二氧化碳电还原催化剂调控策略与结构效应

doi:10.1016/S1872-2067(21)63965-7

催化学报 ›› 2022, Vol. 43 ›› Issue (7): 1618-1633.DOI: 10.1016/S1872-2067(21)63965-7

• 二氧化碳催化转化专栏 • 上一篇下一篇

二氧化碳电还原催化剂调控策略与结构效应

刘聪^a^,^b, 梅轩豪^a^,^b, 韩策^a, 宫雪^a, 宋平^a^,^#(), 徐维林^a^,^b^,^*()

^a中国科学院长春应用化学研究所, 电分析化学国家重点实验室, 吉林省先进低碳化学电源重点实验室, 吉林长春130022
^b中国科学技术大学应用化学与工程学院, 安徽合肥230026

收稿日期:2021-09-30 接受日期:2021-10-16 出版日期:2022-07-18 发布日期:2022-05-20
通讯作者: 宋平,徐维林
基金资助:
国家重点研发计划(2017YFE0197900);国家重点研发计划(2018YFB1502302);国家自然科学基金(21925205);国家自然科学基金(21733004);国家自然科学基金(22072145)

Tuning strategies and structure effects of electrocatalysts for carbon dioxide reduction reaction

Cong Liu^a^,^b, Xuanhao Mei^a^,^b, Ce Han^a, Xue Gong^a, Ping Song^a^,^#(), Weilin Xu^a^,^b^,^*()

^aState Key Laboratory of Electroanalytical Chemistry, Jilin Province Key Laboratory of Low Carbon Chemical Power, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, Jilin, China
^bSchool of Applied Chemistry and Engineering, University of Science and Technology of China, Hefei 230026, Anhui, China.

Received:2021-09-30 Accepted:2021-10-16 Online:2022-07-18 Published:2022-05-20
Contact: Ping Song, Weilin Xu
Supported by:
National Key Research and Development Program of China(2017YFE0197900);National Key Research and Development Program of China(2018YFB1502302);National Natural Science Foundation of China(21925205);National Natural Science Foundation of China(21733004);National Natural Science Foundation of China(22072145)

摘要/Abstract

摘要：

随着化石燃料的消耗, 全球碳排放与日俱增, 由此引发的温室效应对全球气候变化带来巨大的挑战, 温室气体CO₂的减排与利用迫在眉睫. 利用太阳能、风能等可再生资源生产的电能能够将CO₂还原为一系列有附加值的化学品如醇、酸等有机小分子, 人为构造碳循环网络, 实现碳中和. 本文综述了电催化CO₂还原反应(CO₂RR)催化剂的调控策略和结构效应. 从本征结构和外部结构的角度阐述了催化剂活性位点的调控策略. 同时讨论了CO₂RR催化剂的结构效应, 如串联催化、协同效应和限域催化.

关于催化剂的调控策略, 从催化剂的本征结构和外部结构两方面总结了近年CO₂RR催化剂的研究进展. 特定的元素或化合物可以表现出不同的晶体结构, 造成局部电子结构差异. 而局部电子结构与催化剂的催化性能密切相关, 调整晶体结构成为本征结构调控的核心问题, 因此本文探讨了如何通过电化学方法和纳米晶体合成调节催化剂的本征结构. 与本征结构不同, 催化剂的外部结构与活性位点的微环境有关. 催化剂的外部结构调节主要基于各种电子结构的协同作用, 对活性组分的外部配位结构进行调节. 多种高效电催化剂的合成方法, 例如掺杂元素、有机分子改性, 甚至构建单原子材料都与活性位点的外部结构调节有关. 因此, 从无机元素掺杂和有机分子改性两方面讨论了外部结构调节对CO₂RR过程的影响. 与内在结构调节不同, 外部结构调节更多地依赖于对CO₂RR过程的理解, 因此本部分涉及了CO₂RR的反应机制.

