电催化CO2还原过程中非均相界面的动态行为

doi:10.1016/S1872-2067(23)64543-7

催化学报 ›› 2023, Vol. 53: 52-71.DOI: 10.1016/S1872-2067(23)64543-7

电催化CO₂还原过程中非均相界面的动态行为

申珅玉^a, 郭庆丰^b, 武甜甜^a^,^*(), 苏亚琼^a^,^*()

^a西安交通大学化学学院, 储能材料与器件教育部工程研究中心, 储能技术产教融合国家创新平台(中心), 陕西西安710049
^b黄河科技学院, 河南郑州450063

收稿日期:2023-07-29 接受日期:2023-09-20 出版日期:2023-10-18 发布日期:2023-10-25
通讯作者: *电子信箱: tianwu@xjtu.edu.cn (武甜甜); yqsu1989@xjtu.edu.cn (苏亚琼).
基金资助:
国家自然科学基金(22103059)

The dynamic behaviors of heterogeneous interfaces in electrocatalytic CO₂ reduction

Shenyu Shen^a, Qingfeng Guo^b, Tiantian Wu^a^,^*(), Yaqiong Su^a^,^*()

^aSchool of Chemistry, Engineering Research Center of Energy Storage Materials and Devices of Ministry of Education, National Innovation Platform (Center) for Industry-Education Integration of Energy Storage Technology, Xi'an Jiaotong University, Xi'an 710049, Shaanxi, China
^bHuanghe Science and Technology College, Zhengzhou 450063, Henan, China

Received:2023-07-29 Accepted:2023-09-20 Online:2023-10-18 Published:2023-10-25
Contact: *E-mail: tianwu@xjtu.edu.cn (T. Wu); yqsu1989@xjtu.edu.cn (Y. Su).
About author:Tiantian Wu received her Ph.D. from Technical University of Denmark in 2019, and then worked as a postdoc in Technical University of Denmark from 2019 to 2021. She also had an external stay at Prof. Núria López’s group in Institute of Chemical Research of Catalonia (ICIQ), the Barcelona Institute of Science and Technology. Now she is working as an assistant professor in Xi’an Jiaotong University. Her research area is computational catalysis in metal-air batteries, lithium-ion batteries, and electrocatalysis in solid fuel cells (SOECs).
Yaqiong Su received his Master degree from Xiamen University in 2014 and PhD degree from Eindhoven University of Technology in 2019, and then did his postdoctoral research at Eindhoven University of Technology in 2019. He worked as a visiting scholar in 2011-iChEM, Xiamen University from November 2019 to August 2020. He is now a distinguished professor and principal investigator at Xi’an Jiaotong University. His research involves theoretical chemistry, computational catalysis and spectroscopic electrochemistry.
Supported by:
The National Natural Science Foundation of China(22103059)

摘要/Abstract

摘要：

自工业革命以来, CO₂的过量排放导致了环境污染和气候变化, 对人类可持续发展造成了极大的威胁. 由可再生电力驱动的电催化CO₂还原反应(CO₂RR)技术可在较温和的条件下将CO₂转化为高附加价值的燃料和化学品, 因而是一种有效的CO₂转换和利用的方法. 尽管电催化CO₂RR已经取得了较大的研究进展, 但其工业化应用依旧面临着许多挑战: CO₂RR的反应路径涉及多步电子-质子转移, 其产物组分较复杂(包括C₁到C₃的产物), 并且反应过程伴随着析氢反应(HER)副反应发生. 此外, 不同电催化剂的使用以及实验操作条件均对CO₂RR影响较大, 导致目前CO₂RR催化剂性能尚不够理想, 因而难以获得实际应用. 为进一步开发性能良好的电催化CO₂RR体系, 以及认识实际反应过程中催化体系真正的活性位点, 理解电催化剂表面结构演变机制至关重要.

