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研究生： Tamene Simachew Zeleke
Tamene Simachew Zeleke
論文名稱： 新型氫氣氧化反應陰極材料合成與其機制探討
Design of Cathode Materials for Electrolyzer and Propose A Plausible Mechanism for Hydrogen Oxidation Reaction
指導教授： 黃炳照
Bing-Joe Hwang
蘇威年
Wei- Nien Su
口試委員: 葉旻鑫
Min-Hsin Yeh
周澤川
Tse-Chuan Chou
鄧熙聖
Hsisheng Teng
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2019
畢業學年度： 107
語文別： 英文
論文頁數： 156
中文關鍵詞： Cathode material 、Hydrogen evolution reaction 、Single molecule 、Molybdenum disulfide 、Reaction rate 、Reaction Mechanism 、Hydrogen oxidation reaction
外文關鍵詞： Cathode material, Hydrogen evolution reaction, Single molecule, Molybdenum disulfide, Reaction rate, Reaction Mechanism, Hydrogen oxidation reaction
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    • 能源生產和儲存對社會的經濟增長至關重要。 科學界旨在開發替代能源、綠色能源和可再生能源。氫是最具吸引力和環境友好的能源之一。它以電解水生成時所需過電位最低因而成為主流研究領域之一，並且已經進行了許多研究工作。鉑（Pt）及其合金由於所需過電位較低是作為氫氣析出反應(HER)的先進電化學觸媒。 然而，其元素蘊藏量短缺和高成本主要限制其應用。最近，學者們正在努力用高元素豐度及廉價的過渡金屬硫化物、硒化物、氮化物和磷化物來代替鉑觸媒。
    對HER的非貴重材料是實際應用的基礎；然而，它們不能在較低的過電位下產生高電流密度為一大挑戰。目前來說，2D過渡金屬二硫化物（TMDs）因其在催化應用中的活性和穩定性而成為對HER主要的研究課題。
    在第一項工作中，我們製備了在cPAN分子上固定化硫化鉬單分子電催化劑(MoS2-cPAN)，它對HER具有高催化作用。首先，通過SPAN與Li金屬的電化學反應，在碳化PAN分子表面上形成Li2S-cPAN。接著，利用物種間的電位差使Li2S-cPAN與Mo離子反應後形成的cPAN分子表面上固定化單分子的硫化鉬。從結果來看，被固定化的硫化鉬單分子在EXAFS光譜上顯示明顯的鉬-硫鍵結但沒有金屬-金屬鍵結，理論估計其尺寸為1.31nm。硫化鉬單分子表面的低配位數和最大化利用率使得MoS2-cPAN在氫氣析出反應上以高100倍的交換電流密度（jo和TOF明顯優於塊材硫化鉬。

    在第二項研究中，通過誘導額外的活性位點或不對稱電荷轉移，將另一過渡金屬原子結合到MoS2納米薄膜來證明交換電流密度的增加。此方法中，MoSx-cPAN/Cu網狀電催化劑分別通過深層塗布和電化學技術在Cu網表面上沉積SPAN和Mo原子來製備。 然後，在惰性氣氛下以700℃進行熱處理。製備的MoSx-cPAN/Cu網狀電催化劑能夠在350mV的過電位下產生100 mA/cm2的電流密度。除了Mo原子的4d軌道的高空位之外，該活性歸因於CuS作為基質的形成。
    在第三項研究中，我們使用臨場拉曼技術研究氫氧化反應(HOR)的機制。目前尚未清楚地理解AEMFC中工作原理的反應機制。理解HER/HOR的鹼性反應機制對於設計析氫/氧化反應的催化劑是重要的。因此，我們使用臨場拉曼技術提出HOR在鹼性介質中的通用機制。 根據臨場拉曼光譜，在所有施加電位下發現了Pt觸媒表面上吸附的OH物質，且吸附的OH（OHad）的量隨過電位增加而增加。通過臨場拉曼光譜吸附OH物種數據，在碳乘載鉑觸媒電極上提出在酸鹼環境下，反應速率和氫氧化反應機理的關係。

    Energy production and its storage are vital for the economic growth of the society. Consequently, the scientific communities are intended to develop alternatives, green, and renewable energy. Hydrogen is one of the most attractive and environmentally benign energy. Its production electrochemically from water at lowest overpotential is one of a research area and many research efforts have been made. Platinum (Pt) and its alloys are the state of- the-art electrocatalysts for the hydrogen evolution at lower overpotential relatively. However, its shortage and high cost mainly limit its applications. Recently, scholars are striving to replace the precious Pt electrocatalysts with the earth-abundant and inexpensive transition metal of sulfides, selenides, nitrides, and phosphides.
    Non noble materials toward hydrogen evolution reaction (HER) are fundamental for practical implementation; however they are unable to produce high current density at lower overpotential as Pt metals. Now a day, 2D transition metal dichalcogenides (TMDs) are main research interest because of their activity and stability in applications of catalysis.
    Three approaches have been conducted in this research. In our first approach, immobilized single molecular MoS2 electrocatalyst on the surface of carbonized polyacrylonitrile (cPAN) was fabricated. It exhibits high catalysis toward HER. A single molecular MoS2 was prepared on the cPAN surface through electrochemical reaction of sulfur polyacrylonitrile (SPAN) with Li metal to form Li2S-cPAN. Then, the immobilized single molecular MoS2 on the surface of cPAN was formed after Li2S-cPAN reacting with Mo ions. The immobilized single MoS2 has no metal-metal scattering on the EXAFS spectra and it has a size of 1.31 nm. A low coordination number and maximum utilization of a single MoS2 molecule surface enable MoS2-cPAN to demonstrate electrochemical performance significantly better than that of bulk MoS2 by two orders of exchange current density (jo) and turnover frequency at the hydrogen evolution reaction.