关于催化剂的结构效应, 催化剂结构中的晶面、缺陷、空位等结构分因素会影响反应中间步骤进而改变催化活性, 由结构变化引发一系列催化效应, 如串联催化、协同效应和限域催化. 因此, 研究催化剂的结构效应可以从机理层面理解CO₂RR, 以便更好地设计催化剂. 本文从基本的中间体出发, 明确了*COOH和*OCHO两种中间体对于反应路径和产物趋势的影响. 同时讨论了多步催化反应过程中的串联催化机制, 在串联过程中, 不同的中间体可以在不同的活性位点之间转移. 与串联催化不同, 协同效应是不同活性位点之间的非线性累积效应. 在协同过程中, 不同的活性位点可以在一个基元步骤上协同工作. 串联机制和协同效应为催化剂设计提供了多种思路. 同时讨论了反应中间体限域对CO₂RR的调控.

最后本文总结了目前CO₂RR研究中面临的挑战, 包括催化剂的稳定性研究和单原子催化剂的开发, 以及机理研究中表征手段的一些欠缺, 为设计高效的CO₂RR电催化剂提供一定指导, 助力实现碳中和.

关键词: 电化学还原CO₂, 催化剂调控策略, 活性位点调控, 结构效应, 串联催化, 协同效应

Abstract:

Carbon dioxide emissions have increased due to the consumption of fossil fuels, making the neutralization and utilization of CO₂ a pressing issue. As a clean and efficient energy conversion process, electrocatalytic reduction can reduce carbon dioxide into a series of alcohols and acidic organic molecules, which can effectively realize the utilization and transformation of carbon dioxide. This review focuses on the tuning strategies and structure effects of catalysts for the electrocatalytic CO₂ reduction reaction (CO₂RR). The tuning strategies for the active sites of catalysts have been reviewed from intrinsic and external perspectives. The structure effects for the CO₂RR catalysts have also been discussed, such as tandem catalysis, synergistic effects and confinement catalysis. We expect that this review about tuning strategies and structure effects can provide guidance for designing highly efficient CO₂RR electrocatalysts.

Key words: CO₂RR, Tuning strategies, Active sites regulation, Structure effect, Tandem catalysis, Synergistic effect

刘聪, 梅轩豪, 韩策, 宫雪, 宋平, 徐维林. 二氧化碳电还原催化剂调控策略与结构效应[J]. 催化学报, 2022, 43(7): 1618-1633.

Cong Liu, Xuanhao Mei, Ce Han, Xue Gong, Ping Song, Weilin Xu. Tuning strategies and structure effects of electrocatalysts for carbon dioxide reduction reaction[J]. Chinese Journal of Catalysis, 2022, 43(7): 1618-1633.

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图/表 11

Fig. 1. (a) The time-dependent SEM images of Cu-CO2 and Cu-HER during electrodepositions. (b) The ratio of Cu(100) to Cu(111) facets, as measured by OH- electroadsorption; The error bars represent the standard deviation of three independent measurements. (a,b) Reproduced with permission from Ref. [34]. Copyright 2019, Springer Nature. TEM images of ED-Cu catalysts (c) and GB-Cu catalysts (d). Lines of orange dots indicate different orientations of the lattice. The XRD patterns (e) and XPS (f) of ED-Cu and GB-Cu catalysts as prepared. (g) FEs of both C2+ products for ED-Cu and GB-Cu. (c-g) Reproduced with permission from Ref. [33]. Copyright 2020, American Chemical Society.

Fig. 2. Fitting results of the operando EXAFS spectra to R space (a) and K space (b). The working electrode was biased at a few different potentials between the open circuit voltage (OCV) and 0.78 V vs. RHE during the measurements. (a,b) Reproduced with permission from Ref. [54]. Copyright 2019, Springer Nature. (c) CV scan (at 1 mV/s) of Cu foil in the prepared electrolyte (KOH solution, with 2.3 mol/L lactate ions, pH 13.7). (d) During SW treatment, the copper foil was subjected to alternate potentials of -0.45 and -0.75 V vs. SCE for 30 minutes. (e) Oxidation and reduction current densities during the SW treatment of Cu foil in the prepared electrolyte (3.2 mol/L KOH solution, with 2.3 mol/L lactate ions, 40 °C). (f) XRD pattern of SW-Cu2O/Cu, with a strong signal from Cu2O (111)-facets. (g) The aberration-corrected scanning transmission electron microscopy (STEM) image of a single nanoparticle on the SW-Cu2O/Cu surface. (h) The enlarged image of the region marked in (g). The corresponding fast Fourier transform (FFT) pattern shows the lattice spacing (0.248 nm) relevant to the orientation of Cu2O (111). (c-h) Reproduced with permission from Ref. [55]. Copyright 2020, American Chemical Society.

