Visualizing CO₂ Electroreduction Dynamics: Advances in Electrochemical AFM for Catalyst Interfacial Analysis

Abstract

Electrochemical CO₂ reduction (CO₂RR) stands as a transformative pathway for the sustainable synthesis of fuels and chemicals, yet its advancement is hindered by an incomplete mechanistic picture of dynamic catalyst evolution at the electrode-electrolyte interface. This review emphasizes the critical role of in situ electrochemical atomic force microscopy (EC-AFM) in addressing this knowledge gap. As a non-invasive technique capable of nanometer- to near-atomic scale resolution under operando conditions, EC-AFM provides direct, real-time visualization of catalyst dynamics. The review begins by outlining the fundamental principles and advantages of EC-AFM for probing liquid-solid interfaces and then systematically demonstrates its applications across major catalyst systems. These range from revealing potential-dependent reconstruction and roughening on single-crystal and polycrystalline copper electrodes, to tracking the stability and synergistic effects in Cu-based bimetallic catalysts, and to elucidating structure-activity dynamics in emerging systems such as gas diffusion electrodes. Finally, we discuss current technical challenges of EC-AFM and propose future interdisciplinary research directions. This review summarizes how in situ EC-AFM has informed our understanding of CO₂RR by revealing dynamic catalyst reconstruction, tracking active-site evolution, and elucidating interfacial processes. By systematically compiling these advances, it serves as a critical interdisciplinary resource, positioning EC-AFM as a practical tool that offers visual guidance for the rational design of next-generation catalysts and electrochemical systems.

Keywords

catalyst dynamics / CO₂ reduction / EC-AFM / interfacial process

References

[1] A. Goldthau, “The G20 Must Govern the Shift to Low-Carbon Energy,” Nature 546, no. 7657 (2017): 203–205.

[2] Y. C. Liu, M. J. Shi, M. N. Han, et al., “Spontaneous Exfoliation and Tailoring Derived Oxygen-Riched Porous Carbon Nanosheets for Superior Li⁺ Storage Performance,” Chemical Engineering Journal 387 (2020): 124104.

[3] X. Liu, F. Wang, Y. Li, and X. Zhao, “Coupling Pretreatment of Lignocellulosic Biomass for Enzymatic Hydrolysis With Electrochemical Reduction of CO₂ for Production of Formic Acid,” Green Chemical Engineering 7, no. 1 (2026): 70–82.

[4] K. Z. Qi, S. Y. Liu, Y. J. Zhang, H. Zhang, V. Popkov, and O. Almjasheva, “CO₂ Electrolysis to Formic Acid for Carbon Neutralization,” Green Energy & Environment 9, no. 9 (2024): 1333–1335.

[5] A. D. Handoko, F. Wei, B. S. Jenndy, B. S. Yeo, and Z. W. Seh, “Understanding Heterogeneous Electrocatalytic Carbon Dioxide Reduction Through Operando Techniques,” Nature Catalysis 1, no. 12 (2018): 922–934.

[6] L. Fan, C. Xia, F. Yang, J. Wang, H. Wang, and Y. Lu, “Strategies in Catalysts and Electrolyzer Design for Electrochemical CO₂ Reduction Toward C₂₊ Products,” Science Advances 6, no. 8 (2020): eaay3111.

[7] W. Lai, Z. Ma, J. Zhang, Y. Yuan, Y. Qiao, and H. Huang, “Dynamic Evolution of Active Sites in Electrocatalytic CO₂ Reduction Reaction: Fundamental Understanding and Recent Progress,” Advanced Functional Materials 32, no. 16 (2022): 2111193.

[8] Y. Gong and T. He, “Gaining Deep Understanding of Electrochemical CO₂RR With In Situ/Operando Techniques,” Small Methods 7, no. 11 (2023): 2300702.

[9] Z. W. Seh, J. Kibsgaard, C. F. Dickens, I. Chorkendorff, J. K. Nørskov, and T. F. Jaramillo, “Combining Theory and Experiment in Electrocatalysis: Insights Into Materials Design,” Science 355, no. 6321 (2017): eaad4998.

[10] X. Y. Tan, C. Yu, Y. W. Ren, S. Cui, W. B. Li, and J. S. Qiu, “Recent Advances in Innovative Strategies for the CO₂ Electroreduction Reaction,” Energy & Environmental Science 14, no. 2 (2021): 765–780.

