蒸氣相成長金屬有機框架材料合成

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姓名

吳柏融(Bo-Rong Wu) 查詢紙本館藏

畢業系所

化學工程與材料工程學系

論文名稱

蒸氣相成長金屬有機框架材料合成
(Vapor Phase Synthesis of Metal-Organic Frameworks (MOFs))

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摘要(中)

本研究利用傳統電器（Conventional Electric）及微波輔助（Microwave-assisted）方式合成金屬有機框架材料(MOFs)，並嘗試在前驅溶液的蒸氣相中合成MIL-53 (Al)晶體於氧化鋁基材（α-Al2O3）的表面上形成膜（Membrane）或直接將前驅物加熱為蒸氣狀態,進而反應並沈積薄膜在基板，有別於以往傳統製備無機氣體滲透膜的製程是將基材放置於前驅溶液的液相中成長膜及化學氣相沈積法，這是相對成本較低且在蒸氣相合成金屬有機框架薄膜的方法。
在本研究中，我們設計了四種可以在蒸氣相成長膜的方法，並且透過參數的改變及製程上的設計進而提高膜的覆蓋率及均勻性。然而我們也發現，在液相及蒸氣相中以傳統烘箱及微波合成金屬有機框架膜皆有不同的表面形貌產生,大致上可分為塊狀及棒狀。
X-射線繞射分析儀（X-ray diffraction, XRD）可用來驗證成長於基材上的的材料為何，並判斷MIL-53 (Al)是否成功成長於氧化鋁基材上。掃描式電子顯微鏡 (scanning electron microscopy, SEM)用來分析MIL-53 (Al)膜的表面形貌。氮氣吸附孔隙儀 (BET surface area measurement)分別對傳統電器合成的MIL-53 (Al)及微波輔助合成的MIL-53 (Al)量測比表面積，驗證不同合成方法對於材料的比表面積的影響。

摘要(英)

In this study, conventional electric and microwave-assisted heating were used for metal-organic framework synthesis, and we attempted to grow MIL-53 (Al) membrane on α-Al2O3 via vapor processing. Different from conventional method which places α-Al2O3 in the liquid precursor solution for preparing inorganic gas separation membrane, these methods are inexpensive for membrane fabrication in the vapor phase condition.
In this research, we developed four methods for membrane synthesis in the vapor phase. The membrane coverage and uniformity were improved by adjusting the experimental process and parameters. In addition, membrane synthesis with different conditions resulted in different crystal morphologies, such as bulk-like and rod-like crystals. Namely, we could control the membrane morphology by synthetic methods and phases.
Material growing on α-Al2O3 was identified by X-ray diffraction (XRD). Scanning electron microscopy (SEM) was used for morphology analysis. Different surface area of MIL-53 (Al) synthesized by conventional electric and microwave-assisted heating was confirmed by BET surface area measurement.

關鍵字(中)

★ 蒸氣相
★ 金屬有機框架
★ MIL-53 (Al)
★ 溶熱法
★ 傳統電器加熱
★ 微波輔助加熱
★ 氧化鋁基材

關鍵字(英)

★ Vapor phase
★ Metal-organic framework
★ MIL-53 (Al)
★ Solvothermal
★ Conventional electric
★ Microwave-assisted
★ Alumina support

論文目次

摘要 i
Abstract ii
Acknowledgements iii
Table of Contents iv
List of Figures vi
List of Tables xii
Chapter 1 Background 1
1.1 Introduction 1
1.2 Review of Relevant Literature 6
1.2.1 Materials Institute Lavoisier-53, MIL-53 6
1.2.2 Hydrothermal, Solvothermal and Microwave-Assisted Heating 9
1.2.3 MOF Membrane 13
1.2.4 Vapor Processing 19
1.3 Motivation 23
Chapter 2 Experimental Methods 24
2.1 Material 24
2.1.1 Chemical Compounds 24
2.1.2 Porous Inorganic Support 24
2.2 Experimental Procedure 25
2.2.1 MIL-53 (Al) Synthesis via Conventional Electric and Microwave-Assisted Heating 25
2.2.2 Preparation of MIL-53 (Al) Membrane 27
2.3 Equipment Used 43
2.4 Material Characterizations 44
Chapter 3 Results and Discussion 46
3.1 MIL-53 (Al) Synthesis via Conventional Electric and Microwave-assisted Heating 46
3.1.1 Material Identification and Yield 46
3.1.2 Crystal Morphology 49
3.1.3 Nitrogen Adsorption Isotherms, Surface Area and Pore Size Distribution 50
3.2 Preparation of MIL-53 (Al) membrane 52
3.2.1 Secondary Growth Method 53
3.2.2 Solvent Evaporation (oven) Method 60
3.2.3 Solvent Evaporation (hot plate) Method 66
3.2.4 Vapor-Solid Crystallization Method 75
Chapter 4 Conclusions 79
Chapter 5 Future Work 80
References 81

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指導教授

張博凱(Bor Kae Chang)

審核日期

2017-7-26

推文