CO2电还原反应中的基础问题及原位振动光谱的对策

doi:10.1016/S1872-2067(22)64095-6

催化学报 ›› 2022, Vol. 43 ›› Issue (11): 2772-2791.DOI: 10.1016/S1872-2067(22)64095-6

CO₂电还原反应中的基础问题及原位振动光谱的对策

李宏^a, 蒋昆^b, 邹受忠^c^,^#(), 蔡文斌^a^,^*()

^a复旦大学化学系, 能源材料化学协同创新中心, 上海市分子催化与功能材料表面重点实验室, 上海 200438, 中国
^b上海交通大学机械与动力工程学院, 上海 200240, 中国
^c美利坚大学化学系, 华盛顿, 美国

收稿日期:2022-04-30 接受日期:2022-07-27 出版日期:2022-11-18 发布日期:2022-10-20
通讯作者: 邹受忠,蔡文斌
基金资助:
国家自然科学基金(21733004);国家自然科学基金(22002088);上海市“科技创新行动计划”政府间国际科技合作基金项目(17520711200);上海市青年科技英才扬帆计划(20YF1420500)

Fundamental aspects in CO₂ electroreduction reaction and solutions from in situ vibrational spectroscopies

Hong Li^a, Kun Jiang^b, Shou-Zhong Zou^c^,^#(), Wen-Bin Cai^a^,^*()

^aShanghai Key Laboratory of Molecular Catalysis and Innovative Materials, Collaborative Innovation Center of Chemistry for Energy Materials, Department of Chemistry, Fudan University, Shanghai 200438, China
^bSchool of Mechanical Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
^cDepartment of Chemistry, American University, Washington, District of Columbia 20016, United States

Received:2022-04-30 Accepted:2022-07-27 Online:2022-11-18 Published:2022-10-20
Contact: Shou-Zhong Zou, Wen-Bin Cai
About author:Shouzhong Zou (Department of Chemistry, American University) earned his B.S. in Chemistry in 1991 and completed his MS studies in 1994 from Xiamen University under the guidance of Prof. Zhong-Qun Tian. He received his Ph.D. in Chemistry from Purdue University in 1999 under the direction of Prof. Michael J. Weaver. He then did postdoctoral work at Caltech with Profs. Fred C Anson and Ahmed H. Zewail. He started his independent research as an assistant professor in 2002 at Miami University (Oxford, Ohio), and was promoted to associate professor in 2008. He joined American University in the summer of 2015 as a full professor and chair. His research interests include developing catalysts for low temperature fuel cells, CO₂ reduction and gas sensing, and advancing spectroscopic and microscopic techniques for the characterization of surfaces and interfaces.
Wen-Bin Cai (Department of Chemistry, Fudan University) received his B.A. degree and M.S. degree from Shanghai University of Science and Technology in 1989 and 1992, respectively, under the guidance of Prof. Xun-Nan Deng and Ph.D. degree from Fudan University in 1995 under the guidance of Prof. Wei-Fang Zhou. From 1995 to 2002, he did postdoctoral research work consecutively at Xiamen University (with Prof. Zhong-Qun Tian), Hokkaido University (with Prof. Masatoshi Osawa), and Case Western Reserve University (with Profs. Daniel Scherson and James Burgess). Since July 2002, he has been a professor at Fudan University. His research interests cover interfacial spectroelectrochemistry and electrocatalysis, including but not limited to methodological development and application of electrochemical ATR-SEIRAS, mechanistic understanding and catalyst development towards electrocatalysis of small organic molecule oxidation, oxygen reduction and carbon dioxide reduction.
Supported by:
National Natural Science Foundation of China(21733004);National Natural Science Foundation of China(22002088);International Cooperation Program of Shanghai Science and Technology Committee(17520711200);Shanghai Sailing Program(20YF1420500)

摘要/Abstract

摘要：

近年来, 全世界达成了减少温室气体排放、防止气候恶化的共识. 二氧化碳电还原(CO₂RR)是利用可再生能源产生的电能将CO₂气体转化为高能量密度化学品的方案, 可实现CO₂的有效利用和可再生能源的存储, 是其实现碳循环的有效途径. CO₂RR过程涉及多个电子转移与质子耦合, 该反应体系复杂, 中间产物覆盖度低, 因此长期以来有关其电催化机理研究是一个挑战性难题. 同时, CO₂RR过程中催化剂结构演变、活性位点的识别、电解质的作用机制和吸附态CO角色等问题仍存在争议. 原位振动光谱可用于监测界面上CO₂还原反应过程中催化剂结构演变、捕获弱吸附的中间产物, 能够为理清反应机制和反应路径提供关键信息.

