The development of high-efficiency energy storage and conversion devices requires a deeper understanding of the structure-activity relationship of electrocatalysts, material transformations during electrocatalysis processes, and complex electrochemical processes at electrode-electrolyte interfaces. Scanning probe microscopy (SPM) is a powerful tool for visualizing the surface properties and localized electrochemical activity down to the atomic scale in situ and even operando, thus plays an essential role in studying heterogeneous electrocatalysis mechanisms. We summarize recent advancements in SPM for investigating energy-related electrocatalysis based on three unique characteristics of SPM—surface property imaging, in situ/operando monitoring, and nanoscale electrochemical mapping，outline the application of SPM in investigating the structure-activity relationship, material transformations, and electrochemical processes. The specific SPM techniques discussed here include scanning tunneling microscopy, atomic force microscopy, scanning electrochemical microscopy, scanning ion conductance microscopy, and scanning electrochemical cell microscopy. Finally, the opportunities and challenges of SPM in electrocatalysis are discussed.

高效储能和转换装置的发展需要更深入地了解电催化剂的构效关系、电催化过程中的材料转变以及电极-电解质界面的复杂电化学过程。扫描探针显微镜 (SPM) 是一种强大的工具，可用于将表面性质和局部电化学活性可视化到原位甚至原位原子尺度，因此在研究非均相电催化机制中起着至关重要的作用。我们总结了 SPM 在研究能量相关电催化方面的最新进展，基于 SPM 的三个独特特征——表面性质成像，原位/operando 监测和纳米级电化学映射，概述了 SPM 在研究构效关系、材料转变和电化学过程中的应用。此处讨论的特定 SPM 技术包括扫描隧道显微镜、原子力显微镜、扫描电化学显微镜、扫描离子电导显微镜和扫描电化学电池显微镜。最后，讨论了 SPM 在电催化中的机遇和挑战。