In-house setup for laboratory-based x-ray absorption fine structure spectroscopy measurements

Area of Science:

• Materials Science
• Analytical Chemistry
• Spectroscopy

Background:

• X-ray Absorption Fine Structure (XAFS) spectroscopy is a powerful technique for elemental and chemical state analysis.
• Synchrotron radiation facilities are typically required for XAFS measurements, limiting accessibility.

Purpose of the Study:

• To develop and validate a laboratory-based XAFS facility for in-house measurements.
• To assess the reliability and accuracy of the developed setup by comparing results with synchrotron data.
• To investigate the influence of oxidation states on XAFS spectra.

Main Methods:

• Construction of a laboratory XAFS system using a conventional X-ray source and a von Hamos bent crystal spectrometer.
• Acquisition and comparison of XAFS spectra (Cu K-edge, Ta L3-edge) with synchrotron data.
• Determination of K- and L-edge energies and attenuation coefficients for various elements.
• Measurement of XAFS spectra for metallic Fe and its oxides (Fe2O3, Fe3O4) to study oxidation state effects.

Main Results:

• The laboratory XAFS setup successfully reproduced spectra comparable to those obtained at synchrotron facilities.
• Accurate determination of K- and L-edge energies and attenuation coefficients for several elements.
• Demonstrated sensitivity of XAFS spectral shape to the oxidation state of iron samples.

Conclusions:

• The developed laboratory-based XAFS facility provides a reliable and accurate alternative to synchrotron sources for specific applications.
• This setup enhances accessibility for XAFS measurements, particularly for studying elemental properties and chemical states.