設計高選擇性、活性和穩定的電化學觸媒用於甲醇氧化和氧還原反應

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研究生：	Yohannes Ayele Awoke Yohannes Ayele Awoke
論文名稱：	設計高選擇性、活性和穩定的電化學觸媒用於甲醇氧化和氧還原反應 Designing highly Selective, Active, and Stable Electrochemical Catalysts for Methanol Oxidation and Oxygen Reduction Reactions
指導教授：	黃炳照 Bing-Joe Hwang 牟中原 Chung-Yuan Mou
口試委員:	黃炳照 Bing-Joe Hwang 牟中原 Chung-Yuan Mou 蘇威年 Wei-Nien Su 蔡孟哲 Meng-Che Tsai 王迪彥 Di-yan Wang
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：	2023
畢業學年度：	111
語文別：	英文
論文頁數：	152
中文關鍵詞：	單原子催化劑、甲醇氧化反應、雙活性位點、選擇性、H2O2 生產、雙核催化劑、2e-途徑ORR 、異功能、碳基、無金屬
外文關鍵詞：	Single-atom catalyst, methanol oxidation reaction, dual active sites, selectivity, H2O2 production, binuclear catalyst, 2e- pathway ORR, heterofunction, carbon-based, metal-free
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中文摘要
具備高活性、選擇性、穩定性和低成本的電催化劑在能源和化學合成工業中具有很大的需求。這些電催化劑中，單原子催化劑因其特殊性質可以在不同的電化學應用中滿足上述標準，例如氧氣還原反應(ORR)、二氧化碳還原反應(CO2RR)、氫氣析出反應(HER)、氧氣析出反應(OER)、氮還原反應(NRR) 和有機小分子氧化反應(如甲醇氧化(MOR)、甲酸氧化(FAOR))。本論文展示了三種用於MOR和2電子途徑ORR(2eORR)用於生產H2O2之電催化劑的方法。
在第一種方法中，鉑基催化劑和與其他元素合金化的奈米粒子被認為對MOR有效。然而，單原子態的Pt若負載在碳基載體上，則需要 Pt原子結合其他物種來完成甲醇氧化。因此，我們合成一個分散在雙摻雜TiO2上的Pt 單原子(Pt1/Ti0.8W0.2NxOy)作為有效且持久的MOR 催化劑。從量測的結果得知Pt1與載體表面WO3-x的雙活性位點之間的協同作用可允許甲醇吸附和脫氫。DFT研究證實，Pt1/Ti0.8W0.2NxOy中Pt1-WO3-x雙位點間的協同作用有助於提高催化活性、穩定性和選擇性。Pt1/Ti0.8W0.2NxOy催化劑展示了高 MOR效能，在鹼性介質中於0.82 V(vs. RHE)下具有 560 mA mg-1Pt的質量活性。該活性分別比20%Pt/C和同載體上的Pt奈米顆粒(2wt% Pt/Ti0.8W0.2NxOy)高9.3和1.3倍。從動力學上來講，在Pt1/Ti0.8W0.2NxOy上催化MOR更快，這由高的擴散係數1.5×10-12 cm2/s和低Tafel斜率(93 mV dec-1)所證實。此外，Pt1/Ti0.8W0.2NxOy以90%的法拉第效率選擇性地將甲醇氧化為甲酸鹽，而2wt% Pt1/Ti0.8W0.2NxOy以69%的選擇性將甲醇氧化為甲醛。此外，Pt1/Ti0.8W0.2NxOy的質量活性在穩定性測試10小時後僅下降了7.2%；而2wt% Pt/Ti0.8W0.2NxOy和20%Pt/C 的活性損失分別為 23% 和43%。
