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Chinese Journal of Catalysis 43 (2022) 59-70 催化学报 2022年 第43卷 第1期 | www.cjcatal.com available at www.sciencedirect.com journal homepage: www.sciencedirect.com/journal/chinese-journal-of-catalysis Review Modern applications of scanning electrochemical microscopy in the analysis of electrocatalytic surface reactions C. Hyun Ryu † , Yunwoo Nam † , Hyun S. Ahn * Department of Chemistry, Yonsei University, 50 Yonsei-ro, Seodaemun-gu, Seoul 03722, Korea A R T I C L E I N F O A B S T R A C T Article history: Received 16 July 2021 Accepted 2 August 2021 Available online 15 November 2021 Development of reaction-tailored electrocatalysts is becoming increasingly important as energy and environment are among key issues governing our sustainable future. Electrocatalysts are inherently optimized for application towards reactions of interest in rwable energy, such as those involve in water splitting and artificial photosynthesis, owing to its energy efficiency, simple fabrication, and ease of operation. In this view, it is important to secure logical design principles for the synthesiof electrocatalysts for various reactions of interest, and also understand their catalytic mechanisms in the respective reactions for improvements in further iterations. In this review, we introduce several key methods of scanning electrochemical microscopy (SECM) in its applications towards electroca-talysis. A brief history and a handful of seminal works in the SECM field is introduced in advancing the synthetic designs of electrocatalysts and elucidation of the operating mechanism. New devel-opments in nano-sizing of the electrodes in attempts for improved spatial resolution of SECM is also introduced, and the application of nanoelectrodes towards the investigation of formerly inaccessible single catalytic entities is shared. © 2022, Dalian Institute of Chemical Physics, Chinese Academy of Sciences.Published by Elsevier B.V. All rights reserved.Keywords: Scanning electrochemical microscopy Electrocatalysis Surface reaction Electroanalytical chemistry In situ electrochemical analysis Direct quantification 1. Introduction Scanning electrochemical microscopy (SECM) was first in-troduced by Fan et al. [1] in 1989. SECM has been employed to study electrochemical and morphological properties of hetero-geneous and homogeneous reactions of various substrates with high resolution. The applications of SECM have been developed and applied to various analytes, such as electrocatalysts, pho-tocatalysts, nanoparticles, and battery surfaces. Also, many operation modes of SECM recently evolved with the advent of nanotechnology to achieve more meticulous analysis. 1.1. Components A scanning electrochemical microscope consists of four electrodes (tip electrode, counter electrode, reference elec-trode, and substrate electrode) and is mounted on a three-dimensional positioning system. The resolution of an SECM is determined by the ze of the tip electrode and the spatial resolution of the positioner moving the tip. Typical modern commercial SECMs can reach nanometer-level resolu-tions owing to the development in the fabrication of nanoelec-trodes [2-5]. 1.2. Operation modes Since the introduction of SECM (Fig. 1), various operatio modes [6] were developed, each with unique application in mind. Among them, the most basic methods are feedback modes and generation/collection (G-C) modes. Many advanced * Corresponding author. E-mail: ahnhs@yonsei.ac.kr † Contributed equally to this work. DOI: 10.1016/S1872-2067(21)63948-7 | http://www.sciencedirect.com/journal/chinese-journal-of-catalysis | Chin. J. Catal., Vol. 43, No. 1, January 2022 万方数据