Expanding the Potential of Identical Location Scanning Transmission Electron Microscopy for Gas Evolving Reactions: Stability of Rhenium Molybdenum Disulfide Nanocatalysts for Hydrogen Evolution Reaction

[Image: see text] Identical location (scanning) transmission electron microscopy provides valuable insights into the mechanisms of the activity and degradation of nanocatalysts during electrochemical reactions. However, the technique suffers from limitations that hinder its widespread use for nanocatalysts of gas evolving reactions, e.g., the hydrogen evolution reaction (HER). The main issue is the production of bubbles that cause the loss of electric contact in identical location measurements, which is critical for the correct cycling of the nanocatalysts and interpretation of the electron microscopy results. Herein, we systematically evaluate different set-ups, materials, and tools to allow the facile and reliable study of the stability of HER nanocatalysts. The optimized conditions are applied for the study of layered rhenium molybdenum disulfide (Re(0.2)Mo(0.8)S(2)) nanocatalysts, a relevant alternative to Pt catalysts for the HER. With our approach, we demonstrate that although the morphology of the Re(0.2)Mo(0.8)S(2) catalyst is maintained during HER, chemical composition changes could be correlated to the electrochemical reaction. This study expands the potential of the IL(S)TEM technique for the construction of structure–property relationships of nanocatalysts of gas evolving reactions.