[11] J. Zhao, C. Fu, K. Ye, et al., “Manipulating the Oxygen Reduction Reaction Pathway on Pt-Coordinated Motifs,” Nature Communications 13, no. 1 (2022): 685.

[12] Y. Zhao, J. Raj, X. Xu, J. Jiang, J. Wu, and M. Fan, “Carbon Catalysts Empowering Sustainable Chemical Synthesis via Electrochemical CO₂ Conversion and Two-Electron Oxygen Reduction Reaction,” Small 21, no. 28 (2024): 2311163.

[13] M. Re Fiorentin, F. Risplendi, C. Salvini, J. Zeng, G. Cicero, and H. Jónsson, “Silver Electrodes Are Highly Selective for CO in CO₂ Electroreduction Due to Interplay Between Voltage Dependent Kinetics and Thermodynamics,” Journal of Physical Chemistry Letters 15, no. 46 (2024): 11538–11545.

[14] Y. R. Lei, Y. X. Niu, X. L. Tang, et al., “Cu-Based Materials for Electrocatalytic CO₂ to Alcohols: Reaction Mechanism, Catalyst Categories, and Regulation Strategies,” Journal of Energy Chemistry 97 (2024): 593–611.

[15] E. R. Cave, J. H. Montoya, K. P. Kuhl, et al., “Electrochemical CO₂ Reduction on Au Surfaces: Mechanistic Aspects Regarding the Formation of Major and Minor Products,” Physical Chemistry Chemical Physics 19, no. 24 (2017): 15856–15863.

[16] B. Sun, Z. Li, D. Xiao, et al., “Unveiling pH-Dependent Adsorption Strength of *CO₂⁻ Intermediate Over High-Density Sn Single Atom Catalyst for Acidic CO₂-To-HCOOH Electroreduction,” Angewandte Chemie International Edition 63, no. 14 (2024): e202318874.

[17] A. Kemna, N. García Rey, and B. Braunschweig, “Mechanistic Insights on CO₂ Reduction Reactions at Platinum/[BMIM][BF₄] Interfaces From In Operando Spectroscopy,” ACS Catalysis 9, no. 7 (2019): 6284–6292.

[18] M. Zhong, K. Tran, Y. Min, et al., “Accelerated Discovery of CO₂ Electrocatalysts Using Active Machine Learning,” Nature 581, no. 7807 (2020): 178–183.

[19] J. Huang, J. W. Dai, J. N. Zhu, et al., “Bimetallic Au-Cu Gradient Alloy for Electrochemical CO₂ Reduction Into C₂H₄ at Low Overpotential,” Journal of Catalysis 415 (2022): 134–141.

[20] H. Lei, W. Zhang, and J. Yang, “Theoretical Insights into Enhancing Catalytic Performance of Al-Cu Alloy for CO₂ Electroreduction Toward Ethene Production,” Journal of Physical Chemistry Letters 15, no. 21 (2024): 5643–5653.

[21] H. Shang, T. Wang, J. Pei, et al., “Design of a Single-Atom Indium^δ+-N₄ Interface for Efficient Electroreduction of CO₂ to Formate,” Angewandte Chemie International Edition 59, no. 50 (2020): 22465–22469.

[22] M. E. Moberg and C. W. Machan, “Design of Cr-Based Molecular Electrocatalyst Systems for the CO₂ Reduction Reaction,” Accounts of Chemical Research 57, no. 16 (2024): 2326–2335.

[23] M. C. Morrow and C. W. Machan, “Molecular Catalyst and Co-Catalyst Systems Based on Transition Metal Complexes for the Electrochemical Oxidation of Alcohols,” Chemical Communications 61, no. 43 (2025): 7710–7723.

[24] Z. Meng, J. Luo, W. Li, and K. A. Mirica, “Hierarchical Tuning of the Performance of Electrochemical Carbon Dioxide Reduction Using Conductive Two-Dimensional Metallophthalocyanine Based Metal-Organic Frameworks,” Journal of the American Chemical Society 142, no. 52 (2020): 21656–21669.

[25] X. F. Qiu, H. L. Zhu, J. R. Huang, P. Q. Liao, and X. M. Chen, “Highly Selective CO₂ Electroreduction to C₂H₄ Using a Metal-Organic Framework With Dual Active Sites,” Journal of the American Chemical Society 143, no. 19 (2021): 7242–7246.

