Operando Laboratory-Based Multi-Edge X-Ray Absorption Near-Edge Spectroscopy of Solid Catalysts

Area of Science:

• Catalysis research
• Materials science
• Spectroscopy

Background:

• X-ray absorption spectroscopy (XAS) and X-ray absorption near-edge structure (XANES) are powerful tools for catalyst characterization.
• Synchrotron facilities offer valuable but limited access for such analyses.
• Developing laboratory-based XAS/XANES methods provides an accessible alternative and complement.

Purpose of the Study:

• To design and implement a laboratory-based setup for operando XANES analysis.
• To investigate the behavior of multi-element CO2 hydrogenation catalysts under reaction conditions.
• To explore the potential of laboratory XANES as a complementary technique to synchrotron-based studies.

Main Methods:

• Designed a laboratory-based X-ray absorption spectroscopy setup.
• Performed operando, quasi-simultaneous XANES analysis at multiple K-edges.
• Studied mono-, bi-, and trimetallic catalysts containing Ni, Fe, and Cu for CO2 hydrogenation.

Main Results:

• Successfully conducted operando XANES studies on multi-element catalysts.
• Observed distinct metal-dependent differences in reducibility and re-oxidation behavior.
• Correlated these behaviors with catalytic performance in CO2 hydrogenation.

Conclusions:

• Laboratory-based operando XANES is applicable for multi-element catalyst characterization.
• This technique offers valuable insights complementing synchrotron studies.
• Enables advanced analysis of catalyst behavior under reaction conditions.