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In situ cell for grazing-incidence x-ray diffraction on thin films in thermal catalysis
Lukas Thum1, Manuela Arztmann1, Ivo Zizak1
1Helmholtz-Zentrum Berlin für Materialien und Energie, 14109 Berlin, Germany.
The Review of Scientific Instruments
|March 6, 2024
Summary
This study introduces a new gas-phase cell for in situ X-ray diffraction, enabling the study of thin film catalysts under reaction conditions. The cell allows real-time monitoring of structural changes during catalytic processes.
Area of Science:
- Materials Science
- Surface Science
- Catalysis
Background:
- In situ studies of thin film catalysts under reaction conditions are crucial for understanding catalytic mechanisms.
- Existing methods may have limitations in controlling gas atmospheres and simultaneously performing multiple X-ray techniques.
Purpose of the Study:
- To present a novel gas-phase cell for synchrotron-based grazing-incidence X-ray diffraction.
- To enable in situ investigation of thin film samples under catalytically relevant conditions.
- To allow simultaneous X-ray reflectometry and fluorescence studies.
Main Methods:
- Development and testing of a specialized gas-phase cell for X-ray diffraction experiments.
- Utilizing synchrotron radiation for high-resolution structural analysis.
- Studying thin film samples (e.g., 3 nm Pd) under controlled gas atmospheres (H2, acetylene).
Main Results:
- The developed cell effectively minimizes diffraction contributions from sample enclosures.
- Demonstrated applicability for monitoring structural changes in Pd thin films during hydrogenation and semihydrogenation.
- Successfully investigated thin films under industrially relevant catalytic conditions.
Conclusions:
- The novel gas-phase cell is a valuable tool for in situ characterization of thin film catalysts.
- It facilitates the study of dynamic structural changes under realistic catalytic environments.
- Enables a deeper understanding of catalytic processes at the nanoscale.