本文综述了CO₂RR条件下非均相催化界面的动态演变行为. 首先, 本文讨论了催化界面动态演变的原理和分类. 催化剂结构在实时工况下会发生演变, 导致活性位点难以确定, 因此需要明确催化界面动态演变的机制. 动态演变行为主要分为催化剂表面形态演变和性质演变: 表面形态演变主要指原子重排或迁移, 该过程由热力学和动力学驱动; 性质演变主要是化学态发生改变, 它是催化剂表面性质和外界环境共同作用的结果. 目前, 大多数的研究都围绕着催化剂表面和次表面活性位点展开, 所讨论的影响催化剂性质的因素主要包括化学组成、晶面和表面形态等. 除催化剂内在性质外, 还详细讨论了影响动态演变的外界环境因素, 包括外加电位、温度、电解质以及杂质等. 外加电位是影响催化界面的主要因素, 电解质中的阴阳离子也对反应选择性有较大的影响. 为了更好地认识反应过程中催化剂表面的活性位点, 总结了光谱表征、X射线表征、微观表征等技术在研究催化界面动态演变行为中的应用. 特别地, 脉冲CO₂电解技术可以调节催化界面的动态演变行为, 进而更好地调控反应的活性和选择性. 在此基础上, 理论模拟方法如密度泛函从头算和机器学习等方法, 可以模拟环境条件驱动下的催化剂表面重构, 为动态演变机制提供新的认识.

本文还总结了当前研究电催化还原CO₂反应界面的动态演变行为所面临的问题和挑战, 并展望了CO₂RR未来的研究方向.

关键词: CO₂还原反应, 动态行为, 活性位点, 外界环境, 电催化

Abstract:

The electrocatalytic CO₂ reduction reaction (CO₂RR) is a highly promising renewable energy technology that can convert greenhouse gases into valuable fuels and chemicals. However, under ordinary operating conditions, significant dynamic evolution behavior occurs on the catalyst surface, which is mainly manifested as surface morphology evolution and property changes, eventually leading to changes in the active sites of the reaction, affecting selectivity and efficiency. To develop efficient electrocatalytic systems with excellent performance, an essential prerequisite is to understand the underlying mechanism of surface dynamic evolution. Studying the influence of the external environment on dynamic evolution is as important as studying the intrinsic structural properties of catalysts. In this review, we first introduce the concept of dynamic evolution and then emphasize the influence of the external environment (applied potential, temperature, electrolyte, and impurities) on CO₂RR dynamic evolution. We also address the use of operando characterization techniques and pulsed CO₂ electrolysis methods for monitoring and controlling dynamic evolution behaviors under working conditions, along with theoretical methods, including ab initio calculations and machine learning that can simulate dynamic behavior. Finally, we present several current challenges and prospects for the development of techniques for controlling the CO₂RR dynamic evolution.

Key words: CO₂ reduction reaction, Dynamic behavior, Active site, External environment, Electrocatalysis

申珅玉, 郭庆丰, 武甜甜, 苏亚琼. 电催化CO₂还原过程中非均相界面的动态行为[J]. 催化学报, 2023, 53: 52-71.

Shenyu Shen, Qingfeng Guo, Tiantian Wu, Yaqiong Su. The dynamic behaviors of heterogeneous interfaces in electrocatalytic CO₂ reduction[J]. Chinese Journal of Catalysis, 2023, 53: 52-71.

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图/表 12

Fig. 1. (a) HAADF-STEM images and EDS elemental mapping of intermixed AgCu catalysts after the CO2RR has proceeded for 0, 0.5, 1, 3, 6, and 24 h. Scale bars in the top row, 50 nm; bottom row, 20 nm. Reprinted with permission from Ref. [25]. Copyright 2023, American Chemical Society. (b) Structural evolution of CuSiOx and CuO before and after the CO2RR at -1.4 V vs. RHE for 2 h. (c,d) Faradaic efficiencies (FEs) of the CO2RR products on CuO and CuSiOx at different potentials. Reprinted with permission from Ref. [27]. Copyright 2023, American Chemical Society. (e) TEM image after the introduction of Cu2O NPs of size 20 nm. (f) HRTEM image of Cu-based NPs after the CO2RR has proceeded for 10 h. (g) FEs of CO2RR products on fragmented Cu-based NP/C at different potentials. Reprinted with permission from Ref. [29]. Copyright 2019, American Chemical Society.

