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 (Re0.2Mo0.8S2) nanocatalysts,
a relevant alternative to Pt catalysts for the HER. With our approach,
we demonstrate that although the morphology of the Re0.2Mo0.8S2 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.