簡易檢索 / 詳目顯示

研究生: 林靜儀
Ching-Yi Lin
論文名稱: 中孔洞二氧化矽奈米顆粒的合成與鑑定
Synthesis and Characterization of Mesoporous Silica Nanoparticles
指導教授: 楊家銘
Chia-Min Yang
口試委員:
學位類別: 碩士
Master
系所名稱: 理學院 - 化學系
Department of Chemistry
論文出版年: 2007
畢業學年度: 95
語文別: 中文
論文頁數: 104
中文關鍵詞: 中孔洞二氧化矽
外文關鍵詞: Mesoporous, Silica, MCM-41, c2mm
相關次數: 點閱:1下載:0
分享至:
查詢本校圖書館目錄 查詢臺灣博碩士論文知識加值系統 勘誤回報
  • 本論文以陽離子型界面活性劑合成中孔洞MCM-41二氧化矽奈米顆粒。透過改變反應物的濃度,對其顆粒大小進行調控。另外,我們發現藉由添加非離子型界面活性劑,可以調控中孔洞二氧化矽的孔洞結構。其中,我們可成功地合成出具有新穎c2mm結構且橢圓形孔洞截面的中孔洞二氧化矽奈米顆粒。我們以X光小角度散射/繞射實驗探討其合成過程中的結構演化。我們利用X光粉末繞射圖譜及穿透式電子顯微鏡對此一特殊結構加以確認,而SEM鑑定顯示產物有球狀與棒狀兩種規則的外觀形貌。我們更進一步將Pt嵌入具有c2mm結構之二氧化矽奈米顆粒中,觀察到球狀二氧化矽顆粒其孔道連接方式為連續式的迴圈,棒狀二氧化矽顆粒中則為具有掌性的孔洞結構。


    We have synthesized highly ordered mesoporous MCM-41 silica nanoparticles with controlled particle sizes by tuning the concentrations of the reactants. In addition, by mixing non-ionic surfactants with the cationic surfactant cetyltrimethylammoium bromide, the structure of the resulting mesoporous silicas can be tailored. Interestingly, we have successfully prepared mesoporous silica nanoparticles with a novel two-dimensional rectangular c2mm structure and elliptical pore section. In-situ small angle X-ray scattering/diffraction measurements have been applied to follow the structural evolution during the synthesis of the material, and the c2mm structure of the final product has been confirmed by powder X-ray diffraction and transmission electron microscopy. Furthermore, the scanning electron microscopic studies have shown that most of the c2mm mesoporous silica nanoparticles are spherical in shape and uniform in size, and only few particles with rod shape have been observed. We have also infiltrated platinum into the c2mm mesoporous silica nanoparticles, which clearly show that while the mesopore channels in the spherical nanoparticles are circular around the center axis, those in the rod-like nanoparticles have a chiral morphology.

    目錄 第一章 緒論 1-1 中孔洞二氧化矽材料簡介 1 1-2 孔洞結構與型貌的調控與應用 7 1-3 二氧化矽奈米顆粒的嵌入化學與功能化 13 1-4 中孔洞二氧化矽奈米顆粒在生物醫學方面的應用 14 1-5 研究動機與目的 16 第二章 實驗部分 2-1 藥品 17 2-2 實驗步驟 18 2-2-1 MCM-41中孔二氧化矽奈米顆粒的合成 18 2-2-2 以CTAB及非離子型界面活性劑合成中孔二氧化矽奈米顆粒 19 2-2-2-1 以CTAB及C12EO4合成中孔二氧化矽顆粒 19 2-2-2-2 具c2mm結構之中孔二氧化矽顆粒的合成 20 2-2-2-3 以CTAB及C12O10或C18EO2合成中孔二氧化矽顆粒 21 2-2-3 鉑金屬嵌入具c2mm結構之中孔二氧化矽奈米顆粒 22 2-3 鑑定分析 23 2-3-1 X光粉末繞射儀 23 2-3-2 X光小角散射儀 26 2-3-3 熱重分析 29 2-3-4 氮氣吸脫附鑑定 29 2-3-5 固態核磁共振 33 2-3-6 掃描式電子顯微鏡 35 2-3-7 穿透式電子顯微鏡 36 第三章 結果與討論 3-1 MCM-41中孔二氧化矽奈米顆粒合成結果 38 3-2 以CTAB及非離子型界面活性劑合成中孔二氧化矽奈米顆粒 55 3-2-1 以CTAB及C12EO4合成中孔二氧化矽顆粒結果 55 3-2-2 具c2mm結構之中孔二氧化矽顆粒的合成結果 56 3-2-3 以CTAB及C12O10或C18EO2合成中孔二氧化矽顆粒結果 85 3-2-3-1 以CTAB及C12O10合成中孔二氧化矽顆粒 85 3-2-3-2 以CTAB及C18O2合成中孔二氧化矽顆粒 91 3-3 鉑金屬嵌入具c2mm結構之中孔二氧化矽奈米顆粒 97 第四章 結論 99 參考文獻 100