[26] M. Lu, M. Zhang, C. G. Liu, et al., “Stable Dioxin-Linked Metallophthalocyanine Covalent Organic Frameworks (COFs) as Photo-Coupled Electrocatalysts for CO₂ Reduction,” Angewandte Chemie International Edition 60, no. 9 (2021): 4864–4871.

[27] F. Li, H. Tariq, H. Yang, Y. Cao, T. Zhou, and G. Wang, “Steering Electrochemical CO₂ Reduction Selectivity Toward CH₄ or C₂H₄ on N-Doped Carbon-Coated Cu/Cu₂O Composite Catalysts,” ACS Catalysis 14, no. 20 (2024): 15088–15095.

[28] C. Xie, W. Chen, Y. Wang, Y. Yang, and S. Wang, “Dynamic Evolution Processes in Electrocatalysis: Structure Evolution, Characterization and Regulation,” Chemical Society Reviews 53, no. 22 (2024): 10852–10877.

[29] X. Song, L. Xu, X. Sun, and B. Han, “In Situ/Operando Characterization Techniques for Electrochemical CO₂ Reduction,” Science China Chemistry 66, no. 2 (2023): 315–323.

[30] K. G. Schmitt and A. A. Gewirth, “In Situ Surface-Enhanced Raman Spectroscopy of the Electrochemical Reduction of Carbon Dioxide on Silver With 3,5-Diamino-1,2,4-Triazole,” Journal of Physical Chemistry C 118, no. 31 (2014): 17567–17576.

[31] E. Pérez-Gallent, M. C. Figueiredo, F. Calle-Vallejo, and M. T. M. Koper, “Spectroscopic Observation of a Hydrogenated CO Dimer Intermediate During CO Reduction on Cu(100) Electrodes,” Angewandte Chemie International Edition 56, no. 13 (2017): 3621–3624.

[32] X. Zhou, J. Shan, L. Chen, et al., “Stabilizing Cu²⁺ Ions by Solid Solutions to Promote CO₂ Electroreduction to Methane,” Journal of the American Chemical Society 144, no. 5 (2022): 2079–2084.

[33] J. Timoshenko and B. Roldan Cuenya, “In Situ/Operando Electrocatalyst Characterization by X-Ray Absorption Spectroscopy,” Chemical Reviews 121, no. 2 (2021): 882–961.

[34] J. Wang, C. S. Hsu, T. S. Wu, et al., “In Situ X-Ray Spectroscopies beyond Conventional X-Ray Absorption Spectroscopy on Deciphering Dynamic Configuration of Electrocatalysts,” Nature Communications 14, no. 1 (2023): 6576.

[35] A. Zhang, Y. Liang, H. Li, et al., “In Situ Surface Reconstruction of InN Nanosheets for Efficient CO₂ Electroreduction Into Formate,” Nano Letters 20, no. 11 (2020): 8229–8235.

[36] C. L. Bentley, M. Kang, and P. R. Unwin, “Nanoscale Surface Structure-Activity in Electrochemistry and Electrocatalysis,” Journal of the American Chemical Society 141, no. 6 (2019): 2179–2193.

[37] V. Beermann, M. E. Holtz, E. Padgett, J. F. de Araujo, D. A. Muller, and P. Strasser, “Real-Time Imaging of Activation and Degradation of Carbon Supported Octahedral Pt-Ni Alloy Fuel Cell Catalysts at the Nanoscale Using In Situ Electrochemical Liquid Cell STEM,” Energy & Environmental Science 12, no. 8 (2019): 2476–2485.

[38] X. Wang, K. Klingan, M. Klingenhof, et al., “Morphology and Mechanism of Highly Selective Cu(II) Oxide Nanosheet Catalysts for Carbon Dioxide Electroreduction,” Nature Communications 12, no. 1 (2021): 794.

[39] R. M. Arán-Ais, R. Rizo, P. Grosse, et al., “Imaging Electrochemically Synthesized Cu₂O Cubes and Their Morphological Evolution Under Conditions Relevant to CO₂ Electroreduction,” Nature Communications 11, no. 1 (2020): 3489.

[40] J. Kim, C. Renault, N. Nioradze, N. Arroyo-Currás, K. C. Leonard, and A. J. Bard, “Electrocatalytic Activity of Individual Pt Nanoparticles Studied by Nanoscale Scanning Electrochemical Microscopy,” Journal of the American Chemical Society 138, no. 27 (2016): 8560–8568.

