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研究生:邱茂森
研究生(外文):Mau-Sen Chiu
論文名稱:中尺度孔洞薄膜與大分子單晶X光繞射之研究
論文名稱(外文):X-ray diffraction in mesoporous tube thin film (MCM-41) and macromolecular crystal
指導教授:張石麟
指導教授(外文):Shih-Lin Chang
學位類別:碩士
校院名稱:國立清華大學
系所名稱:物理學系
學門:自然科學學門
學類:物理學類
論文種類:學術論文
論文出版年:2003
畢業學年度:91
語文別:中文
論文頁數:70
中文關鍵詞:溶菌酶三光複繞射三重積相位中尺度孔洞掠角入射小角度散射
外文關鍵詞:lysozymethree beam multiple diffractiontriplet phaseMCM-41GISAXS
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本論文分為兩部分,第一部份為利用X光繞射協助清華大學化學系教授趙桂蓉老師分析中尺度二氧化矽孔洞(MCM41)薄膜的結構.趙桂蓉老師將C16EO10(模板劑的前驅物),以浸渍塗佈(dip-coating)的方式,塗佈在矽晶片(100)的表面,並加以熱處理,形成中尺度二氧化矽孔洞薄膜.本論文利用X光徑向(θ-2θ)掃描, X光平面(α-β)掃描,X光掠角繞射(GID)影像等方式,分析薄膜結構.我們發現孔洞薄膜同時有兩種結構存在,孔洞薄膜會形成二維晶格,但從穿透式的X光繞射圖形出現繞射環的情形來看,並沒有特定的排列方向.
第二部份為大分子X光繞射用之CCD測試,利用同步輻射光源配合高精度八環繞射儀,收集溶菌脢蛋白質分子之X光繞射圖形.文中並將描述此套儀器及軟體操作說明.此部份尚在測試儀器的階段.

Thesis contain two parts, the firt part utilize grazing incidence small angle x-ray scattering (GISAXS)to study the structure of the mesopoeous tube thin film (MCM-41), the thin film contains two structure, one is face-center rectangular and the other is rectangular.No prefered orientaqtion.
The second part test the ability of CCD to collect the x-ray diffraction patteren of macromolecular (lysozyme)in national synchron radiation research center. The data quality is very good.

目錄
第一部份
第一章 簡介…………………………………………1
第二章 實驗原理………………………………………2
2-1 X光繞射物理………………………………………2
2-2 X光掠角繞射……………………………………3
2-3 繞射峰形……………………………………….5
第三章 樣品製備……………………………………. 10
第四章 儀器設備………………………………………11
4-1 同步輻射光源………………………………….11
4-2 八環繞射儀…………………………………….15
4-3 影像板………………………………………….16
4-4 閃爍計數器…………………………………….18
第五章 實驗步驟………………………………………19
5-1 實驗裝置及條件……………………………….19
5-2 光掠角繞射影像……………………………….19
5-3 徑向掃瞄……………………………………….20
5-4 平面掃描……………………………………….21
第六章 結果與分析…………………………………..22
6-1 二維影像……………………………………….22
6-2 徑向掃描……………………………………….26
6-3 平面掃描……………………………………….26
附錄
A 數據分析流程…………………………………….28
B 校正繞射儀環心………………………………….30
C 調整繞射儀的環心使之位於光經過的路徑上….30
D 直射光原點校正………………………………….31
E 樣品調平………………………………………….31
參考資料……………………………………………….33
第二部分
第一章 序論……………………………………………38
第二章 複繞射…………………………………..……40
2-1 向位問題………………………………………40
2-2 不變相位………………………………………40
2-3 傳統複繞射……………………………………41
2-4 雙向複繞射……………………………………44
第三章 複繞射之動力繞射理論………………………47
3-1 基本波場方程式………………………………47
3-2 相位分析理論…………………………………51
第四章 轉動矩陣晶體方向矩陣……………………..54
4-1 轉動矩陣………………………………………54
4-2 晶體的方向矩陣………………………………55
第五章 樣品製備………………………………………58
第六章 CCD系統介紹………………………………….59
6-1 Jupiter-140……………………………………59
6-2 d*TREK 軟體操作說明……………………….62
第七章 結果與展望……………………………………66
參考文獻……………………………………………….68