Fig. 3. (a) Based on the diameter of Ag nanocrystals, the percentage of different active sites. Reproduced with permission from Ref. [63]. Copyright 2020, American Chemical Society. (b) Atomic force microscopy (AFM) images of CuZn NPs with different compositions. From left to right are Cu100, Cu50Zn50, and Zn100 (For the symbol CuxZn100-x, X/100-X means the ratio of Cu to Zn. Scale bar: 200 nm). (c) Geometric current density and (d) products distribution (0.1 mol/L KHCO3, -1.35 V vs. RHE, 1 h electrolysis) as a function of the NP composition. (e) A time-dependent stability test of Cu50Zn50 NPs for the main products of CO2RR at -1.35 V vs. RHE. (c-e) Reproduced with permission from Ref. [67]. Copyright 2019, American Chemical Society.

Fig. 4. (a) TEM image of triangular Cu nanosheets. (b) AFM image of a single Cu nanosheet. (c) HRTEM image showing a Cu nanosheet in its basal plane. (d) The (111) peak is more prominent in the XRD pattern of Cu nanosheets deposited on a Si wafer; Inset: the selected area electron diffraction (SAED) pattern of copper nanosheets. (a-d) Reproduced with permission from Ref. [103]. Copyright 2019, Springer Nature. Typical (e) TEM image and (f) AFM image of Bismuthene. (g) The height profiles of three Bismuthene nanosheets shown in (f). (h) Typical lateral high angle annular dark-field scanning TEM (HAADF-STEM) image of a Bismuthene nanosheet, a zig-zag pattern directly displaying the single atom thickness. (e-g) Reproduced with permission from Ref. [115]. Copyright 2020, Springer Nature.

Fig. 5. Typical SEM image (a) and HRTEM image (b) of the F-Cu catalysts. (c) XPS of the F-Cu catalysts (Fluorine 1s). (d) The CO2RR energy diagram (C2H4 products) on Cu(111) and F-Cu(111), direct *CO dimerization or *CO hydrogenation (formation of *CHO) followed by dimerization. (e) A proposed CO2RR mechanism (C2H4 products); Purple, blue, red, grey, and white colours represent K, F, O, C, and H, respectively. (a-e) Reproduced with permission from Ref. [121]. Copyright 2020, Springer Nature. SEM image (f) and the corresponding HAADF-STEM image (g) of N-C/Cu. (h) Scheme of N-C/Cu/PTFE nanofibre; Green, yellow, and white colours represent N-C, copper, and PTFE, respectively. (i) The density of electrons for N-C/Cu with two adsorbed *COs and a charged water layer. Charge accumulations are indicated by yellow contours, and depressions by blue contours. (j) On Cu, C/Cu, and N-C/Cu, the CO dimerization energy profiles are shown for the initial states (IS), transition states (TS), and final states (FS). (f-j) Reproduced with permission from Ref. [122]. Copyright 2020, Springer Nature.

Fig. 6. (a) Illustration of the heterogenization of molecules on the Cu surface; Due to a local reaction environment with sufficient CO, the ethanol pathway on the Cu surface is preferred over the ethylene pathway. (b) Structure of iron porphyrin metal complexes. (a,b). Reproduced with permission from Ref. [129]. Copyright 2020, Springer Nature. (c) Investigated iron porphyrins. Reproduced with permission from Ref. [139]. Copyright 2012, The American Association for the Advancement of Science. (d) Results of the modifications of secondary ligands. (e) Synthesized Bipyridine-Mn Complexes with different ligand structures (number 1-8). (f) Products distribution of Bipyridine-Mn complexes (number 1-8) after 1 h CO2RR (at -2.17 V vs. Fc+/Fc in CO2-saturated 0.2 mol/L Bu4NBF4/MeCN). (g) Based on IR analysis, a catalytic cycle was proposed (CO2 to HCOOH); The formation of manganese-hydride intermediate (Mn-H) is a key step. (d-f) Reproduced with permission from Ref. [140]. Copyright 2020, American Chemical Society.

