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 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 Carnauba 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.

Automated summary

Real electrocatalysts are heterogeneous and their activity depends on specific active sites. Spatially resolved techniques can characterize different regions of catalysts. Spectroelectrochemical cells enable obtaining X-ray and vibrational spectroscopy contrast images, facilitating complete analysis of catalyst performance.