Versatile Homebuilt Gas Feed and Analysis System for Operando TEM of Catalysts at Work

Microsc Microanal. 2020 Apr;26(2):220-228. doi: 10.1017/S143192762000015X.

Abstract

Understanding how catalysts work during chemical reactions is crucial when developing efficient catalytic materials. The dynamic processes involved are extremely sensitive to changes in pressure, gas environment and temperature. Hence, there is a need for spatially resolved operando techniques to investigate catalysts under working conditions and over time. The use of dedicated operando techniques with added detection of catalytic conversion presents a unique opportunity to study the mechanisms underlying the catalytic reactions systematically. Herein, we report on the detailed setup and technical capabilities of a modular, homebuilt gas feed system directly coupled to a quadrupole mass spectrometer, which allows for operando transmission electron microscopy (TEM) studies of heterogeneous catalysts. The setup is compatible with conventional, commercially available gas cell TEM holders, making it widely accessible and reproducible by the community. In addition, the operando functionality of the setup was tested using CO oxidation over Pt nanoparticles.

Keywords: Pt nanoparticles; conversion detection; heterogeneous catalysis; temporal and spatial resolution; working conditions.