[41] T. Sun, Y. Yu, B. J. Zacher, and M. V. Mirkin, “Scanning Electrochemical Microscopy of Individual Catalytic Nanoparticles,” Angewandte Chemie International Edition 53, no. 51 (2014): 14120–14123.

[42] D. Cheng, Z. Wei, Z. Zhang, P. Broekmann, A. N. Alexandrova, and P. Sautet, “Restructuring and Activation of Cu(111) Under Electrocatalytic Reduction Conditions,” Angewandte Chemie International Edition 62, no. 20 (2023): e202218575.

[43] Y. Q. Wang, J. Fu, Y. Feng, et al., “Alkali Metal Cations Induce Structural Evolution on Au(111) During Cathodic Polarization,” Journal of the American Chemical Society 146, no. 40 (2024): 27713–27724.

[44] Y. Q. Wang and D. Wang, “Electrochemical Scanning Tunneling Microscopy in Electrocatalysis,” Current Opinion in Electrochemistry 46 (2024): 101512.

[45] X. Deng and J. Liu, “Probing Electrochemical CO₂ Reduction: Insights From In Situ Scanning Probe Microscopy,” Chemsuschem 19, no. 1 (2026): e202501581.

[46] J. Limb, L. F. Gaudin, and C. L. Bentley, “Structure-Dependent CO₂ Reduction on Molybdenite (MoS₂) Electrocatalysts,” Chemical Communications 60, no. 36 (2024): 4781–4784.

[47] B. Bhushan, “Nanotribology and Nanomechanics,” Wear 259 (2005): 1507–1531.

[48] W. W. Wang, H. Yan, Y. Gu, J. W. Yan, and B. W. Mao, “In Situ Electrochemical Atomic Force Microscopy: From Interfaces to Interphases,” Annual Review of Analytical Chemistry 17 (2024): 103–126.

[49] Y. X. Zhong, J. W. Yan, M. G. Li, X. Zhang, D. W. He, and B. W. Mao, “Resolving Fine Structures of the Electric Double Layer of Electrochemical Interfaces in Ionic Liquids With an AFM Tip Modification Strategy,” Journal of the American Chemical Society 136, no. 42 (2014): 14682–14685.

[50] W. W. Wang, Y. Gu, H. Yan, et al., “Evaluating Solid-Electrolyte Interphases for Lithium and Lithium-Free Anodes From Nanoindentation Features,” Chem 6, no. 10 (2020): 2728–2745.

[51] Z. Z. Shen, X. S. Zhang, J. Wan, et al., “Nanoscale Visualization of Lithium Plating/Stripping Tuned by On-Site Formed Solid Electrolyte Interphase in All-Solid-State Lithium-Metal Batteries,” Angewandte Chemie International Edition 63, no. 13 (2024): e202316837.

[52] S. Manne, P. K. Hansma, J. Massie, V. B. Elings, and A. A. Gewirth, “Atomic-Resolution Electrochemistry With the Atomic Force Microscope: Copper Deposition on Gold,” Science 251 (1991): 183–186.

[53] J. L. Li, Y. N. Wang, S. Y. Sun, et al., “Understanding and Regulating the Mechanical Stability of Solid Electrolyte Interphase in Batteries,” Advanced Energy Materials 15, no. 4 (2025): 2403845.

[54] H. L. Thaman, M. Li, J. A. Rose, et al., “Two-Stage Growth of Solid Electrolyte Interphase on Copper: Imaging and Quantification by Operando Atomic Force Microscopy,” ACS Nano 19, no. 12 (2025): 11949–11960.

[55] W. Zheng, “Spatiotemporal Visualisation of Electrocatalyst/Electrolyte Interfaces With Electrochemical Atomic Force Microscopy: Applications and Notes,” Journal of Microscopy 302, no. 1 (2025): 5–16.

[56] P. Grosse, D. Gao, F. Scholten, I. Sinev, H. Mistry, and B. Roldan Cuenya, “Dynamic Changes in the Structure, Chemical State and Catalytic Selectivity of Cu Nanocubes During CO₂ Electroreduction: Size and Support Effects,” Angewandte Chemie International Edition 57, no. 21 (2018): 6192–6197.

[57] H. Wang, L. D. B. Mandemaker, J. de Ruiter, X. Yu, W. van der Stam, and B. M. Weckhuysen, “Identical Grain Atomic Force Microscopy Elucidates Facet-Dependent Restructuring of Copper for CO₂ Electroreduction,” Angewandte Chemie International Edition 64, no. 16 (2025): e202424530.

