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Fluorescence-detected quick-scanning X-ray absorption spectroscopy

Adam H. Clark, Patrick Steiger, Benjamin Bornmann, Stephan Hitz, R. Frahm, Davide Ferri, Maarten Nachtegaal

2020Journal of Synchrotron Radiation49 citationsDOIOpen Access PDF

Abstract

Time-resolved X-ray absorption spectroscopy (XAS) offers the possibility to monitor the state of materials during chemical reactions. While this technique has been established for transmission measurements for a number of years, XAS measurements in fluorescence mode are challenging because of limitations in signal collection as well as detectors. Nevertheless, measurements in fluorescence mode are often the only option to study complex materials containing heavy matrices or in samples where the element of interest is in low concentration. Here, it has been demonstrated that high-quality quick-scanning full extended X-ray absorption fine-structure data can be readily obtained with sub-second time resolution in fluorescence mode, even for highly diluted samples. It has also been demonstrated that in challenging samples, where transmission measurements are not feasible, quick fluorescence can yield significant insight in reaction kinetics. By studying the fast high-temperature oxidation of a reduced LaFe 0.8 Ni 0.8 O 3 perovskite type, an example where the perovskite matrix elements prevent measurements in fluorescence, it is shown that it is now possible to follow the state of Ni in situ at a 3 s time resolution.

Topics & Concepts

FluorescenceAbsorption (acoustics)SpectroscopyAbsorption spectroscopyFluorescence spectroscopyMaterials scienceAnalytical Chemistry (journal)OpticsChemistryPhysicsChromatographyQuantum mechanicsCatalytic Processes in Materials ScienceX-ray Spectroscopy and Fluorescence AnalysisMachine Learning in Materials Science
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