    1. Ciesla, U. ; Schüth, F. Microporous Mesoporous Mater. 1999, 27, 131.
    2. Kresge, C. T. ; Leonowicz, M. E. ; Roth, W. J. ; Vatuli, J. C. ; Beck , J. S. Nature 1992, 359, 710.
    3. Schmidt, R. ; Hansen, E. W. ; Stöcker, M. ; Akporiate, D. ; Fllestad, O. H. J. Am. Chem. Soc. 1995, 117, 4049.
    4. Raman, N. K. ; Anderson, M. T. ; Brinker, C. J. Chem. Mater. 1996, 8, 1682.
    5. Huo, Q. ; Margolese, D. l. ; Ciesla, U. ; Feng, P. ; Gier, T. E. ; Sieger, P. ; Leon, R. ; Petroff, P. M. ; Schüth, F ; Stucky, G. D. Nature 1994, 368, 317.
    6. Hoffmann, F. ; Cornelius, M. ; Morell, J. ; Fröba, M. Angew. Chem. Int. Ed. 2006, 45, 3216.
    7. Beck, J. S. ; Vartuli, J. C. ; Roth, W. J. ; Leonowicz, M. E. ; Kresge, C. T. ; Schmitt, K. D. ; Chu, C. T. W. ; Olson, D. H. ; Sheppard, E. W. ; McCullen, S. B. ; Higgins, J. B. ; Schlenker, J. L. J. Am. Chem. Soc. 1992, 114, 10834.
    8. Yanagisawa, T. ; Shimizu, T. ; Kuroda, K. ; Kato, C. Bull. Chem. Soc. Jpn. 1990, 63, 988.
    9. Inagaki, S. ; Fukushima, Y. ; Kuroda, K. J. Chem. Soc., Chem. Commun. 1993, 680.
    10. Monnier, A. ; Schüth, F. ; Huo, Q. ; Kumar, D. ; Margolese, D. ; Maxwell, R. S. ; Stucky, G. D. ; Krishnamurty, M. ; Petroff, P. ; Firouzi, A. ; Janicke, M. ; Chmelka, B. F. Science 1993, 261, 1299
    11. Zhao, D. ; Huo Q. ; Feng, J. ; Chemlka, B. F. ; Stucky G. D. J. Am. Chem. Soc. 1998, 120, 6024.
    12. Ryoo, R. ; Joo, S. H. ; Kim, J. M. J. Phys. Chem. B 1999, 103, 7435.
    13. Chel, S. ; Liu, Z. ; Ohsuna, T. ; Sakamoto, K. ; Terasaki, O. ; Tatsumi, T. Nature 2004, 429, 281.
    14. Yang, Y. ; Suzuki, M. ; Owa, S. ; Shirai, H. ; Hanabusa, K. J. Mater. Chem. 2006, 16, 1644.
    15. Wu, X. ; Jin, H. ; Liu, Z. ; Ohsuna, T. ; Terasaki, O. ; Sakamoto, K. ; Che, S. Chem. Mater. 2006, 18, 241.
    16. Jin, H ; Liu, Z. ; Ohsuna, T. ; Terasaki, O. ; Inoue, Y. ; Sakamoto, K. ; Nakanishi, T. ; Ariga, K. ; Che, S. Adv. Mater. 2006, 18, 593.
    17. Lin, G. L. ; Tsai, Y. H. ; Lin, H. P. ; Tang, C.-Y. ; Lin, C. Y. Langmuir 2007, 23, 4115.
    18. Trewyn, B. G. ; Whitman, C. M. ; Lin, V. S. Y. Nano Lett. 2004, 4, 11, 2139.
    19. Wang, B. ; Chi, C. ; Shan, W. ; Zhang, Y. ; Ren, N. ; Yang, W. ; Tang, Y. Angew. Chem., Int. Ed. 2006, 45, 2088.
    20. Chen, H. T. ; Huh, S. ; Wiench, J. W. ; Pruski, M. ; Lin, V. S. Y. J. Am. Chem. Soc. 2005, 127, 13305.
    21. Kumar, R. ; Chen, H. T. ; Escoto, J. L. V. ; Lin, V. S. Y. ; Pruski, M. Chem. Mater. 2006, 18, 4319.
    22. Moller, K. ; Bein, T. Chem. Mater. 1998, 10, 2950.
    23. Fukuoka, A. ; Higuchi, T. ; Ohtake, T. ; Oshio, T. ; Kimura, J. I. ; Sakamoto, Y. ; Shimomura, N. ; Inagaki, S. ; Ichikawa, M. Chem. Mater. 2006, 18, 337.
    24. Yang, C. M. ; Sheu, H.-S. ; Chao, K. J. Adv. Funct. Mater. 2002, 12, 143.
    25. Feng, X. ; Fryxell, G. E. ; Wang, L. Q. ; Kim, A. Y. ; Liu, J. ; Kemner, K. M. Science 1997, 276, 923.