[58] P. De Luna, C. Hahn, D. Higgins, S. A. Jaffer, T. F. Jaramillo, and E. H. Sargent, “What Would It Take for Renewably Powered Electrosynthesis to Displace Petrochemical Processes?,” Science 364, no. 6438 (2019): eaav3506.

[59] R. Reske, H. Mistry, F. Behafarid, B. Roldan Cuenya, and P. Strasser, “Particle Size Effects in the Catalytic Electroreduction of CO₂ on Cu Nanoparticles,” Journal of the American Chemical Society 136, no. 19 (2014): 6978–6986.

[60] R. M. Arán-Ais, D. Gao, and B. Roldan Cuenya, “Structure- and Electrolyte-Sensitivity in CO₂ Electroreduction,” Accounts of Chemical Research 51, no. 11 (2018): 2906–2917.

[61] W. Zhu, R. Michalsky, Ö. Metin, et al., “Monodisperse Au Nanoparticles for Selective Electrocatalytic Reduction of CO₂ to CO,” Journal of the American Chemical Society 135, no. 45 (2013): 16833–16836.

[62] S. Popović, M. Smiljanić, P. Jovanovič, J. Vavra, R. Buonsanti, and N. Hodnik, “Stability and Degradation Mechanisms of Copper-Based Catalysts for Electrochemical CO₂ Reduction,” Angewandte Chemie International Edition 59, no. 35 (2020): 14736–14746.

[63] J. Kok, P. P. Albertini, J. Leemans, R. Buonsanti, and T. Burdyny, “Overcoming Copper Stability Challenges in CO₂ Electrolysis,” Nature Reviews Materials 10, no. 7 (2025): 550–563.

[64] K. J. P. Schouten, E. Pérez Gallent, and M. T. M. Koper, “Structure Sensitivity of the Electrochemical Reduction of Carbon Monoxide on Copper Single Crystals,” ACS Catalysis 3, no. 6 (2013): 1292–1295.

[65] F. Calle-Vallejo and M. T. M. Koper, “Theoretical Considerations on the Electroreduction of CO to C₂ Species on Cu(100) Electrodes,” Angewandte Chemie International Edition 52, no. 28 (2013): 7282–7285.

[66] J. H. Montoya, C. Shi, K. Chan, and J. K. Nørskov, “Theoretical Insights Into a CO Dimerization Mechanism in CO₂ Electroreduction,” Journal of Physical Chemistry Letters 6, no. 11 (2015): 2032–2037.

[67] F. S. Roberts, K. P. Kuhl, and A. Nilsson, “High Selectivity for Ethylene From Carbon Dioxide Reduction Over Copper Nanocube Electrocatalysts,” Angewandte Chemie International Edition 54, no. 17 (2015): 5179–5182.

[68] I. Zegkinoglou, A. Zendegani, I. Sinev, et al., “Operando Phonon Studies of the Protonation Mechanism in Highly Active Hydrogen Evolution Reaction Pentlandite Catalysts,” Journal of the American Chemical Society 139, no. 41 (2017): 14360–14363.

[69] D. Gao, I. Zegkinoglou, N. J. Divins, et al., “Plasma-Activated Copper Nanocube Catalysts for Efficient Carbon Dioxide Electroreduction to Hydrocarbons and Alcohols,” ACS Nano 11, no. 5 (2017): 4825–4831.

[70] G. H. Simon, C. S. Kley, and B. Roldan Cuenya, “Potential-Dependent Morphology of Copper Catalysts During CO₂ Electroreduction Revealed by In Situ Atomic Force Microscopy,” Angewandte Chemie International Edition 60, no. 5 (2021): 2561–2568.

[71] K. J. P. Schouten, Z. Qin, E. Pérez Gallent, and M. T. M. Koper, “Two Pathways for the Formation of Ethylene in CO Reduction on Single-Crystal Copper Electrodes,” Journal of the American Chemical Society 134, no. 24 (2012): 9864–9867.

[72] G. L. De Gregorio, T. Burdyny, A. Loiudice, P. Iyengar, W. A. Smith, and R. Buonsanti, “Facet-Dependent Selectivity of Cu Catalysts in Electrochemical CO₂ Reduction at Commercially Viable Current Densities,” ACS Catalysis 10, no. 9 (2020): 4854–4862.

