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研究生: 王盟強
Wang, Meng-chiang
論文名稱: pH值對以θ-Al2O3/boehmite水性漿料系統製備< 100 nm α-Al2O3之影響
pH Impact of Nano-Structural Processing on < 100 nm Alpha-Alumina Particle Fabrication
指導教授: 顏富士
Yen, Fu-su
學位類別: 碩士
Master
系所名稱: 工學院 - 資源工程學系
Department of Resources Engineering
論文出版年: 2008
畢業學年度: 96
語文別: 中文
論文頁數: 69
中文關鍵詞: pH值調整凝聚體
外文關鍵詞: pH value adjusting, agglomerate
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  • 本研究探討θ-Al2O3/boehmite混合水系漿料系統,因其pH值不同可能形成的θ-Al2O3/boehmite凝聚狀態差異,可致以其乾膠熱處理所得之α-Al2O3粒體特性也不同。使用之θ-Al2O3/boehmite原料重量比固定為30對82.35(Al2O3/Al2O3=30/70)。混合後漿料固粒含量為20 wt%。兩成分的混合採取兩種方式:系統A是先將二者分散良好(pH=4)再混合,再調整為不同的pH漿料系統。系統B則將兩成分各調整至預定相同pH後再混合。混好樣品均以DTA觀察系統粉末之熱行為,瞭解其α-Al2O3出現溫度。利用XRD、BET、TEM等儀器進行所得煆燒樣品之特性分析。
    研究結果顯示:混合系統(A、B)均會隨pH升高而有較大凝聚體產生且θ-到α-Al2O3的相轉換溫度有隨pH值升高而延後發生的現象。兩種方式均有可能形成類似core(θ-Al2O3)–shell(boehmite)之結構。二者因pH值不同產生的最大差異在於A系統可造成相近的θ-Al2O3/boehmite分佈關係,凝聚體粒子間距離雖改變,但core-shell的質量不變,因此對於所得到的α-Al2O3粒子也因此差異不大。B系統則因二成分已先作凝聚狀態的改變,當進入混合形成core-shell時,θ-Al2O3凝聚體大者會導致core-shell顆數的減少,每顆質量變大。結果可知B系統透過pH調整,可對所得之α-Al2O3粉末晶徑進行調整。

    In this study, the mixed slurries of θ-Al2O3 and boehmite may be different in the agglomeration by pH value adjusting. The characterizations of α-Al2O3 were further different by calcining the mixed slurries of θ-Al2O3 and boehmite. The alumina ratio of θ-Al2O3 to boehmite was 30 to70.The solid contain of θ-Al2O3 and boehmite were 20 wt%. There were two ways to mix. First, pH value of A system adjusted after two dispersal materials mixing. Second, two materials mixed after two materials adjusting pH value variously. The thermal behavior of the samples, which were from the mixed slurries, was examined by differential thermal analysis (DTA). The characterizations of α-Al2O3, which were form the mixed slurries, were examined by XRD、BET、TEM analysis.
    The results showed that: A、B systems both arise larger agglomerates and lead to a higher transformation temperature when pH value is higher. This two ways may both bulid homo-core(θ-Al2O3)-shell(boehmite) structure. Although the agglomeration has changed, the mass of core-shell was in the same which caused the size of α-Al2O3 constant in A system. Contrarily, because the two components had changed in the agglomeration, the larger agglomerate of θ-Al2O3 caused the number of core-shell lower and the mass of core-shell biger. Finally, the size of α-Al2O3 could be altered via pH adjusting in B system.

    摘要 I Abstract...II 誌謝...III 表目錄 VI 圖目錄 VII 第一章 緒論 1 1.1 前言 1 1.2 研究動機與目的 2 第二章 理論基礎與前人研究 3 2.1 氧化鋁的過渡相 3 2.1.1 Boehmite的結晶相 3 2.1.2 θ-Al2O3的結晶相 3 2.2 α-Al2O3的結晶相 3 2.3 θ-→α-Al2O3相轉換 4 2.4 粉體之分散與凝聚 11 2.5 凝聚體的成長過程 15 2.6 θ-Al2O3/boehmite系統相關前人研究 15 第三章 實驗步驟及方法 17 3.1 實驗構想與設計 17 3.2 實驗原料 20 3.2.1 θ-Al2O3 20 3.2.2 boehmite 20 3.3 實驗步驟與流程 25 3.4 特性分析 27 3.4.1 粉末結晶相分析 27 3.4.2 熱差分析 27 3.4.3 晶徑及粒徑分析 27 3.4.4 α-生成量定量分析 28 3.4.5 粒徑分佈量測 29 3.4.6 顯微影像及結構分析 29 第四章 結果與討論 31 4.1 pH值對θ-Al2O3/boehmite系統之影響 31 4.1.1 θ-Al2O3 31 4.1.2 boehmite 31 4.1.3 θ-Al2O3/boehmite混合系統 32 4.2 混合粉末之熱行為 41 4.3 α-粒子的觀察 45 4.3.1 α-Al2O3粒子的尺寸 45 4.3.2 α-Al2O3之TEM觀察 46 4.4 綜合討論 54 第五章 結論 56 參考文獻 57 Appendices 61 自述 69

    1. T. G. Peason, “The Chemical Background of the Aluminum Industry”,
    Monograph of the Royal Institute of Chemistry, London, 1995.
