Development of Electrochemical Cells and Their Application for Spatially Resolved Analysis Using a Multitechnique Approach: From Conventional Experiments to X‑Ray Nanoprobe Beamlines

Real (electro)­catalysts are often heterogeneous, and their activity and selectivity depend on the properties of specific active sites. Therefore, unveiling the so-called structure–activity relationship is essential for a rational search for better materials and, consequently, for the development of...

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Veröffentlicht in:Analytical chemistry (Washington) 2023-11, Vol.95 (44), p.16144-16152
Hauptverfasser: Vicente, Rafael Alcides, Raju, Swathi Patchaiammal, Gomes, Heloisa Vampré Nascimento, Neckel, Itamar Tomio, Tolentino, Hélio Cesar Nogueira, Fernández, Pablo Sebastián
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Sprache:eng
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Zusammenfassung:Real (electro)­catalysts are often heterogeneous, and their activity and selectivity depend on the properties of specific active sites. Therefore, unveiling the so-called structure–activity relationship is essential for a rational search for better materials and, consequently, for the development of the field of (electro-)­catalysis. Thus, spatially resolved techniques are powerful tools as they allow us to characterize and/or measure the activity and selectivity of different regions of heterogeneous catalysts. To take full advantage of that, we have developed spectroelectrochemical cells to perform spatially resolved analysis using X-ray nanoprobe synchrotron beamlines and conventional pieces of equipment. Here, we describe the techniques available at the Carnaúba beamline at the Sirius-LNLS storage ring, and then we show how our cells enable obtaining X-ray (XRF, XRD, XAS, etc.) and vibrational spectroscopy (FTIR and Raman) contrast images. Through some proof-of-concept experiments, we demonstrate how using a multi-technique approach could render a complete and detailed analysis of an (electro)­catalyst overall performance.
ISSN:0003-2700
1520-6882
DOI:10.1021/acs.analchem.3c02695