[73] S. Nitopi, E. Bertheussen, S. B. Scott, et al., “Progress and Perspectives of Electrochemical CO₂ Reduction on Copper in Aqueous Electrolyte,” Chemical Reviews 119, no. 12 (2019): 7610–7672.

[74] J. Wang, H. Y. Tan, Y. Zhu, H. Chu, and H. M. Chen, “Linking the Dynamic Chemical State of Catalysts With the Product Profile of Electrocatalytic CO₂ Reduction,” Angewandte Chemie International Edition 60, no. 32 (2021): 17254–17267.

[75] X. Yuan, S. Chen, D. Cheng, et al., “Controllable Cu⁰-Cu⁺ Sites for Electrocatalytic Reduction of Carbon Dioxide,” Angewandte Chemie International Edition 60, no. 28 (2021): 15344–15347.

[76] Z. Q. Liang, T. T. Zhuang, A. Seifitokaldani, et al., “Copper-on-Nitride Enhances the Stable Electrosynthesis of Multi-Carbon Products From CO₂,” Nature Communications 9 (2018): 3828.

[77] G. J. Liu, M. Lee, S. Kwon, et al., “CO₂ Reduction on Pure Cu Produces Only H₂ After Subsurface O Is Depleted: Theory and Experiment,” Proceedings of the National Academy of Sciences of the United States of America 118, no. 23 (2021): e2012649118.

[78] S. H. Lee, N. Devi, Y. Li, et al., “Formate-Induced Dissolution and Reprecipitation of a Copper Electrocatalyst During Electrochemical CO₂ Reduction Reaction,” Journal of Physical Chemistry C 129, no. 40 (2025): 18011–18024.

[79] Y. Peng, C. Zhan, H. S. Jeon, W. Frandsen, B. R. Cuenya, and C. S. Kley, “Organic Thin Films Enable Retaining the Oxidation State of Copper Catalysts During CO₂ Electroreduction,” ACS Applied Materials & Interfaces 16, no. 5 (2024): 6562–6568.

[80] Y. Yue, Z. Wu, Z. Ye, et al., “Identifying Cu Reconstruction Mechanism in CO₂ and CO Electroreduction via Cu⁺ Detection and In Situ Atomic Force Microscopy,” Science China Materials 68, no. 7 (2025): 2381–2387.

[81] A. Vasileff, C. Xu, Y. Jiao, Y. Zheng, and S. Z. Qiao, “Surface and Interface Engineering in Copper-Based Bimetallic Materials for Selective CO₂ Electroreduction,” Chem 4, no. 8 (2018): 1809–1831.

[82] C. Zhu, S. Zhao, G. Shi, and L. Zhang, “Structure-Function Correlation and Dynamic Restructuring of Cu for Highly Efficient Electrochemical CO₂ Conversion,” Chemsuschem 15, no. 7 (2022): e202200068.

[83] D. Ren, B. S. H. Ang, and B. S. Yeo, “Tuning the Selectivity of Carbon Dioxide Electroreduction Toward Ethanol on Oxide-Derived Cu_xZn Catalysts,” ACS Catalysis 6, no. 12 (2016): 8239–8247.

[84] S. Ma, M. Sadakiyo, M. Heima, et al., “Electroreduction of Carbon Dioxide to Hydrocarbons Using Bimetallic Cu-Pd Catalysts With Different Mixing Patterns,” Journal of the American Chemical Society 139, no. 1 (2017): 47–50.

[85] J. Huang, M. Mensi, E. Oveisi, V. Mantella, and R. Buonsanti, “Structural Sensitivities in Bimetallic Catalysts for Electrochemical CO₂ Reduction Revealed by Ag-Cu Nanodimers,” Journal of the American Chemical Society 141, no. 6 (2019): 2490–2499.

[86] Y. Lum and J. W. Ager, “Sequential Catalysis Controls Selectivity in Electrochemical CO₂ Reduction on Cu,” Energy & Environmental Science 11, no. 10 (2018): 2935–2944.

[87] M. Liu, Y. Pang, B. Zhang, et al., “Enhanced Electrocatalytic CO₂ Reduction via Field-Induced Reagent Concentration,” Nature 537, no. 7620 (2016): 382–386.

[88] M. Munz, J. Poon, W. Frandsen, B. R. Cuenya, and C. S. Kley, “Nanoscale Electron Transfer Variations at Electrocatalyst-Electrolyte Interfaces Resolved by In Situ Conductive Atomic Force Microscopy,” Journal of the American Chemical Society 145, no. 9 (2023): 5242–5251.