    26. Liu, J. ; Feng, X. ; Fryxell, G. E. ; Wang, L. Q. ; Kim, A. Y. ; Gong, M. Adv. Mater. 1998, 10, 161.
    27. Wang, Y. Q. ; Yang, C. M. ; Schmidt, W. ; Spliethoff, B. ; Bill, E. ; Schüth, F. Adv. Mater. 2005, 17, 53
    28. Ko, C. H. ; Ryoo, R. Chem. Commun. 1996, 2467.
    29. Liu, Z. ; Sakamoto, Y. ; Ohsuna, T. ; Hiraga, K. ; Tersaki, O ; Ko, C. H. ; Shin, H. J. ; Ryoo, R. Angew. Chem., Int. Ed. 2000, 39, 17, 3107.
    30. Jun, S. ; Joo, S. H. ; Ryoo, R. ; Kruk, M. ; Jaroniec, M. ; Liu, Z. ; Ohsuna, T. ; Terasaki, O. J. Am. Chem. Soc. 2000, 122, 10712.
    31. Ryoo, R. ; Joo, S. H. ; Kruk, M. ; Jaroniec, M. Adv. Mater. 2001, 13, 677.
    32. Gallis, K. W. ; Araujo, J. T. ; Duff, K. J. ; Moore, J. G.; Landry, C. C. Adv. Mater. 1999, 11, 17.
    33. Zhu, Y. F. ; Shi, J. L. ; Li, Y. S. ; Chen, H. R. ; Shen, W. H. ; Dong, X. P. Microporous Mesoporous Mater. 2005, 85, 75.
    34. Lai, C.-Y. ; Trewyn, B. G. ; Jeftinija, D. M. ; Jeftinija, K. ; Xu, S. ; Jeftinija, S. ; Lin, V. S. Y. J. Am. Chem. Soc. 2003, 125, 4451.
    35. Radu, D. R. ; Lai, C. Y. ; Wiench, J. W. ; Pruski, M. ; Lin, V. S. Y. J. Am. Chem. Soc. 2004, 126, 1640.
    36. Lin, Y.-S. ; Tsai, C. P. ; Huang, H.-Y. ; Kuo, C. T. ; Hung, Y. ; Huang, D. M. ; Chen, Y. C. ; Mou, C. Y. Chem. Mater. 2005, 17, 4570.
    37. Slowing, I. ; Trewyn, B. G.; Lin, V. S. Y. J. Am. Chem. Soc. 2006, 128, 14792.
    38. Mal, N. K. ; Fujiwara, M. ; Tanaka, Y. Nature 2003, 421, 350.
    39. Mal, N. K. ; Fujiwara, M. ; Tanaka, Y. ; Taguchi, T. ; Matsukata, M. Chem. Mater. 2003, 15, 3385.
    40. Giri, S. ; Trewyn, G. B. ; Stellmaker, M. P. ; Lin, V. S. Y. Angew. Chem. Int. Ed. 2005, 44, 5038.
    41. Zhu, Y. ; Shi, J. ; Shen, W. ; Dong, X. ; Feng, J. ; Ruan, M. ; Li, Y. Angew. Chem. Int. Ed. 2005, 44, 5083.
    42. Yeh, Y. Q. ; Chen, B. C. ; Lin, H. P. ; Tang, C. Y. Langmuir 2006, 22, 6.
    43. Lin, H. P. ; Tsai C. P. Chem. Lett. 2003, 32, 12.
    44. Li, Y. ; Shi, J. ; Hua, Z. ; Chen, H. ; Ruan, M. ; Yan, D. Nano Letters. 2003, 3, 609.
    45. Chen, M. ; Wu, L. ; Zhou, S. ; You, B. Adv. Mater. 2006, 18, 801.
    46. Fujiwara, M. ; Shiokawa, K. ; Tanaka, Y. ; Nakahara, Y. Chem. Mater. 2004, 16, 5420.
    47. Šegota, S. ; Težak, D. Adv. Colloid Interface Sci. 2006, 121, 51.
    48. Shimura, N. ; Ogawa, M. Bull. Chem. Soc. Jpn. 2005, 78, 1154.
    49. Cai, Q. ; Lin, W. Y. ; Xiao, F. S. ; Pang, W. Q ; Chen, X. H. ; Zou, B. S. Microporous Mesoporous Mater. 1999, 32, 1
    50. 鄭有舜,X-光小角度散射在軟物質研究上的應用,物理雙月刊,廿六卷第二期,2004,416頁
    51. 汪建民,材料分析,中國材料科學學會,2006.
    52. Ravikovitch, P. I. ; Vishnyakov, A ; Neimark, A. V. Phys. Rev. E. 2001, 64, 011602
    53. Kleitz, F. ; Blanchard, J. ; Zibrowius, B. ; Schuth, F. langmuir 2002, 18, 4963

    無法下載圖示 全文公開日期 本全文未授權公開 (校內網路)
    全文公開日期 本全文未授權公開 (校外網路)

    QR CODE