Agradecimentos: This research was funded by Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) (grants: 2017/11986-5, 2020/04431-0, 2020/07955-0, and 2021/02678-0), the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) (grant: 653684/2021-00). And by CNPq (Conselho Nacional de Desenvolvimento Científico e Tecnológico) (grants: 402481/2021-6 and 304772/2021-6). The authors thank the support from Shell and the strategic importance of the support given by ANP (Brazil’s National Oil, Natural Gas, and Biofuels Agency) through the R&D levy regulation. This research used resources of the Brazilian Synchrotron Light Laboratory (LNLS), part of the Brazilian Center for Research in Energy and Materials (CNPEM), a private nonprofit organization under the supervision of the Brazilian Ministry for Science, Technology, and Innovations (MCTI). The Carnaúba beamline staff is acknowledged for the assistance during the experiments (20210015) Ver menos

Abstract: 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 Ver menos