在第二種方法中，單原子催化劑在2eORR中比奈米粒子催化劑更有效，這是由於單原子催化劑的活性位點可使OOH反應中間體更合適地吸附在催化劑表面上，這阻礙了O-O鍵斷裂，提高了H2O2選擇性。非貴金屬單原子催化劑可成為2eORR的最佳選擇。然而，活性和選擇性仍然無法令人滿意。因此，設計高活性和選擇性的原子分散催化劑，用於通過 2eORR綠色合成全球需求最高的化學物質H2O2是一種很有前途的方法。在此研究中，我們通過配體介導的裂解過程開發了雙(N, O)配位的雙核鈷單原子催化劑作為高選擇性和高效的2eORR 催化劑(Co2N2O4/C)。結果發現，Co2N2O4/C催化劑在η ~ 0的寬電位範圍(0.1 V至0.7 V vs. RHE)下，對 2eORR具有近100%的優異H2O2選擇性。比較使用M-N4型催化劑Co Pc，Co2N2O4/C表現出高活性和高選擇性，且在12小時穩定性測試中活性損失可忽略不計。Co2N2O4/C催化劑還提供了高 H2O2生產率---在 H 型電池/流動電池中。在DFT計算研究中，雙核原子鈷催化劑，通過 N 和O配位進行電子結構修飾，在ORR物種吸附自由能與電位的火山型關係(Volcano plot)中，Co2N2O4具有最佳的 OOH*吸附能(4.21 eV)。這為通過 2電子途徑氧還原反應來高效生產過氧化物的電活性材料設計提供了見解。
在第三種方法中，雖然在第一和第二配位層中具有雜原子元素配位的非貴金屬單原子催化劑提供了高選擇性和H2O2的生產率，然而，非金屬催化劑(Metal-free catalyst)可以是一種成本低、資源豐富、且對2eORR具有高活性的潛力電催化劑。這項研究工作使用了精氨酸-水楊醛作為雜原子摻雜劑，並通過低溫熱裂解製備催化劑(Sal-Arg/C-300)。所製備的 Sal-Arg/C-300是一種雙雜原子(N, O)功能化碳材料，富含醚(環氧)和吡咯-N官能基團。與單氧或氮功能化的碳材料相比，Sal-Arg/C-300 在鹼性介質中的各種電位(0.1 - 0.7 V vs. RHE)中表現出顯著的ORR活性和近100% H2O2的選擇性。雜原子催化劑可以在 H型電解槽中以378 mmol h-1gcat-1 的優異速率生成H2O2，超過其他報導的碳基ORR催化劑。Sal-Arg/C-300 中的吡咯-N 和醚基 (C-O-C) 之間的協同作用與 2eORR活性和選擇性密切相關。這一發現為H2O2的電化學合成提供了巨大的潛力，為提供了一種低成本、豐富且高效的催化劑。

Abstract
Electrochemical catalysts with high activity, selectivity, stability, and low cost are highly demanding in the energy sector as well as in chemical synthesis industries. Among the catalyst groups, single-atom catalysts can fulfill the mentioned criteria in different electrochemical applications such as ORR, CO2RR, HER, OER, NRR, and small alcohol oxidations (MOR) formic acid oxidation if their coordination is well managed. This thesis has demonstrated three approaches for designing highly active, selective, and stable catalysts for MOR and two electron pathway ORR for H2O2 Production.
