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http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/79267完整後設資料紀錄
| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 陳浩銘(Hao Ming Chen) | |
| dc.contributor.author | Chia-Jui Chang | en |
| dc.contributor.author | 張家睿 | zh_TW |
| dc.date.accessioned | 2022-11-23T08:57:01Z | - |
| dc.date.available | 2023-07-01 | |
| dc.date.available | 2022-11-23T08:57:01Z | - |
| dc.date.copyright | 2022-02-21 | |
| dc.date.issued | 2022 | |
| dc.date.submitted | 2022-01-21 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/79267 | - |
| dc.description.abstract | 為了因應氣候變遷，近年來科學家嘗試以電催化還原二氧化碳成可再利用的產物，並輔以再生能源以達成發展，因此如何有效地降低電催化二氧化碳還原的過電位以及提高其單一產物的選擇性是近年來相當熱門的議題，而了解催化劑在反應過程中的動態結構變化及價態改變對於發展高效能的催化劑是相當重要的，然而這方面詳盡的研究仍有待探討。 本研究論文著重於三個部分，首先，銅金屬是電催化二氧化碳還原中最重要的催化劑，但是近年來，科學家對於銅在進行反應時的價態改變與結構變化仍有待商榷，因此，我們藉由先進的臨場分析技術，發現電催化二氧化碳還原的產物選擇性與銅結構變化有想當大的關聯，當施加一定程度的還原電位後，我們發現銅原子穩定的還原價態有助於碳氫化合物與醇類的生成，因此我們推論在還原電位的環境之下，原子的動態價態會與二氧化碳還原做競爭反應，進而造成只有在穩定金屬銅價態下，碳氫化合物與醇類才能順利生成。 另外，雙金屬催化劑也能夠有效提升反應的選擇性以及活性，但是科學家們對於活性的提升往往歸咎於偕同效應的籠統概念，除此之外，他們往往忽略了催化劑在反應過程當中，可能會有結構重組的現象，對此我們以銅銀雙金屬的核殼結構去探討此一現象。藉由臨場X光繞射實驗分析，我們發現催化過程中，銀原子會擴散至銅原子上形成銅銀合金，此一特殊結構有利於提升甲烷產物的選擇性，再結合先前的實驗，我們推測銅銀合金的形成，源自於銅原子在低還原電位時的動態價態，當施予足夠的還原電位後，銅原子的還原過程將銀一同帶入形成銅銀合金，以利二氧化碳還原成甲烷。 最後我們重新探討銅在電催化二氧化碳還原時的價態，我們以雙金屬的銅鋅氧化物做為催化劑並使用脈衝電化學方法還原能夠有效提升活性，再以臨場快速吸收譜觀察後我們發現，脈衝電化學方法會將催化劑結構重組成分相的銅鋅結構，鋅會作為路易士酸使銅在還原電位下仍保有氧化價態，並在不施加還原電位時，強鹼的電解液能夠重新補充銅的氧化價態，我們認為在還原電位下穩定帶價態的銅是提升二碳產物的重要因素。 在本研究主題中，我們成功地解釋催化劑的結構變化對於活性以及產物分布造成的影響，提供電催化二氧化碳還原催化劑的設計構想。我們期望這些研究成果能夠對當前的環境問題提供些許幫助，讓人類未來的生活更美好。 | zh_TW |
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| dc.description.tableofcontents | "CONTENTS List of Figures………………………………………………………….……………..VII List of Tables……………………………...………………………………………XVIII Chapter 1. Background………………...…………………………………1 1.1 Introduction…………………………………………………………………………1 1.2 Electrochemical CO2 Reduction Reaction…………….…………………………...3 1.2.1 Overview of Electrochemical CO2 Reduction Reaction………………………....3 1.2.2 Products and Product Distribution under Different Applied Potentials...…….…..5 1.2.3 Mechanism of CO2RR …………………………………………………………7 1.2.4 Oxide-derived Copper Catalysts……………………………………………...11 1.2.5 Bimetallic Catalysts…………………………………………………….……..17 1.3 Research Motive……………………………………………………......……………22 1.4 References……………………………………………………………...……………25 Chapter 2. Characterization Techniques…………………….…………30 2.1 Scanning Electron Microscope (SEM)……………………………………………...30 2.2 Transmission Electron Microscope (TEM)…………………………...………….31 2.3 Energy-dispersive X-ray Spectroscopy…………………………………………...33 2.4 Electrochemical Measurements………………………………………..…………34 2.4.1 Linear Sweep Voltammetry ……………………………………………….34 2.4.2 Chronoamperometry……………………………………………...…………34 2.4.3 Faradaic Efficiency………………………………………………………..35 2.5 Electrochemical Cells……………………………………………………………36 2.6 Product Analysis…………………………………………………………………...39 2.6.1 Gas Chromatography …………………………………………....…………..39 2.6.2 Gas Chromatography-mass Spectrometry…………………………………40 2.7 In situ Techniques for Electrolysis………………………………………………41 2.7.1 Raman Spectroscopy……………………………………………..………..41 2.7.2 X-ray Diffraction……………………………………………………………42 2.7.3 X-ray Absorption Spectroscopy…………………………………….…………44 2.8 References…………………………………………………………………..……..47 Chapter 3. Quantitatively Unraveling the Redox Shuttle of Spontaneous Oxidation/Electroreduction of CuOx on Silver Nanowires Using in Situ X‑ray Absorption Spectroscopy…………………………………………48 3.1 Introduction…………………………………………………………………………49 3.2 Experimental Section……………………………………………………………53 3.2.1 Preparation of Catalysts……………………………………………………...53 3.2.2 Structural Characterization ……………………………………..…………...54 3.2.3 XAS Data Collection and Analysis…………………………….…………….55 3.2.4 EXAFS Fittings……………………………...…………………..…………..56 3.2.5 In situ Raman Characterization……………...………………………………57 3.2.6 Electrochemical Characterization……………………………...……...57 3.2.7 Analysis of the CO2 reduction Products……………………….…….59 3.3 Results and Discussion……………………………...………………………..