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研究生： 羅嘉雁
Angelia Sulaiman Lo
論文名稱： 以X光吸收光譜法分析嵌入微孔及中孔無機物質的金屬
Applications of X-ray Absorption Spectroscopy on characterization of metal containing zeolites and mesoporous materials
指導教授： 趙桂蓉博士
Kuei-Jung Chao
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： 2005
畢業學年度： 93
語文別： 英文
論文頁數： 96
中文關鍵詞： X光吸收光譜 、氧化釕 、ZSM-5沸石 、FAU沸石
相關次數： 點閱：67  下載：0 
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    • Ruthenium oxide particles were introduced into ZSM-5 (MFI type) by aqueous ion exchange and hydrothermal zeolite synthesis methods in the presence or absence of tetrapropyl ammonium ions as organic template. The local structure of ruthenium has been studied by XAS, PXRD, and TEM characterization methods.
    The aqueous ion exchange method leads to anhydrous ruthenium oxide with average particle size of 2.0 nm by TEM and □ 2 nm by PXRD, while small hydrous ruthenium oxide particles with diameter 0.6 nm are obtained by template-free synthesis. Similar template-free method was applied to introduce ruthenium oxide particles into FAU pores, which leads to hydrous ruthenium oxide with diameter 1.3 nm. In the presence of organic template (TPA), hydrous ruthenium oxide particles were introduced, but after subsequent calcination, large anhydrous ruthenium oxide particles □ 2 nm detected by PXRD were obtained.
    The effect of solvent, concentration and reduction treatment on the sizes and morphologies on the local structure of platinum, palladium, and gold incorporated in mesoporous silicas were also investigated by XAS characterization method. Pt nanonetworks and nanoparticles were observed in Pt/MCM-48 sample prepared from an aqueous solution and ethanol solution of Pt-precursor, respectively. Different average sizes of Au metals (~3 and ~5 nm) also have been observed in Au/SBA-15 samples reduced under NaBH4 solution and H2 gas flow treatment, respectively.

    Contents Abstract i Acknowledgement ii Contents iii Figure Captions v Table Captions xi CHAPTER I. Introduction 1 1.1 Microporous zeolites, mesoporous silicas and metal-containing mesoporous silicas 1 1.2 Synchrotron X-ray Radiation 4 1.3 X-ray Absorption Spectroscopy (XAS) 6 1.3.1 Theory of EXAFS 7 1.3.2 Data Analysis 11 1.4 The aim of this thesis 19 1.5 References 20 CHAPTER II. Characterization of Ru-containing Zeolites 24 2.1 Introduction 24 2.2 Experimental 25 2.2.1 Sample description 25 2.2.2 Characterization Methods 27 2.3 Results and Discussion 29 2.3.1 Ru K-edge XANES analysis 29 2.3.2 Ru K-edge EXAFS analysis 31 2.3.3 Powder-XRD measurement 43 2.3.4 TEM measurement 47 2.4 Summary 49 2.5 References: 50 CHAPTER III. Characterization of transition metals (Pt, Pd, Au) incorporated in mesoporous silica materials 51 3.1 Introduction 51 3.2 Experimental 52 3.2.1 Sample Preparation 52 3.2.2 X-ray absorption measurement and analysis 53 3.2.3 X-ray diffraction measurement 54 3.2.4 TEM with electron diffraction 54 3.3 Results and Discussion 55 3.3.1 Pt/MCM-48 55 3.3.2 Pd/MCM-48 64 3.3.3 Au/SBA-15 74 3.4 References 83 Chapter IV. Conclusion 84 Appendix B 88 Appendix C 90 Appendix D 96

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