In the first approach, for MOR, platinum-based catalyst nanoparticles, nanocluster, alloyed with other elements are considered effective. However, Pt in a single atom state is effective for methanol oxidation since Pt ensembles are needed to complete methanol oxidation if supported on carbon-based support. So, we synthesize the first Pt single atom dispersed over dual-doped TiO2 (Pt1/Ti0.8W0.2NxOy) as an effective and long-lasting MOR catalyst. It has been discovered that synergy between Pt1-WO3-x dual-active sites allows for methanol adsorption and dehydrogenation. DFT studies confirmed the synergistic interactions between the Pt1-WO3-x dual active sites in Pt1/Ti0.8W0.2NxOy contribute to the high catalytic activity, stability, and selectivity. High MOR performance is demonstrated by the Pt1/Ti0.8W0.2NxOy catalyst, which has a mass activity of 560 mA mg-1Pt at 0.82 V vs. RHE in an alkaline medium. This activity is 9.3 and 1.3 times higher than the equivalent samples of 20% Pt/C and Pt nanoparticles (2wt% Pt/Ti0.8W0.2NxOy), respectively. Kinetically, MOR is faster on Pt1/Ti0.8W0.2NxOy than reference nanoparticle samples 20% Pt/C and 2wt% Pt/Ti0.8W0.2NxOy as confirmed by the higher diffusion coefficient of 1.5 x 10-12 cm2/s and lower Tafel slope 93 mV dec-1. Furthermore, Pt1/Ti0.8W0.2NxOy selectively oxidizes methanol to formate with 90% faradaic efficiency whereas, 2wt% Pt/Ti0.8W0.2NxOy oxidizes methanol to formaldehyde with 69% selectivity. Additionally, the mass activity of Pt1/Ti0.8W0.2NxOy only decreased by 7.2% after 10 hours of the stability test. However, activity loss in 2wt% Pt/Ti0.8W0.2NxOy and 20% Pt/C getting worsen with activity losses of 23% and 43 respectively.
In the second approach, Single-atom catalysts are more efficient than nanoparticle samples in a 2e- route ORR, since single-atom catalysts prefer ende on OOH- intermediate adsorption on the catalyst surface, which hinders O-O bond breaking, improve H2O2 selectivity. Non-precious transition metal single-atom catalysts become the best choice for 2e-route ORR. However, the activity and selectivity are still not satisfactory. So, designing highly active and selective atomically dispersed catalysts for green synthesis of the most globally demanding chemical H2O2 through ORR in a 2e- the pathway is a promising approach. Herein, we develop a dual (N, O) coordinated binuclear cobalt single-atom catalyst through a ligand-mediated pyrolysis process as highly selective and efficient ORR catalysts. It was found that the Co2N2O4/C catalyst has an outstanding selectivity of ~100% to a 2e- route ORR for the production of H2O2 in a wide range of Potentials (0.1v to 0.7 V vs.RHE) at η ~ 0. Compared with the M-N4 Type catalyst CoPC/C, Co2N2O4/C displays high activity, and selectivity, with negligible activity loss over 12 hours. The intended binuclear atom cobalt catalyst, electronically modified with N, and O coordination (Co2N2O4/C) possess an optimal OOH* intermediate adsorption energy at the volcano Peak (4.21 eV). This provided insights into the design of electroactive materials for efficient peroxide production through a 2e-path oxygen reduction
In the third approach, although non-precious single-atom catalysts with heteroatomic elemental coordination in the first and second coordination sphere provide high selectivity and production rate of H2O2, an electrocatalyst with low cost, abundant resources with high activity towards two-electron 2e- ORR still highly demanding. Metal-free carbon-based catalysts are the best alternative in this regard. This work reports a heteroatomic doped ordinary carbon as a metal-free catalyst (Sal-Arg/C-300) using arginine-salicylaldehyde as a heteroatomic dopant through in-situ doping at low-temperature pyrolysis. The as-prepared Sal-Arg/C-300 is a dual heteroatomic (N, O) functionalized carbon material rich in ether (epoxy) and pyrrolic-N functional groups. Sal-Arg/C-300 exhibits remarkable ORR activity and 100% H2O2 record selectivity in a wide range of potentials (0.1 - 0.7 V vs. RHE) in alkaline media compared to singly oxygen or nitrogen-functionalized carbon materials. The heteroatomic catalyst can produce H2O2 at a superior rate of 378 mmol h-1gcat-1 in an H-cell, surpassing other reported carbon-based ORR catalysts. Optimal *OOH adsorption energy achieved with the combination of Py-N and C-O-C functional groups on the carbon material through DFT calculation. The synergy between the pyrrolic-N and ether groups (C-O-C) in Sal-Arg/C-300 strongly correlates with its high ORR activity and selectivity in the 2e- ORR performance. This discovery offers significant potential for the electrochemical synthesis of H2O2, providing a low-cost, abundant, and highly efficient catalyst.

