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研究生： 王宜晴
Wang, Yi-Ching
論文名稱： 金屬有機骨架與其衍生物於電觸媒之應用
The application of metal−organic frameworks and their derived materials as electrocatalysts
指導教授： 龔仲偉
Kung, Chung-Wei
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2022
畢業學年度： 110
語文別： 中文
論文頁數： 134
中文關鍵詞： 電催化 、金屬有機骨架 、亞硝酸根離子感測 、電合成 、電分析
外文關鍵詞： electrocatalysis, MOF, nitrite sensor, electrosynthesis, electroanalysis
相關次數： 點閱：182  下載：25 
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    • 金屬有機骨架（Metal−organic frameworks, MOFs）是一系列由金屬節點與有機連結器構成的奈米孔洞材料，由於其高比表面積與化學可調性，以MOF製成的修飾電極可提升單位體積內的電化學活性位點密度，在電催化領域中極具發展力。然而大部分MOF缺乏水穩定性，使其在水溶液中的電化學應用受到限制，其中以鋯為金屬節點的MOF因金屬節點與有機連結器之間的強鍵結而能在水溶液中保持穩定。因此在本碩論的第一部分會使用溶劑輔助配體法搭配離子交換的方式將銀安裝以鋯為基底的MOF，NU-902。將該複合材料作為電觸媒應用在亞硝酸根離子於水溶液中的電化學感測，可得到比使用純NU-902更佳的感測效果。
    另外MOF也因為缺乏導電度，使其在需高電流密度的應用受到限制，而將MOF作為前驅物在惰性氣體中高溫碳化可得由金屬、金屬氧化物與多孔碳組成的MOF衍生材料，高導電度與孔洞性的特性使其適用於需高電流密度的應用，例如電解。因此在本碩論的第二部分會使用以鉛為基底的MOF衍生材料作為電催化生產己二腈的電觸媒，使用塔菲爾分析可知MOF衍生材料確實能達到與未使用觸媒相比時較快的反應動力學，進行電解實驗也可在較低過電位下觀察到顯著的催化效果。

    In this thesis, the application of metal−organic frameworks (MOFs) and their derived materials as electrocatalysts would be respectively investigated, and it could be separated to two parts.
    In the first part, silver nanoparticles (NPs) are installed into a porphyrinic zirconium-based metal−organic framework (Zr-MOF), NU-902, through a postsynthetic modification followed by an ion-exchange process. As both the silver NPs and porphyrinic linkers of NU-902 are electrocatalysts for the oxidation of nitrite, the obtained nanocomposite can be applied for the electrochemical nitrite sensor, and the resulting sensing performance is significantly better than that of the pristine porphyrinic Zr-MOF. The Ag-SO3-NU-902 thin films can be further applied for amperometric nitrite sensors. In the second part, nanoporous and electrically conductive MOF-derived materials composed of Pb, PbO, and carbon are synthesized by carbonizing a Pb-based MOF through thermal treatments, and these MOF-derived materials are served as electrocatalysts for the electrosynthesis of adiponitrile (ADN), the raw material for the production of Nylon 66. Electrolytic experiments at various applied potentials are conducted to quantify the production rate and faradaic efficiency toward ADN, and the result shows that the MOF-derived materials can act as electrocatalysts to initiate the electrochemical reduction of AN to produce ADN at a reduced overpotential.