Fig. 7. (a) Ni-N4-TPP and Ni-N3O-TPP synthesized by modified Lindsey's methods. (b) 3D structure determined by single-crystal X-ray diffraction of Ni-N3O-TPP. (c) Ni K-edge XANES spectra; Red, blue, and dark lines represent Ni-N4-TPP, Ni-N3O-TPP, and Ni foil, respectively. (d) Polarization curves of Ni-N4-TPP and Ni-N3O-TPP (CO2 saturated 0.5 mol/L KHCO3 electrolyte, scan rate 50 mV s-1); Red and blue represent Ni-N4-TPP and Ni-N3O-TPP, respectively. (e) FECO and FETotal acquired at different potentials (in a two-compartment H-cell for 1 h). CV results of (f) Ni-N3O-TPP and (g) Ni-N4-TPP with different lower potential limit; Voltammograms were obtained by varying the lower potential limit from -0.5 to -0.8 VRHE (CO2 saturated 0.5 mol/L KHCO3 electrolyte, scan rate 50 mV s-1). Reproduced with permission from Ref. [170]. Copyright 2021, American Chemical Society.

Fig. 8. Reaction pathways for CO2RR. C, H, and O elements are represented by the black, grey, and red circles, respectively. The blue layer represent the catalytic surface.

Fig. 9. Various copper coverages on an Ag-Cu model catalyst. SEM images of Ag-Cu surfaces at Cu2+ concentrations of 0.5 ppm (a), 1.5 ppm (b), and 2.5 ppm (c). (d) Comparison of the FEs of Ag-Cu surfaces with different Cu coverages at -1.10 V (vs. RHE). At least three independent measurements are used to calculate the error bars. Operando attenuated total reflectance surface-enhanced infrared absorption spectroscopy (ATR-SEIRAS) studies of CO surface-adsorption on Cu, bare Ag, and Ag-Cu films. (e) Atop-bonded CO and (f) bridge-bonded CO on different surfaces under -0.4?V (vs. RHE). Reproduced with permission from Ref. [196]. Copyright 2019, Springer Nature.

Fig. 10. (a) Activation energies (at U = -0.9 V) of CO2 on MM (metallic matrix, blue), FOM (fully oxidized matrix, red), and MEOM (Cu metal embedded in the oxidized matrix, green) models, as well as the resulting chemisorbed CO2 structures. (b) The free energy profiles for CO dimerization (pH = 7) in MM, FOM, and MEOM models, and for CO hydrogenation to form surface *CHO species in MEOM (grey-green) models; The right image shows the surface OCCO structures, while the left image shows the initial structure from the MEOM simulation. Reproduced with permission from Ref. [199] Copyright 2017, American National Academy of Sciences. (c) A catalytic cycle with TPY-MOL-CoPP and BTB-MOL-CoPP for CO2RR; BTB-MOL and TPY-MOL were MOLs with triangular benzenetribenzoate (BTB) and 4′-(4-benzoate)-(2,2′,2″-terpyridine)-5,5″-dicarboxylate (TPY) sites, respectively. The DFT calculations also provide the pKa values and redox potentials. (d) The calculated HER and CO2RR energy profiles of TPY-MOL-CoPP and BTB-MOL-CoPP. Reproduced with permission from Ref. [130]. Copyright 2019, American Chemical Society.

Fig. 11. Plastron effects: trapping a layer of gas between the solution-solid interfaces with a hydrophobic surface; An illustration of this is shown on a diving bell spider (a) and a hydrophobic dendritic Cu surface (b) for subaquatic breathing and aqueous CO2 reduction; The photo of the diving bell spider is adapted from Seymour and Hetz [218] with permission from the company of biologists. The contact angle measurements of the (c) wettable and (d) hydrophobic dendrite. (e) HRTEM image of 1-octadecanethiol-treated Cu dendrite demonstrate the alkanethiol layer attached to the Cu surface. (a-e) Reproduced with permission from Ref. [216] Copyright 2019, Springer Nature. (f) Raman spectra of the multi-hollow Cu2O catalyst when 60 mA cm-2 of current is applied; At 2053 cm-1, a peak of *CO vibrations can be seen. (g) Cu+/Cu0 ratio calculated from Cu K-edge XAS at -0.61 V (vs. RHE). (f,g) Reproduced with permission from Ref. [217]. Copyright 2020, American Chemical Society.

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二氧化碳电还原催化剂调控策略与结构效应

Tuning strategies and structure effects of electrocatalysts for carbon dioxide reduction reaction

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