Versatile in situ/operando Setup for Studying Catalysts by X‐Ray Absorption Spectroscopy under Demanding and Dynamic Reaction Conditions for Energy Storage and Conversion

Abstract

AbstractX‐ray absorption spectroscopy (XAS) is one of the powerful operando tools to track structural variations in heterogeneous catalysts. The nature of active sites in catalyst research is of great relevance, especially given the growing importance of energy storage using CO2 as feedstock and the need for dynamic availability of electric power. Due to the pressure/temperature prerequisite of catalyst performance, the characterization of catalyst structure during catalysis under such high‐pressure reaction conditions is important to further improve catalyst design at a molecular level. Investigating catalysts in a controlled reaction atmosphere, while probing with X‐rays, offers an excellent opportunity for developing infrastructure at the synchrotron. Herein, a mobile setup with a robust spectroscopic cell for in situ and operando XAS applications, including a high‐pressure gas dosing equipment for such catalytic systems, is presented. The in situ/operando cell is operational for both the transmission and the fluorescence XAS mode at up to 50 bar and 450 °C. The setup comes with a protective box with Kapton windows, which holds the cell and serves as a miniature fume hood, and on‐line product analysis. Furthermore, the gas dosing equipment is compact, light‐weighted and can be easily transported to different synchrotrons and allows an optimum pre‐mix of gas flows and pressure build‐up. Methanol and Fischer‐Tropsch syntheses are used as examples for the highly flexible instrumentation.