本综述介绍了原位振动光谱包括红外、拉曼和和频光谱等对CO₂RR中关键基本问题的解决策略, 主要包括: (1)揭示了不同电极上CO₂RR的反应中间体和反应路径; (2)探讨了CO在CO₂RR中的角色, 包括CO的吸附构型、覆盖度以及作为分子探针的作用; (3)明确了催化剂(主要Cu基催化剂)的结构与组成对CO₂RR活性和选择性的影响; (4)讨论了CO₂RR过程阴、阳离子对界面局部电场和pH, 以及反应中间体的影响.

CO₂RR过程的复杂性为该领域的研究带来了更多的挑战和机遇, 本文对原位振动光谱的未来发展和应用策略提出以下建议: (1)发展和应用能涵盖指纹区检测的高灵敏宽频红外光谱技术, 获取更多更可靠的中间物种和产物信息; (2)耦合多种原位和在线谱学方法深入揭示CO₂还原催化剂构效关系; (3)发展和应用适合于膜电极体系的振动光谱技术, 探索工况条件下的CO₂RR反应机制.

关键词: 二氧化碳电还原, 电催化机制, 振动光谱, 中间体, 构效关系, 电解质效应

Abstract:

Using renewable energy to drive carbon dioxide reduction reaction (CO₂RR) electrochemically into chemicals with high energy density is an efficient way to achieve carbon neutrality, where the effective utilization of CO₂and the storage of renewable energy are realized. The reactivity and selectivity of CO₂RR depend on the structure and composition of the catalyst, applied potential, electrolyte, and pH of the solution. Besides, multiple electron and proton transfer steps are involved in CO₂RR, making the reaction pathways even more complicated. In pursuit of molecular-level insights into the CO₂RR processes, in situ vibrational methods including infrared, Raman and sum frequency generation spectroscopies have been deployed to monitor the dynamic evolution of catalyst structure, to identify reactive intermediates as well as to investigate the effect of local reaction environment on CO₂RR performance. This review summarizes key findings from recent electrochemical vibrational spectrosopic studies of CO₂RR in addressing the following issues: the CO₂RR mechanisms of different pathways, the role of surface-bound CO species, the compositional and structural effects of catalysts and electrolytes on CO₂RR activity and selectivity. Our perspectives on developing high sensitivity wide-frequency infrared spectroscopy, coupling different spectroelectrochemical methods and implementing operando vibrational spectroscopies to tackle the CO₂RR process in pilot reactors are offered at the end.

Key words: Carbon dioxide electroreduction reaction, Electrocatalytic mechanism, Vibrational spectroscopy, Intermediate, Structure-performance relation, Electrolyte effect

李宏, 蒋昆, 邹受忠, 蔡文斌. CO₂电还原反应中的基础问题及原位振动光谱的对策[J]. 催化学报, 2022, 43(11): 2772-2791.

Hong Li, Kun Jiang, Shou-Zhong Zou, Wen-Bin Cai. Fundamental aspects in CO₂ electroreduction reaction and solutions from in situ vibrational spectroscopies[J]. Chinese Journal of Catalysis, 2022, 43(11): 2772-2791.

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图/表 11

Fig. 1. Fundamental issues for the electrochemical reduction of CO2.

Fig. 2. The schematic setup of electrochemical attenuated total reflection (ATR) infrared spectroscopy (a) and Raman spectrocopy (b). Reprinted with permission from Ref. [32]. Copyright 2020, Proceedings of the National Academy of Sciences. (c) Sum-frequency generation spectroscopy. Reprinted with permission from Ref. [33]. Copyright 2019, American Chemical Society. Note: WE refers to working electrode, RE to reference electrode and CE to counter electrode.

Fig. 3. Simplified flowchart of CO2RR mechanisms leading to C1 and C2+ product generation. * Corresponds to adsorbed species, > 2e- reduction products of CH4 and C2+ that go through the reduction of *CO intermediate (*COR) are marked in light blue. Reprinted with permission from Ref. [52]. Copyright 2020, American Chemical Society.

Fig. 4. (a) In situ time-dependent ATR-IR spectra of CO2RR on Sn electrodes at -1.4 V vs. Ag/AgCl in 0.1 mol/L K2SO4 solution saturated with CO2. The black arrow shows the direction of evolution with time and the red frame shows the carbonate species. Reprinted with permission from Ref. [53]. Copyright 2015, American Chemical Society. (b) ATR-IR spectra of thin films of indium, tin, lead, and bismuth on exposure to CO2 under reducing conditions. Reprinted with permission from Ref. [54]. Copyright 2016, American Chemical Society. In situ ATR-SEIRAS collected under different applied potentials in CO2 saturated (c) and Ar-saturated (d) 0.5 mol/L KHCO3. Reprinted with permission from Ref. [55]. Copyright 2020, John Wiley and Sons.