    中文摘要 I Extend Abstract II 致謝 XI 目錄 XIII 表目錄 XIX 圖目錄 XX 第一章 緒論 1 1-1 電化學介紹 1 1-1-1 電化學反應簡介 1 1-1-2 修飾電極與電化學相關應用 4 1-1-3 電化學感測 7 1-1-4 電化學催化 14 1-2 金屬有機骨架 18 1-2-1 金屬有機骨架介紹 18 1-2-2 金屬有機骨架衍生材料介紹 20 第二章 金屬有機骨架鑲嵌之銀奈米粒子於亞硝酸根離子感測之應用 22 2-1 實驗背景介紹 22 2-1-1 前言 22 2-1-2 電流式感測亞硝酸根離子觸媒 22 2-1-3 金屬有機骨架於電化學亞硝酸根離子感測上的應用 24 2-1-4 研究動機 26 2-2 實驗藥品與儀器介紹 28 2-2-1 實驗藥品 28 2-2-2 實驗儀器 30 2-3 實驗方法 31 2-3-1 金屬有機骨架NU-902的合成 31 2-3-2 後修飾鉀鹽（-K+SO3-）於NU-902 32 2-3-3 離子交換 33 2-3-4 修飾電極的製備 34 2-3-5 電化學分析方法 34 2-3-6 核磁共振（Nuclear Magnetic Resonance, NMR）樣品製備 35 2-4 材料鑑定結果分析 35 2-4-1 粉末X射線繞射圖譜（X ray diffraction patterns, XRD patterns） 35 2-4-2 掃描式電子顯微鏡圖（Scanning Electron Microscopic images, SEM images） 38 2-4-3 能量色散X射線光譜（Energy-dispersive X-ray spectroscopy, EDS） 40 2-4-4 核磁共振光譜（Nuclear Magnetic Resonance, NMR） 42 2-4-5 紫外光與可見光吸收圖譜（Ultraviolet-visible spectroscopy, UV-vis spectroscopy） 43 2-4-6 氮氣吸脫附曲線與孔徑分布圖（Nitrogen adsorption and desorption isotherm and Density Functional Theory (DFT) pore size distribution） 44 2-4-7 X射線光電子光譜（X-ray photoelectron spectroscopy, XPS） 46 2-4-8 穿透式電子顯微鏡圖（Transmission Electron Microscopic images, TEM images） 48 2-5 電化學結果分析 49 2-5-1 循環伏安分析（Cyclic voltammetric analysis, CV analysis） 49 2-5-2 電流式感測分析 56 2-5-3 干擾物測試 59 2-6 小結 61 第三章 多孔電觸媒開發與其修飾電極於選擇性電催化生產己二腈之應用 63 3-1 背景介紹 63 3-1-1 前言 63 3-1-2 己二腈的電解合成法 64 3-1-3 研究動機 68 3-2 實驗藥品與儀器介紹 69 3-2-1 實驗藥品 69 3-2-2 實驗儀器 71 3-3 實驗方法 72 3-3-1 金屬有機骨架衍生材料的合成 72 3-3-2 修飾電極的製備 73 3-3-3 錠片的製備 74 3-3-4 產物鑑定 74 3-3-5 導電度測試實驗 78 3-3-6 修飾電極前處理 78 3-3-7 電化學實驗 79 3-4 材料鑑定結果分析 81 3-4-1 熱重分析曲線（Thermogravimetry Analysis curve, TGA curve） 81 3-4-2 粉末X射線繞射圖譜（X ray diffraction patterns, XRD patterns） 83 3-4-3 掃描式電子顯微鏡圖（Scanning Electron Microscopic images, SEM images） 86 3-4-4 能量色散X射線光譜圖（Energy dispersive X-ray spectroscopy, EDS） 88 3-4-5 穿透式電子顯微鏡圖（Transmission Electron Microscopic images, TEM images） 89 3-4-6 氮氣吸脫附曲線與BJH孔徑分布圖（Nitrogen adsorption and desorption isotherm and Barret-Joyner-Halenda (BJH) pore size distribution） 93 3-4-7 X射線光電子光譜（X-ray photoelectron spectroscopy, XPS） 94 3-4-8 拉曼光譜（Raman spectrometry） 95 3-4-9 電流對電壓曲線 97 3-5 電化學結果分析 99 3-5-1 電化學活性面積（ECSA）分析 99 3-5-2 線性掃描伏安（LSV）分析 101 3-5-3 電解過程的電流對時間曲線 104 3-5-4 不同電位下電解的產物分析 106 3-6 小結 111 第四章 未來展望與建議 113 參考文獻 115

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