參考文獻
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Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism
Nature 359, 710-712, 1992
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Photoluminescent silicon clusters in oriented hexagonal mesoporous silica film
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Continuous formation of supported cubic and hexagonal mesoporous films by sol-gel dip-coating
Nature 389, 364-368, 1997
[4] S. H. Tolbert, A. Firouzi, G. D. Stucky, and B. F. Chmelka
Magnetic Field Alignment of Ordered Silicate-Surfactant Composites and Mesoporous Silica
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The true structure of hexagonal Mesophase-templated silica films as revealed by X-ray scattering: Effect of thermal treatments and nanoparticle seeding
Chem. Mater. 12, 1721-1728, 2000
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Preferred alignment of mesochannels in a mesoporous silica film grown on a silicon (110) surface
J. Am. Chem. Soc. 121, 7618-7624, 1999
[7] H. Miyata, T. Noma, M. Watanabe, and K. Kuroda
Preparation of mesoporous silica films with fully aligned large mesochannels using nonionic surfactants
Chemistry of Materials 14, 766-772, 2002
[8] D. Zhao, P. Yang, N. Melosh, J. Feng, B.F. Chmelka, and G. D. Stucky
Continuous mesoporous silica films with highly ordered large pore structures
Adv. Mater. 10, 1380-1385, 1998
[9] H. W. Hillhouse, J. W. van Egmond, M. Tsapatsis, J. C. Hanson, E. E. Larese
The interpretation of X-ray diffraction data for the determination of channel orientation in mesoporous films
Microporous and Mesoporous Materials 44, 639-643, 2001
[10]張石麟 掠角X光繞射儀, 儀器總攬-表面分析儀器, 45-46, 國科會精密儀器中心 (1998)
[11] E. Dershem & M. Schein
The reflection of the Kα line of carbon from quartz and its relation to index of refraction and absorption coefficient
Phys. Rev. 37, 1246-1251, 1931
[12] J. D. Jackson Classical electrodynamics pp309-310, 3rd, wiley
[13]林文智 X光繞射倒異空間圖譜分析之簡介 科儀新知, 22卷2期, 14-22, (2000)
[14] Leonid V. Azaroff
Elements of X-ray crystallography, Ch9, McGraw-Hill, (1968)
[15]許樹恩&吳泰伯 X光繞射原理與材料結構分析, Ch7, 中國材料科學學會, (1996)
參考文獻
[1]. S. L. Chang and M. T. Tang
Quantitative determination of phases of X-ray reflection from three-beam diffraction. Theoretical considerations
Acta Cryst. A44, 1065-1072, 1988
[2]. S. L. Chang, H. E. King, Jr., M. T. Huang, Y. Gao
Direct phase determination of large macromolecular crystals using three-beam x-ray interference
Phys. Rev. Lett. 67, 3113-3116, 1991
[3]. S. L. Chang, C. H. Chao, Y. S. Huang, Y. C. Jean, H. S. Sheu, F. J. Liang, H. C. Chien, C. K. Chen, and H. S. Yuan
Quantitative phase determination for macromolecular crystals using stereoscopic multibeam imaging
Acta Cryst. A55, 933-938, 1999
[4]. C. H. Chao, C. Y. Hung, Y. S. Huang, C. H. Ching, Y. R. Lee, Y. C. Jean, S. C. Lai, Y. P. Stetsko, Hanna Yuan, and S. L. Chang
Multiple diffraction data analysis for macromolecular crystals in stereoscopic multibeam imaging
Acta Cryst. A58, 33-41, 2002
[5]. S. L. Chang, Y. P. Stetsko, Y. S. Huang, C. H. Chao, F. J. Liang, C. K. Chen
Quasi-universality and scaling behaviour of three-wave X-ray interference in crystals: A novel way for the quantitative determination of X-ray reflection phases
Phys. Let. A 264, 328-333, 1999
[6]. C. M. Wang, C. H. Chao, and S. L. Chang
Phase determination and extension using X-ray multiple diffraction and the maximum-entropy method
Acta Cryst. A57, 420-428, 2001
[7]. Q. Shen
Solving the phase problem using reference-beam x-ray diffraction
Phys. Rev. Lett. 80, 3268-3271, 1998
[8]. Q. Shen, S. Kycia, and I. Dobrianov
Enantiomorph determination using inverse reference-beam diffraction images
Acta Cryst. A56, 264-267, 2000
[9]. Q. Shen, S. Kycia, and I. Dobrianov
Triplet-phase measurements using reference-beam x-ray diffraction
Acta Cryst. A56, 268-279, 2000
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Multiple-beam x-ray diffraction for physical determination of reflection phases and its applications
Acta Cryst. A53, 108-143, 1997
[11]. J.W. Pflugrath d*TREK version 4.4 Feb 27 1998

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