Dual‐Mode Imaging of Dynamic Interaction between Bubbles and Single Nanoplates during the Electrocatalytic Hydrogen Evolution Process

Abstract Gas bubble formation at electrochemical interfaces can significantly affect the efficiency and durability of electrocatalysts. However, obtaining comprehensive details on bubble evolution dynamics, particularly their dynamic interaction with high‐performance structured electrocatalysts, poses a considerable challenge. Herein, dual‐mode interference/total internal reflection fluorescence microscopy is introduced, which allows for the simultaneous capture of the evolution pathway of bubbles and the 3D motion of nanoplate electrocatalysts, providing high‐resolution and accurate spatiotemporal information. During the hydrogen evolution reaction, the dynamics of hydrogen bubble generation and their interactions with single nanoplate electrocatalysts at the electrochemical interface are observed. The results unveiled that, under constant potential, bubbles initially manifest as fast‐moving nanobubbles, transforming into stationary microbubbles subsequently. The morphology of stationary nanoplates regulates the trajectories of these moving nanobubbles while the pinned microbubbles induce the motion of the electrocatalysts. The dual‐mode microscopy can be employed to scrutinize numerous multiphase electrochemical interactions with high spatiotemporal resolution, which can facilitate the rational design of high‐performance electrocatalysts.