    The second approach demonstrated the increasing of exchange current density by incorporating the transition metal atoms to MoS2 nanofilms composite by induces extra active site or asymmetric charge transfer. Herein, the MoSx- cPAN/Cu mesh electrocatalyst is prepared by the deposition of SPAN and Mo atoms on the surface of Cu mesh via deep coating and electrochemical techniques, respectively. Then, it is treated at 700 oC under inert atmosphere. The as prepared MoSx-cPAN/Cu mesh electrocatalyst able to produce 100 mA/cm2 at 350 mV. The activity is attributed from the formation of CuS as a matrix in addition to high vacancy of 4d orbital of Mo atom.
    In third approach, we studied the mechanism of hydrogen oxidation reaction using in situ Raman technique. The mechanisms for the reactions of the working principles in the AEMFC are not clearly understood yet. Understanding the mechanisms of HER/HOR is important to design appropriate catalyst for hydrogen evolution/oxidation reactions. Thus, herein we proposed universal mechanism of HOR in basic media using in situ Raman technique. From the spectra of in situ Raman, an adsorbed OH- species on Pt surface have been found at all applied potential and the amounts of adsorbed OH- (OHad) are increased with potentials. The rate of chemical reaction at equilibrium and the mechanism of hydrogen oxidation reaction have been proposed on Pt/C electrode from the data of adsorbed hydroxyl (OHad) species

    中文摘要 i Abstract iii Acknowledgments v Table of content vi List of Figures x List of Tables xvii List of Units and Abbreviation xviii Chapter 1: General Background 1 1.1 Energy, Its Sources and Storage 1 Chapter 2: Hydrogen Evolution /Oxidation Reaction (HER / HOR) 3 2.1. Methods of Hydrogen Evolution Reaction 4 2.1.1. Photocatalytic Water Splitting 4 2.1.2. Electrochemical Water Splitting 5 2.2. HER Activity Measuring Parameters 7 2.2.1. Onset overpotential and Overpotential 7 2.2.2. Exchange Current Density 8 2.2.3. Tafel slope 8 2.2.4. Turnover Frequency (TOF) 9 2.2.5. Gibbs free energy 10 2.3. Mechanism of HER /HOR 11 2.3.1. HER /HOR in Acidic Electrolyte 11 2.3.2. HER in Basic Electrolyte 12 2.3.3. HOR in Basic Electrolyte 13 2.4. Challenges of Hydrogen Evolution Reaction 14 2.5. Materials as Electrocatalyst for HER 15 2.5.1. Precious Metal Based Electrocatalyst 15 2.5.2. Non-Precious Metals and Their Alloys as Electrocatalyst 17 2.5.3. Transition Metal Carbide, Phosphides and Nitrides 18 2.5.4. Transition Metal Dichalcogenides (TMDCs) 20 2.5.5. Single Atom Catalysts (SACs) 25 2.6. Motivation and Objectives of the Study 29 2.6.1. Motivation 29 2.6.2. Objectives 30 Chapter 3: Experimental Section and Characterization 31 3.1 General Experimental Sections 31 3.1.1 Chemicals and Reagents 31 3.1.2 Synthesis of SPAN (Sulfur- Polyacrylonitrile) 32 3.1.3 Synthesis of Li2S-cPAN 34 3.1.4 Synthesis of MoS2-cPAN 34 3.1.5 Synthesis of MoSx-cPAN/Cu mesh 35 3.2 Sample Preparation for Characterizations and Measurements 37 3.3 Materials Structure Characterization 37 3.3.1 Physical Characterization Techniques 37 3.3.2 Electrochemical Measurement 39 Chapter 4: Synthesis of Single Molecular Molybdenum Disulfide on Carbonized Polyacrylonitrile for Cathode Electrolyzer 41 4.1 Introduction 41 4.2 Results and Discussion 42 4.2.1 Materials Characterization 42 4.2.2 Electrochemical Performance 58 4.3 Summary 64 Chapter 5: MoSx-cPAN/ Cu mesh as Efficient Electrocatalyst to Hydrogen Evolution Reaction 65 5.1 Introduction 65 5.2 Results and discussion 66 5.2.1 Material characterization 66 5.2.2 Electrochemical Performance 72 5.3 Summary 76 Chapter 6: Universal Rate Equation and Mechanism for Hydrogen Oxidation Reaction 77 6.1 Introduction 77 6.2 Results and Discussion 81 6.3 Summary 91 Chapter 7: Summary and Perspectives 92 7.1 Summary 92 7.2 Perspective 94 References 95 Appendices 125 Approach I 125 Approach II 129 Approach III 130 List of Research Papers 131 Conference Presentations 132

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