酐和氨基甲酸銨鹽反應生成4-羧基氨基-4酮基-2-丁烯酸銨鹽單體，再與丙烯醯胺經自由基聚合反應而得。所得之PCOB以H1-NMR及FTIR確認其結構並利用GPC測定其分子量。
    而評估添加分散劑對於鈦酸鋇漿體穩定性的影響，主要方法有黏度，沈降體積，粒徑分佈，並利用高分子之解離率，表面電位，及吸附量來加以解釋，且利用ICP-MASS來測量Ba2+的溶出量，實驗發現添加PCOB能減少鋇離子的溶出，因為PCOB吸附量較PMAA-Na多，且PCOB擁有兩個羧基可以吸附較多鋇離子。由黏度實驗、沈降實驗及粒徑分佈發現添加PCOB能穩定鈦酸鋇漿體，其分散效果可和PMAA-Na相當，且隨著pH值越高，所需要的漿體穩定劑量越少。另外胚體在經過壓胚、燒結後，發現其密度及介電常數均較PMAA-Na高，顯示PCOB確實能有效分散鈦酸鋇漿體。
    實驗結果顯示鈦酸鋇漿體在pH=7、9、12時，對於漿體之穩定皆存在一飽和劑量，在此劑量以上，漿體可維持良好之分散，且隨著pH值增加，達到穩定分散所需之飽合劑量越少，即在pH值較高時，僅需較少量之分散劑即可使漿體達到良好之分散。

    This study continues the research and development of an anionic water-soluble copolymer,poly〔(4-carboxyamino-4-oxo-2-butenate) acrylamide〕(PCOB),which was copmared with PMAA-Na〔sodium salt of poly(methacrylic acid)〕and applied to BaTiO3 powder at different pH to characterise the dispersive ability. PCOB was prepared from 4-carboxyamino- 4-oxo-2-butenate and acrylamide through a free radical copolymerization.4-carboxy
    amino-4-oxo-2-butenate was made by reacting maleic anhydride with ammonium carbamate. The chemical structure of PCOB were verified from their H1-NMR and FTIR spectra.,and the molecular weight of PCOB was measured by GPC.
    The dispersion ability of PCOB on aqueous BaTiO3 slurries was evaluated from viscosity, sedimentation volume , particle size distribution, and dissussed by using the dissociation of PCOB ,zeta potential of particles, and adsorption of PCOB onto particles.Also, the amount of leached Ba2+ ion from BaTiO3 to slurry was measured.The result shows that PCOB causes less Ba2+ ion dissolved into solution.,because greater amount of PCOB adsorbed on BaTiO3 particles.From the experimental results
    of viscosity, sediment volume, and particle size distribution, added PCOB was found to be effective in making a stable BaTiO3 slurry.The dispersion effect is similar to PMAA-Na. The amount of PCOB or PMAA-Na required to stabilize aqueous BaTiO3 suspensions are decreased with increasing pH.
    Finally, the sintered parts with PCOB exhibits higher density and dielectric constant than those with PMAA-Na.
    Experimental results exhibit BaTiO3 slurries with pH=7,9,12,have a appropriate amount of dispersant for stabilize
    aqueous BaTiO3 suspensions,above the point ,slurry can maintain
    well dispersion. When the pH value is higher,less amount of dispersant that can making BaTiO3 slurry stable.

    第一章 緒論……………………………………………………………..1 第二章 文獻回顧………………………………………………………..3 2-1鈦酸鋇粉末的合成…………………………………………………..3 2-2粉體分散系統穩定性分析之文獻探討……………………………..7 2-3鈦酸鋇微結構與電性的研究……………………………………….17 2-4分散原理...............................................21 2-4-1粒子的特性……………………………………………………...21 2-4-2膠體粒子間表面作用力的形式…………...................23 2-4-3分散機構………………………………………………………...25 2-5電雙層理論………………………………………………………….33 2-6分散效果之評估方法……………………………………………….35 2-6-1粒子的沈降方式………………………………………………...35 2-6-2沈降法的原理…………………………………………………...36 2-6-3分散系統的流變性質…………………………………………...38 2-7有機分子對粒子表面的吸附行為及吸附等溫線………………….41 第三章高分子的合成與鑑定………………………………………....44 3-1前言………………………………………………………………….44 3-2高分子的合成……………………………………………………….44 3-2-1實驗藥品和儀器設備…………………………………………...44 3-2-2實驗步驟………………………………………………………...46 3-3核磁共振(NMR)光譜分析……………………………………......47 3-4紅外線(IR)光譜分析……………………………………………….48 3-5分子量的評估……………………………………………………….48 3-6 PCOB之固含量測定………………………………………………..49 3-7結果與討論………………………………………………………….50 3-7-1高分子結構鑑定………………………………………………...50 3-7-2分子量的量測…………………………………………………...50 3-7-3固含量的量測…………………………………………………...51 第四章BaTiO3粒子分散效果評估……………………………………..56 4-1前言………………………………………………………………...56 4-2實驗評估…………………………………………………………….57 4-2-1藥品與儀器設備………………………………………………...57 4-2-2實驗材料………………………………………………………...58 4-3實驗製程…………………………………………………………….58 4-3-1漿體的製備……………………………………………………...58 4-3-2燒結體的製備…………………………………………………...58 4-4性質分析…………………………………………………………….59 4-4-1 X光粉末繞射(XRD)分析………………………………………..59 4-4-2分散劑解離率的量測…………………………………………...59 4-4-3黏度量測………………………………………………………...59 4-4-4沈降高度………………………………………………………...60 4-4-5粒徑分佈………………………………………………………...60 4-4-6表面電位………………………………………………………...60 4-4-7吸附量…………………………………………………………...61 4-4-8鋇離子溶出量…………………………………………………...61 4-4-9胚體密度………………………………………………………...62 4-4-10介電常數與介電損失…………………………………………..63 4-4-11微結構分析..........................................64 第五章 鈦酸鋇之分散行為結果與討論……………………………..69 5-1鈦酸鋇在水中的解離……………………………………………….69 5-2分散劑在水中的解離率…………………………………………….72 5-3鈦酸鋇漿體的黏度………………………………………………….76 5-4鈦酸鋇漿體的粒徑分佈…………………………………………….81 5-5鈦酸鋇粒子的表面電位…………………………………………….89 5-6 鈦酸鋇粒子的沈降………………………………………………..94 5-7分散劑在鈦酸鋇粒子上的吸附…………………………………..103 5-8鈦酸鋇漿體之Ba2+溶出量………………………………………..113 5-9鈦酸鋇胚體的密度………………………………………………..118 5-10鈦酸鋇胚體的之電性…………………………………………….123 5-11鈦酸鋇胚體的微結構分析……………………………………….129 5-12鈦酸鋇與PCOB及PMAA-Na系統之凝膠穩定圖……………......148 第六章 結論………………………………………………………….150 第七章 參考資料…………………………………………………….152

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