However, most of the studies characterize the catalytic activity of S vacancies with macroscopic methods, making it a great challenge to accurately obtain the electro chemical activities of specific active site for catalysts with multiple types of active sites/areas (for example, MoS 2 's edge, S vacancies, metallic phase, etc.). Moreover, the unstable chalcogen atomic defects in MoS 2 is another challenge to achieve in situ characterization because the dynamic evolution of the defects, such as the type, composition, geometry, and concentration, easily occurs by physical and chemical stimuli. [12,13] Characterizing