Table of Contents
中文摘要    i
Abstract    iii
Acknowledgment    vi
Index of figures    xi
Index of Tables    xviii
Index of Units and Abbreviations    xix
Chapter 1: General Background    1
1 Background of the Study    1
2. Electrochemical Oxidation of Small Molecular Weight Alcohols    2
2.1 Methanol Electrochemical Oxidation Reactions (MOR) for Energy Conversion    3
2.2. Methanol Electrochemical Oxidation Reactions (MOR)  for Value-added Product Synthesis    4
3.    Electrochemical Oxygen Reduction Reaction (ORR)    7
3.1.    H2O2 as a Valuable Product    8
Chapter 2. Development of Selective Electrocatalyst for MOR and H2O2 Production    11
1. Precious Metal-Based Catalyst for MOR    11
1.1. Carbon-Supported Pt-Based Catalyst for MOR    12
1.2. Metal Oxide Supported Pt-Based Electrocatalyst for MOR    13
1.2.1 Pt Nanoparticle  on the metal oxide support    13
1.2.2. Metal Oxide Supported Platinum Single-Atom Catalyst for MOR    16
2. Electrocatalyst for Selective ORR    18
2.1. Precious Metal Alloy and Single-Atom Catalysts for ORR    19
2.2. Non-Precious Metal Single-atom Catalysts for ORR    21
3. Metal-Free Catalysts for ORR    26
3.1. Oxygen doping    27
3.2. N doping    29
3.3. Multi-heteroatom codoping    32
4.    Motivation and Objectives of the Study    35
4.1.    Motivations    35
4.2 Objectives of the study    36
Chapter 3: Experimental Section and Characterization    39
1.  Chemicals and Reagents    39
2.  Synthesis of Dual Doped TiO2 (Ti0.8 W0.2NxOy) and Pt1/ Ti0.8 W0.2NxOy    40
3. Synthesis of Salicylidene-l-Alanine and bi-Atomic Cobalt Single Atom    40
4. Synthesis of Salicylidene-l-Arginine and Dual Functionalized (N, O) Metal-Free Carbon Catalyst (Sal-Agr/C-300)    41
5. Material Characterization Techniques    42
6. Electrochemical Measurements    44
6.1. Electrochemical (MOR) Performance of Pt1/Ti0.8W0.2NxOy    44
6.2. Electrochemical Performance of Co2N2O4/C    45
6.3. Electrochemical Performance of Sal-Agr/C-300    47
Chapter 4. The synergistic effect of Pt1-W dual sites as a highly active and durable catalyst for electrochemical methanol oxidation    49
1. Introduction    49
2. Result and Discussion    51
2.1 Synthesis and Morphology Characterization    51
2.2. Structural Composition and local structure Characterizations    56
2.3. Electrochemical Performance and Stability Test    63
2.4. MOR Mechanism    70
3. Summary    74
Chapter 5.  Boosting Catalytic Activity and Selectivity of 2e- ORR by Controlling The Local Coordination and the Atomic Nature of Cobalt Single Atom    77
1.Introduction    77
2. Result and Discussion    78
2.1. Synthesis and Characterization    78
2.2. Synthesis and Characterization of Co2N2O4/C    80
2.3 Structural and composition characterizations    82
2.4. Electrochemical Performance    88
2.5. Theoretical Prediction of Electrocatalytic Activity and Selectivity    90
3. Summary    92
Chapter 6: Tuning the synergy between the heteroatomic functionalities of carbon material as an efficient metal-free electrocatalyst for H2O2 production    93
1. Introduction    93
2. Result and Discussion    95
2.1. Material Synthesis and Characterization    95
2.1.1 Material physical characterizations    99
2.1.2 Structural and  Surface composition analysis    101
2.2 Electrochemical performance    110
2.3 Active Site Identification and Post-Electrochemical Surface Properties    115
2.4. Theoretical Calculations    117
3. Summary    118
Chapter 7. Conclusions and Perspectives    121
1 Conclusions    121
2 Perspective    122
References    125


                                

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