[89] S. T. Hamilton, M. Kelly, W. A. Smith, and A. A. Park, ““Electrolyte-Electrocatalyst Interfacial Effects of Polymeric Materials for Tandem CO₂ Capture and Conversion Elucidated Using In Situ Electrochemical AFM,” ACS Applied Materials & Interfaces 16, no. 32 (2024): 42021–42033.

[90] C. Liu and S. Ye, “In Situ Atomic Force Microscopy (AFM) Study of Oxygen Reduction Reaction on a Gold Electrode Surface in a Dimethyl Sulfoxide (DMSO)-Based Electrolyte Solution,” Journal of Physical Chemistry C 120, no. 44 (2016): 25246–25255.

[91] N. T. Nesbitt and W. A. Smith, “Operando Topography and Mechanical Property Mapping of CO₂ Reduction Gas-Diffusion Electrodes Operating at High Current Densities,” Journal of the Electrochemical Society 168, no. 4 (2021): 044505.

[92] W. Fu and W. Zhang, “Hybrid AFM for Nanoscale Physicochemical Characterization: Recent Development and Emerging Applications,” Small 13, no. 11 (2017): 1603525.

[93] S. Jiang, J. Xue, T. Liu, et al., “Visualization of the Distance-Dependent Synergistic Interaction in Heterogeneous Dual-Site Catalysis,” Journal of the American Chemical Society 146, no. 42 (2024): 29084–29093.

[94] J. X. Tian, Y. Li, X. S. Zhang, et al., “Breaking Single-Reaction Limits: In Situ Visualization of TiS₂-Driven Conversion-Intercalation Synergy in Lithium-Sulfur Batteries,” Advanced Materials (2026): e22007.

[95] D. Faggion, W. D. G. Gonçalves, and J. Dupont, “CO₂ Electroreduction in Ionic Liquids,” Frontiers in Chemistry 7 (2019): 102.

[96] Y. S. Li, F. F. Li, A. Laaksonen, et al., “Electrochemical CO₂ Reduction With Ionic Liquids: Review and Evaluation,” Industrial Chemistry & Materials 1, no. 3 (2023): 410–430.

[97] A. Zafar, K. Matuszek, D. R. MacFarlane, and X. Y. Zhang, ““Recent Progress and Future Perspectives of Ionic Liquid-Based Carbon Dioxide Capture and Conversion,” Green Energy & Environment 10, no. 6 (2025): 1097–1129.

[98] K. X. Li, W. W. Wang, Y. Ding, et al., “Real-Time AFM Analysis of the Impact of CO₂ on Solid-Supported Ionic Liquid Nanomembranes,” Journal of Membrane Science 713 (2025): 123330.

[99] R. Atkin and G. G. Warr, “Structure in Confined Room-Temperature Ionic Liquids,” Journal of Physical Chemistry C 111, no. 13 (2007): 5162–5168.

[100] R. Hayes, N. Borisenko, M. K. Tam, P. C. Howlett, F. Endres, and R. Atkin, “Double Layer Structure of Ionic Liquids at the Au(111) Electrode Interface: An Atomic Force Microscopy Investigation,” Journal of Physical Chemistry C 115, no. 14 (2011): 6855–6863.

[101] X. Zhang, Y. X. Zhong, J. W. Yan, Y. Z. Su, M. Zhang, and B. W. Mao, “Probing Double Layer Structures of Au (111)-BMIPF₆ Ionic Liquid Interfaces From Potential-Dependent AFM Force Curves,” Chemical Communications 48, no. 4 (2012): 582–584.

[102] S. Zhou, K. S. Panse, M. H. Motevaselian, N. R. Aluru, and Y. Zhang, “Three-Dimensional Molecular Mapping of Ionic Liquids at Electrified Interfaces,” ACS Nano 14, no. 12 (2020): 17515–17523.

[103] J. Li, H. Yang, X. Gu, Y. Zou, D. Zhan, and J. Peng, “Recent Advances in Scanning Electrochemical Microscopy for Probing the Sites in Electrocatalysts,” Journal of Materials Chemistry A 12, no. 30 (2024): 18733–18750.

Rights & permissions

2026 The Author(s). Interdisciplinary Materials published by Wuhan University of Technology and John Wiley & Sons Australia, Ltd.