Fig. 2. (a) XANES spectra of Cu(pc) in CO2-saturated 0.1 mol L-1 KHCO3 as a function of the applied potentials. (b) EXAFS spectra of Cu(pc) thin-film electrode. Reprinted with permission from Ref. [31]. Copyright 2021, American Chemical Society. (c) EXAFS spectra of as-prepared Zn NPs. (d) EXAFS spectra of Zn NPs during CO2RR. Reprinted with permission from Ref. [38]. Copyright 2018, American Chemical Society. (e,f) The trend of methanol production and coordination numbers of In-O and In-In changes with the variation of TOS (time on stream). Reprinted with permission from Ref. [40]. Copyright 2019, American Chemical Society.

Fig. 3. High-resolution transmission electron microscopy (HR-TEM) images of ET-H (+1.2 VRHE) (a) and ET-L (+0.8 VRHE) (b) catalysts. ET refers to electrochemical treatment. The grain boundaries are highlighted with red lines. Reprinted with permission from Ref. [50]. Copyright 2022, American Chemical Society. (c) Grand free energy profiles of CO2 activation on Cu(100) through the SEPT and CPET mechanisms. Reprinted with permission from Ref. [54]. Copyright 2023, American Chemical Society. (d) Electrochemical scanning tunneling microscopy (EC-STM) images of polycrystalline copper surface at -0.9 V in 0.1 mol L-1 KOH. Reprinted with permission from Ref. [52]. Copyright 2014, American Chemical Society.

Fig. 4. Faradaic efficiency (in dark circles) and partial current density (in light squares) during CO2RR at different reaction temperatures in 0.1 mol L-1 KHCO3 at ?1.1 V vs. RHE for C2H4 (a) and H2 (b). (c) Carbon efficiency towards CO at ?1.1 V vs. RHE. SEM micrographs after CO2RR at -1.1 V vs. RHE at 25 °C (d), 48 °C (e) and 70 °C (f). Reprinted with permission from Ref. [61]. Copyright 2023, American Chemical Society.

Fig. 5. (a) CO2RR in 0.2 mol L-1 phosphate buffers with pH values of 1 and 7 on Cu(111) and Cu(100). Reprinted with permission from Ref. [82]. Copyright 2013, Elsevier. (b) Surface Pourbaix diagram under global thermodynamic equilibrium. The color bar represents the H coverage (in ML). (c) Root-mean-square deviation (RMSD) of the top-layer Cu positions during equilibrated 10 ps Born-Oppenheimer molecular dynamics (BOMD) simulations of the unrestructured surface with 0-, 1/6-, and 1/3-ML H coverage. (d) Key snapshots during an equilibrated 10 ps BOMD simulation of the 12 H state with an unrestructured initial configuration (the shifting row is highlighted by green or blue, before or after the shift). Reprinted with permission from Ref. [84]. Copyright 2022, American Chemical Society. (e) STEM-HAADF image of the surface of a Cu2O nanocube. The different atomic structures are labeled by regions I and II. Reprinted with permission from Ref. [41]. Copyright 2022, Elsevier. Time- and potential-dependent sequences of EC-STM images of Cu(111) at a pH of 13 (f) and 11 (g). Reprinted with permission from Ref. [86]. Copyright 2021, American Chemical Society.

Fig. 6. (a) The activity of CO generation in the presence of different cations. Reprinted with permission from Ref. [87]. Copyright 2021, American Chemical Society. (b,c) CV of the platinum ultramicroelectrode (Pt-UME) after CO2RR on gold and silver electrodes. Reprinted with permission from Ref. [88]. Copyright 2021, Springer Nature. (d-f) The partial current densities of the main products on Cu(100) in the presence of different cations. Reprinted with permission from Ref. [90]. Copyright 2017, American Chemical Society. (g-i) SEM images of electropolished Cu (EP-Cu), oxidized Cu (Ox-Cu), and Re-Cu-I. (j) FE of C2 products on Re-Cu-I, Re-Cu-Br, Re-Cu-Cl, and EP-Cu at different potentials. Reprinted with permission from Ref. [94]. Copyright 2020, Royal Society of Chemistry.