    2. 汪建民,陶瓷技術手冊 ( 下),中華民國粉末冶金協會,中華民國 83 年。
    3. R. W. Siegel, S. Ramasamy, H. Hahn, R. Gronsky, Z. Q. Li, and T. Lu,
    “Synthesis, Characterization, and Properties of Nanophase TiO2”, J. Mater.
    Res., 3 1367-1372 (1988).
    4. M. Ciftcioglu and M. J. Mayo, “Processing of Nanocrystalline Ceramics”,
    pp.77-86 in Superplasticity in Merals, Ceramics, and Intermetallics(Mater.
    Res. Soc. Symp. Proc. 196), Edited by M. J. Mayo, M. Kobayashi, and J.
    Wadsworh, Pittsburgh, MRS, 1990.
    5. T. G. Nieh, C. M. McNally, and J. Wadsworth, “Superplasticity in
    Intermetallic Alloys and Ceramics”, JOM, 41, 31-35 (1989).
    6. M. Uchic, H. H. Hofler, W. J. Flick, R. Tao, P. Kurath, and R. S. Averback,
    “Sinter-Forging of Nanophase TiO2”, Scripta Metall. Mater., 26, 791-796
    (1992).
    7. A. Tonejc, A. M. Tonejc and D. Bagovic, “Comparison of the
    transformation sequence from γ -AlOOH (boehmite) to α-Al2O3
    (corundum) induced by heating and by ball milling”, Materials Science and
    Engineering, 1227-1231 (1994).
    8. Y. Wang, C Suryanarayana, and L. An, “Phase Transformation-Sized γ
    -Alumina by Mechanical Milling”, J. Am. Ceram. Soc., 88 [3] 780-783
    (2005).
    9. S. Liu, L. Zhang, and L. An, “Phase Transformation of Mechanically Milled
    Nano-Sized γ-Alumina”, J. Am. Ceram. Soc., 88 [9], 2559-2563 (2005).
    10. P. K. Sharma, M. H. Jilavi, D. Burgard, R. Nass, and H. Schmidt,
    “Hydrothermal Synthesis of Nanosize α-Al2O3 from Seeded AluminumHydroxide”, J. Am. Ceram. Soc., 81 [10], 2732-2734 (1998).
    11. J. Yang, S. Mei, and José M. F. Ferreira, “Hydrothermal Synthesis of
    Submicrometer α-Alumina from Seeded Tetraethylammonium Hydroxide
    -Peptized Aluminum Hydroxide”, J. Am. Ceram. Soc., 86 [12], 2055-2058
    (2003).
    12. K. Kamiya, J. Yotani, R. Senba, J. Matsuoka and H. Nasu, “Sol-Gel
    Preparation of Alumina Gels Forming α-Alumina around 500℃”, Journal
    of the Ceramic Society of Japan, Int. Edition, Vol.104, No.7, pp. 685-687
    (1996).
    13. J. Li, Y. Pan, C. Xiang, Q. Ge, J. Guo, “Low temperature synthesis of
    ultrafine α-Al2O3 powder by a simple aqueous sol-gel process”, Ceramics
    International 32, 587-591 (2006).
    14. P. C. Yu, R. J. Yang, Y. T. Chang, and F. S. Yen, “Fabrication of Nano-scaled
    α-Al2O3 Crystallites through Heterogeneous Precipitation of Boehmite in a
    Well-dispersed θ-Al2O3-suspension”, J. Am. Ceram. Soc. 90 [8] 2340-2346
    (2007).
    15. F. J. Ewing, “The Crystal Structure of Lepidocrocite”, J. Chem. Phys, 3,
    420-454 (1935).
