同步輻射所產生的X光光源具有能量連續且可調變,準直性佳,高亮度等優點,非常適合進行掠角X光繞射,粉末X光繞射,X光反射率及X光吸收光譜等實驗上,並用以鑑定奈米材料之結構。
在論文的第一章將對孔洞性材料及所論文中所用到的各種分析鑑定做一個簡單的介紹。第二章則是以掠角X光繞射及X光反射率來鑑定矽晶片基材上的中孔洞二氧化矽薄膜,並配合電子顯微鏡及電子繞射所觀察到的結果,以了解其中尺度之孔洞結構。另外在氧化鋁管的內壁所鍍上約1微米厚之沸石透膜,利用掠角X光繞射可不破壞管子來進行其X光繞射圖譜之偵測以確定其結構。第三章中,粉末X光繞射及X光吸收光譜被用來分析奈米金及奈米鉑的粒子大小,我們發現奈米金屬的大小及形態可以藉由不同的製備及還原過程來加以操控。在原位X光繞射實驗則可用來監控奈米金屬顆粒大小在高溫下的變化。第四章則是使用電腦模擬及X光吸收光譜(包含近吸收邊緣及延伸吸收精細結構之分析)來分析微孔洞沸石中所填入的鎵的形態。電腦摸擬的結果與X光吸收光譜及紅外光光譜的結果相當吻合,並可用以推測鎵在沸石中的位置。鎵在TMG/ZSM-5沸石中的化學狀態也可以原位X光近吸收邊緣光譜來監測,被還原的TMG/ZSM-5在773K高溫下極易被氧化。直接氧化與先還原再氧化之TMG/ZSM-5中,鎵的物種是不同的,也因而其催化活性上會有所差異。

Structural characterization of zeolite and mesoporous silica in the forms of film and membrane as well as their incorporated nano-sized metals were performed by X-ray diffraction (GIXD and PXRD), reflectivity (XRR) and X-ray absorption spectroscopy (XAS) using synchrotron X-ray source.
In the first chapter, an introduction of porous materials, nano-sized metals in porous materials and structural characterization methods employed in this thesis are described.
In Chapter 2, on-substrate mesoporous silica films were investigated by GIXD, XRR and TEM. The better structured thin films were proved to have better mechanical properties. A thin layer of zeolite coated on the inner wall of an asymmetric ceramic tube was detected non-destructively by reducing the contribution of the crystalline support using GIXD.
In the third chapter, the sizes of nano-Au and Pt were evaluated by both PXRD and XAS. It is interesting that sizes and morphologies were observed to be controlled through manipulating preparation and reduction conditions. In-situ PXRD was performed to detect the size increase of Au nanoparticles in reduced samples during thermal treatment.
In Chapter 4, the local structure of gallium species in zeolites studied by computation simulation and XAS including XANES and EXAFS techniques is given. The simulation results of Ga/beta zeolites are in good agreement with previous EXAFS and FTIR results and can be used to predict the possible locations of gallium species in beta zeolites. The chemical state of Ga in as-synthesized TMG/ZSM-5 was monitored by in-situ XANES during reduction process. The reduced form sample was found to be oxidized fast at 773 K under oxygen atmosphere. Two kinds of oxidized gallium species, generated by direct oxidation and oxidation after reduction, respectively, were found to possess different catalytic activities.

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