Fig. 7. (a) Pd-induced surface restructuring strategy. Reprinted with permission from Ref. [98]. Copyright 2017, John Wiley and Sons. (b,c) FEs of CO2RR products of pure CO2 and CO2/O2 at different applied potentials. Reprinted with permission from Ref. [107]. Copyright 2016, Elsevier. (d) BF-TEM image of Cu catalyst after electrolysis in CO2 + SO2 experiment. Reprinted with permission from Ref. [108]. Copyright 2019, American Chemical Society.

Fig. 8. (a) IR spectra at different applied potentials on Ag catalyst in CO2-saturated 0.1 mol L-1 KCl electrolyte. Reprinted with permission from Ref. [9]. Copyright 2017, American Chemical Society. (b,c) In situ SERS of Cu surface in CO2-saturated 0.1 mol L-1 KHCO3. Reprinted with permission from Ref. [121]. Copyright 2021, John Wiley and Sons. (d) A schematic of the developed operando Raman measurement system. (e) Operando Raman spectra of the peroxo O-O band evolution. Reprinted with permission from Ref. [122]. Copyright 2022, American Chemical Society.

Fig. 9. (a) In situ In K-edge XANES of InZr_7.1 at different temperatures in CO2 or reaction atmosphere. (b) The corresponding Fourier transformed EXAFS spectra of InZr_7.1. Reprinted with permission from Ref. [125]. Copyright 2019, American Chemical Society. (c,d) In situ XPS spectra of the Cu 2p3/2 and Zn 2p3/2 core level regions before and after 1 h of CO2RR. Reprinted with permission from Ref. [126]. Copyright 2019, American Chemical Society. (e) XRD patterns of intermixed AgCu particles after CO2RR. Reprinted with permission from Ref. [25]. Copyright 2023, American Chemical Society.

Fig. 10. (a) STEM-HAADF images of the morphology of Cu2O nanocubes at different stages. Reprinted with permission from Ref. [41]. Copyright 2022, Elsevier. (b,c) In situ EC-AFM images of electropolished Cu(100) surface at -0.5 and -1.0 V vs. RHE. Reprinted with permission from Ref. [57]. Copyright 2020, John Wiley and Sons. (d-f) AFM images that depict the surface morphologies of EP-Cu, E-ID-Cu and W-ID-Cu. Reprinted with permission from Ref. [129]. Copyright 2023, John Wiley and Sons.

Fig. 11. (a) FEs of CO2RR products on Cu electrode at constant potential and pulsed potential with different cathodic intervals (tc) and anodic intervals (ta). Reprinted with permission from Ref. [120]. Copyright 2018, John Wiley and Sons. (b) FEs of CO2RR products on Cu electrodes at constant potential and pulsed potential in a 0.1 mol L-1 KHCO3 electrolyte and a 0.1 mol L-1 KCl electrolyte. Reprinted with permission from Ref. [138]. Copyright 2020, John Wiley and Sons. (c-e) AFM images of Cu(100) electrode at constant potential and pulsed potential for different anodic potentials. Reprinted with permission from Ref. [131]. Copyright 2020, Springer Nature.

Fig. 12. (a,b) Grand potential interface energies of Cu surfaces with the adsorption of H and CO. (c) pH- and potential-dependent Wulff-shapes of Cu nanoparticles with different adsorbates covered. Reprinted with permission from Ref. [53]. Copyright 2018, Springer Nature. Dynamic evolution of the Cu-N bond length with adsorption of one H atom (d) and two H atoms (e). (f) Dynamic evolution of the bond length in the process of Cu atom aggregation. Reprinted with permission from Ref. [153]. Copyright 2022, American Chemical Society.

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电催化CO₂还原过程中非均相界面的动态行为

The dynamic behaviors of heterogeneous interfaces in electrocatalytic CO₂ reduction

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