……60 3.3.1 Structural Characterization…………………………………………….…….60 3.3.2 Catalytic Performance……………………...…………………………67 3.3.3 In situ XAS Characterization………………...………………………..73 3.3.4 In situ Raman Characterization………………..………………………86 3.3.5 Proposed Reoxidation of Cu under Cathodic Potentials……...…….....93 3.3.6 The Role of Silver Nanowire under CO2RR………………………...……….95 3.4 Conclusions………………………………………………………………...……....99 3.5 References………………………………………………………………….……..100 Chapter 4. Dynamic Reoxidation/reduction-Driven Atomic Interdiffusion for Highly Selective CO2 Reduction toward Methane………………….104 4.1 Introduction………………………………………………………………………105 4.2 Experimental Section………………………………………...……………..……109 4.2.1 Chemicals and Materials………………………………...…………………109 4.2.2 Synthesis of Cu Nanowires…………………………………………………109 4.2.3 Synthesis of Ag Nanowires…………………………………………………110 4.2.4 Synthesis of Cu100-XAgX Nanowires………………………………….…..110 4.2.5 Structural Characterization………………………………..………………..111 4.2.6 Operando X-ray Absorption Spectroscopy and in situ Grazing-angle X-ray Scattering Technique Analysis.…………..……………………………....111 4.2.7 In situ Raman Characterization………………………………….….112 4.2.8 Electrochemical Measurements……………………...……………..113 4.2.9 Analysis of the CO2 Reduction Performance………………………….….114 4.3 Results and Discussion……………………………………………..…………….115 4.3.1 Structural Characterization…………………………………………….…115 4.3.2 Electrochemical Properties toward CO2RR…………………..…………….123 4.3.3 In situ Grazing-angle X-ray Scattering Characterization……………......….132 4.3.4 Operando Chemical State and Tensile Strain Analyses……………………..137 4.3.5 Proposed Dynamic Reoxidation/reduction-driven Atomic Interdiffusion.....151 4.4 Conclusions…………………………………………………………………….....158 4.5 References…………………………………………………………………….......160 Chapter 5. Lewis Acid Universally Controls the Oxidation State of Cu during Pulsed Electrochemical CO2 Reduction with High Turnover Frequency for C2+ Products……………………………………………164 5.1 Introduction………………………………………………………………..………165 5.2 Experimental section……………………………………………………...…….…168 5.2.1 Chemicals and Materials……………………………………………...……...168 5.2.2 Synthesis of CuxZn0.2-x………………………………………………...……..168 5.2.3 Synthesis of Cu010Mn010, and Cu010Cd010…………………………………..169 5.2.4 Structural Characterization………………………………………….......……169 5.2.5 X-ray Absorption Spectroscopy……………………………………………170 5.2.6 Electrochemical Characterization……………………………………....……170 5.2.7 Analysis of the CO2 Reduction Products……………………………….…….171 5.3 Results and Discussion……………………………………………………….......172 5.3.1 Structural Characterization………………………………………………....172 5.3.2 CO2RR Performance Evaluation………….……...………………………...180 5.3.3 In situ XAS Investigation………………………………………………..…187 5.3.4 Proposed Structural Evolution…………………………………………….207 5.4 Conclusions…………………………………………………………….................211 5.5 Reference…………………………………………………………………...….....212 Chapter 6. Concluding Remarks……………………………………..…215 Appendix Curriculum Vitae……………………………………………………………….217 " | |
| dc.language.iso | zh-TW | |
| dc.title | 以臨場與非臨場技術分析電催化二氧化碳還原催化劑於反應時之結構變化對於活性之影響 | zh_TW |
| dc.title | Probing the Structural Transformation of Electrochemical CO2 Reduction Reaction Catalysts via In/Ex situ Analysis | en |
| dc.date.schoolyear | 110-1 | |
| dc.description.degree | 博士 | |
| dc.contributor.advisor-orcid | 陳浩銘(0000-0002-7480-9940) | |
| dc.contributor.oralexamcommittee | 洪崧富(Hsin-Tsai Liu),陳効謙(Chih-Yang Tseng),廖彥發,郭聰榮,林律吟,廖尉斯 | |
| dc.subject.keyword | 電催化二氧化碳還原反應,電化學,臨場分析,X光吸收譜,X光繞射譜, | zh_TW |
| dc.subject.keyword | Electrochemical CO2 Reduction Reaction,Electrocatalyst,Electrochemistry,In situ Analysis,X-ray Absorption Spectroscopy,X-ray Diffraction, | en |
| dc.relation.page | 218 | |
| dc.identifier.doi | 10.6342/NTU202104601 | |
| dc.rights.note | 同意授權(全球公開) | |
| dc.date.accepted | 2022-01-22 | |
| dc.contributor.author-college | 理學院 | zh_TW |
| dc.contributor.author-dept | 化學研究所 | zh_TW |
| dc.date.embargo-lift | 2023-07-01 | - |
| 顯示於系所單位： | 化學系 | |
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