Identifying and Mitigating Adverse X‑ray Induced Effects in Operando Spectroscopic Studies of Copper Exchanged...

Area of Science:

• Materials Science
• Analytical Chemistry
• Physics

Background:

• Synchrotron radiation is crucial for modern scientific research.
• Increasingly powerful X-ray sources pose a risk of beam-induced sample alterations.
• These alterations can compromise experimental data and lead to erroneous conclusions.

Purpose of the Study:

• To present a methodology for mitigating X-ray beam-induced effects during synchrotron experiments.
• To ensure the integrity of observed phenomena by preventing the observation method from causing alterations.
• To enable reliable operando measurements at advanced synchrotron facilities.

Main Methods:

• Implementation of a mesh scan technique, rastering the X-ray beam across the sample.
• Utilizing time-resolved X-ray absorption spectroscopy (XAS) to monitor changes in copper oxidation state.
• Investigating copper-exchanged zeolites under various atmospheric conditions (oxidizing, reducing, inert) as a function of X-ray dose.

Main Results:

• Beam-induced effects were observed at lower X-ray doses than previously reported for copper-exchanged zeolites.
• The mesh scan methodology effectively mitigates local overexposure and preserves sample integrity.
• Demonstrated the capability to conduct uncompromised operando measurements.

Conclusions:

• The mesh scan technique is a vital tool for accurate synchrotron-based research.
• This method ensures the full exploitation of state-of-the-art synchrotron facilities.
• Provides a reliable approach for obtaining uncompromised results in X-ray spectroscopy studies.