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| Journal Article | PUBDB-2022-08083 |
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2023
ACS Publications
Washington, DC
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Please use a persistent id in citations: doi:10.1021/acs.accounts.2c00525 doi:10.3204/PUBDB-2022-08083
Abstract: CONSPECTUS. Water splitting is intensively studied for sustainable and effective energy storage in green / alternative energy harvesting-storage-release cycles. In this work, we present our recent developments for combining liquid-jet microtechnology with different types of soft X-ray spectroscopy at high flux X-ray sources, in particular developed for studying the oxygen evolution reaction (OER). We are particularly interested in the development of in-situ photon-in / photon-out techniques, such as in-situ Resonant Inelastic X-ray Scattering (RIXS) techniques at high repetition frequency X-ray sources, pointing towards operando capabilities. The pilot catalytic systems we use are perovskites, with the general structure ABO3 with lanthanides or group II elements on the A-site and transition metals on the B-site. Depending on the chemical substitutions of ABO3, their catalytic activity for OER can composition-dependent be tuned. In this work, we present our in-situ RIXS studies of the manganese L-edge of perovskites during OER. We have developed various X-ray spectroscopy approaches like transmission zone plate-, reflection zone plate- and grating-based emission spectroscopy techniques. Combined with tunable incidence X-ray energies, we yield complementary information about changing (inverse) X-ray absorption features of the perovskites allowing us to deduce element- and oxidation-state-specific chemical monitoring of the catalyst. Adding liquid jet technology, we monitor element- and oxidation-state specific the catalyst with water adsorbate during OER. By comparing the different technical spectroscopy approaches combined with high-repetition frequency experiments at synchrotrons and free-electron lasers, we conclude that the combination of liquid jet with low-resolution zone-plate based X-ray spectroscopy are sufficient for element- and oxidation-state specific chemical monitoring during OER and easy to handle. For an in-depth study of OER mechanisms, however, including the characterization of catalyst-water adsorbate as their charge transfer properties and specially valence intermediates formed during OER high-resolution spectroscopy tools based on a combination of liquid jets with gratings bear bigger potential since they allow to resolve otherwise overlapping X-ray spectroscopy transitions. Common for all experimental approaches is the conclusion that without the versatile developments of liquid jets and liquid beam technologies, elaborate experiments such as the highly repetitive experiments at high flux X-ray sources (like synchrotrons or free-electron lasers) would hardly be possible. Such experiments allow a sample refreshment for every single X-ray shot up to 5 MHz repetition frequencies so that it is possible (a) to study X-ray radiation-sensitive samples but also (b) utilize novel types of flux-hungry X-ray spectroscopy tools like photon-in / photon-out X-ray spectroscopy for studying the OER.
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