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Scanning electrochemical microscopy (SECM) is an attractive technology to in-situ characterize the structural evolution and catalytic performance for various electrocatalysts. However, spatial and temporal resolution coupling are still the obstacles that limit its wide applications. Herein, a new operation mode, Fast Scan mode, was developed by improving the dual-pass scan mode, designing novel hardware structure, and employing thermal drift calibration software to achieve a high spatial and temporal resolution simultaneously. The temporal speed can achieve 4 Hz for a high spatial resolution (less than 30 nm) image. This operation mode was employed to dynamically track the phase transition process of molybdenum disulfide (MoS2) over time and characterize the hydrogen evolution reaction (HER) catalytic activity on the edge of semiconducting MoS2 quantitatively while minimizing the diffusional broadening effect and total amount of catalytic products generated above the surface. This new approach should be useful for in-situ tracking dynamic electrochemical processes, establishing the structure-activity relationship for structural complex electrocatalysts, and offering a strategy for high-speed scanning with other electrochemical imaging techniques.
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