Fig. 5. (a) In situ SERS spectra of CO2RR at nanoporous Ag surfaces in 0.1 mol/L KHCO3 solution saturated with CO2. The arrow on the right shows the potential scanning direction. Peaks marked with black and red dashed lines are attributed to the reported and new SERS signals, respectively. Reprinted with permission from Ref. [64]. Copyright 2020, American Chemical Society. (b) Vibrational sum-frequency generation study of CO2RR at Pt/EMIM-BF4 interfaces. Reprinted with permission from Ref. [65]. Copyright 2016, Elsevier.

Fig. 6. (a) Simulated structures of possible adsorbates on Cu(100) for CO2RR and their calculated infrared-active vibrational frequencies. Cu, Li, C, O, and H atoms are depicted as orange, yellow, gray, red and white spheres. Reprinted with permission from Ref. [60]. Copyright 2017, John Wiley and Sons. (b) The vibrational density of states (v-DoSs) of *OC-CO, *OC-COH, *HOC-COH, *C-COH, *CH-COH, *C-CH, *C-CH2, and *C=C=O intermediate. In A2-G2, v-DoS from quantum mechanics molecular dynamics (QM-MD) is shown as a solid black line, the experimental frequencies are shown as a red dashed line, and the vibrational frequencies from v-QM optimization are shown as solid blue lines for comparison. Reprinted with permission from Ref. [51]. Copyright 2019, Proceedings of the National Academy of Sciences. (c) In situ Raman spectra in CO2-saturated 0.2 mol/L NaHCO3 for iodide-derived copper (ID-Cu) and oxide-derived copper (OD-Cu) samples shown the enlarged region between 850-1150 cm-1 at -1.0 V vs. Ag/AgCl. (d) The -CHx stretching region between 2700-3000 cm-1 at -0.8 V vs. Ag/AgCl. Reprinted with permission from Ref. [72]. Copyright 2020, John Wiley and Sons.

Fig. 7. The adsorption configuration of CO on metal electrodes and the corresponding positions in the vibrational spectrum.

Fig. 8. The schematic diagrams showing the roles of COtop and CObrigde on different electrodes. (a) Au electrode. Reprinted with permission from Ref. [84]. Copyright 2016, Proceedings of the National Academy of Sciences. (b) Pd electrode. Reprinted with permission from Ref. [85]. Copyright 2021, American Chemical Society. (c) Polycrystalline Cu electrode. Reprinted with permission from Ref. [82]. Copyright 2018, American Chemical Society. (d) Cu electrode with Cu(0) and Cu(I). Reprinted with permission from Ref. [86]. Copyright 2020, American Chemical Society.

Fig. 9. Schematic diagrams for the observed processes on anodic treatment of mechanically polished polycrystalline Cu electrode during CO2RR using in situ time-resolved surface-enhanced Raman spectroscopy. Reprinted with permission from Ref. [98]. Copyright 2021, John Wiley and Sons.

Fig. 10. Controversial views on OD-Cu catalysts during CO2RR. (a) Partially positive-charged copper (Cuδ+) is to boost the formation of highly valued multicarbon C2+ products during CO2RR. Reprinted with permission from Ref. [111]. Copyright 2020, American Chemical Society. (b) The electrochemical prereduction process, during which Cu2O nanocubes were converted into metallic Cu phase under a negative potential of -0.34 V vs. RHE. Reprinted with permission from Ref. [32]. Copyright 2020, Proceedings of the National Academy of Sciences of the United States of American. (c) Cu(100)/Cu(111) interfaces as superior active sites for CO dimerization during CO2RR. Reprinted with permission from Ref. [109]. Copyright 2021, American Chemical Society. (d) Role of a hydroxide layer on Cu electrodes in electrochemical CO2 Reduction. Reprinted with permission from Ref. [95]. Copyright 2019, American Chemical Society.

Fig. 11. (a) Schematic illustration of the effect of alkali metal cations on the local interfacial electric field on Cu electrodes. (b) Peak frequencies of the C≡O stretch band of linearly-bonded CO as a function of applied potential in CO-saturated 0.1 mol/L alkali metal bicarbonates as indicated. Reprinted with permission from Ref. [149]. Copyright 2017, The Royal Society of Chemistry. (c) Schematic illustration of the effect of alkali metal cations on local pH on Cu electrodes. (d) Steady-state pH at the metal-electrolyte interface during the electroreduction of CO2 at -1.0 V vs. RHE in CO2-saturated 0.05 mol/L M2CO3 solutions (M = Li+, Na+, K+, Cs+). Reprinted with permission from Ref. [154]. Copyright 2017, American Chemical Society.

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CO₂电还原反应中的基础问题及原位振动光谱的对策

Fundamental aspects in CO₂ electroreduction reaction and solutions from in situ vibrational spectroscopies

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