    16. J. A. Kohn, G. Katz, and J.D. Broder, “β-Ga2O3 and Its Alumina Isomorph,
    θ-Al2O3”, Am. Miner., 42, 398-408 (1957).
    17. Y. M. Chiang, D. P. Birnie, III, and W. D. Kingery, Physical
    Ceramics-Principles for Ceramic Science and Engineering, Wiley , New
    York (1997).
    18. F. W. DYNYS AND J. W. Halloran, “Alpha Alumina Formation in Alum
    Derived Gamma Alumina”, J. Am. Ceram. Soc., 65 [9], 442-448 (1982).
    19. J. L. McArdle and G. L. Messing, “Seeding with γ-Alumina for
    Transformation and Microstructure Control in Boehmite-Derived
    α-Alumina”, J. Am. Ceram. Soc., 69, C98-101 (1986).
    20. 溫惠玲,由Boehmite 製得之氧化鋁粉末的θ→α-Al2O3 相轉換,國立成
    功大學資源工程研究所,博士論文,中華民國 89 年 1 月。
    21. H. L. Wen and F. S. Yen, “Growth Characteristics of Boehmite-DerivedUltrafine Theta and Alpha-Alumina Particles During Transformation”, J.
    Cryst. Growth, 208 696-708 (2000).
    22. P. L. Chang, F. S. Yen, K. C. Cheng, and H. L. Wen, “Examination on the
    Critical and Primary Crystallite Sizes During θ- to α-Phase Transformation
    on Ultrafine Alumina Powders”, Nano Letters, 5 253-261 (2001).
    23. R. J. Hunter, “Introduction to Modern Colloid Science” (1993).
    24. 高濂、孫靜、劉陽橋, 奈米粉體的分散及表面改性,五南圖書出版股份
    有限公司,中華民國 94 年。
    25. M. N. Rahaman, Ceramic Processing and Sintering, M. Dekker, New York,
    (1995).
    26. T. Seto, A. Hirota, T. Fujimoto, M. Shimado, and K. Okuyama, “Sintering
    of Polydisperse Nanometer-Sized Agglomerates”, Aerosol Science and
    Technology 27:422-438 (1997).
    27. M. Shimada, T. Seto and K. Okuyama, “Size Change of very Fine Silver
    Agglomerates by Sintering in a Heated Flow”, J. Chem. Eng. Jpn.
    27:795-802 (1994).
    28. S. N. Rogak, “Modeling Small Cluster Deposition on the Primary Particles
    of Aerosol Agglomerate”, Aerosol Science and Technology 26:127-140
    (1997).
    29. B. Kindl, D. J. Carlsson, Y. Deslandes, and J. M. Hoddenbagh, “Preparation
    of α-Alumina Ceramics: The Use of Boehmite Sols as Dispersing Agents”,
    Ceram. Int., 17 347-350 (1991).
    30. S. Anathakumar, V. Raja, and K. G. K. Warrier, “Effect of Nanoparticulate
    Boehmite Sol as A Dispersant for Slurry Compaction of Alumina Ceramics”,
    Mater. Lett., 43 174-179 (2000).
    31. S. T. Kwon and G. L. Messing, “Constrained Densification in
    Boehmite-Alumina Mixtures for the Fabrication of Porous Alumina
    Ceramics”, J. Mater. Sci., 33 913-921 (1998).
    32. 陳秀雯,利用Boehmite 分散及包覆θ-Al2O3 粉生產30-50nm α-Al2O3,
    國立成功大學資源工程研究所,碩士論文,中華民國 93 年 6 月。33. 游佩青, 楊榮澤, 顏富士, “θ→α-Al2O3 相變系統中的晶種效應,” 第二屆
    資源工程研討會, 2005.
    34. 楊榮澤, 顏富士, 葉雅青, 陳秀雯, “Boehmite/θ-Al2O3系統之θ-到α-氧化
    鋁相轉換過程之活化能研究,” 第二屆資源工程研討會, 2005.
    35. F. S. Yen, J. L. Chang, and P. C. Yu, “Sintering Characteristics of
    Theta-Alumina Powders during Alpha-Phase Transformation”, Journal of
    Materials Science and Engineering, Vol. 34, No. 3, PP. 165-172 (2002).
    36. R. J. Yang, F. S. Yen, S. M. Lin and C. C. Chen, “Microstructure-controlled
    effects on temperature reduction of α-Al2O3 crystallite formation”, Journal
    of Crystal Growth, 299, 429-435 (2007)

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