Development of electrochemical cells for spatially resolved analysis using a multi-technique 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 the field of (electro-)catalysts. 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 (SEC) 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 Sirius-LNLS storage ring, then we show how our SECs 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.