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

Author(s)

Vicente, Rafael Alcides ; Raju, Swathi Patchaiammal ; Gomes, Heloisa Vampre Nascimento ; Neckel, Itamar Tomio ; Tolentino, Helio Cesar Nogueira ; Fernandez, Pablo Sebastian

• Document type: Journal article
• Source: Analytical Chemistry; v. 95, n. 44, p. 9-pg., 2023-10-26.

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 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. (AU)

• FAPESP's process: 20/07955-0 - Development and characterization of microfluidic electrochemical cells for measurements of Bragg coherent diffraction imaging in situ
• Grantee: Heloísa Vampré Nascimento Gomes
• Support Opportunities: Scholarships in Brazil - Scientific Initiation
• FAPESP's process: 17/11986-5 - Generation and storage of New Energy: bringing technological development for the country
• Grantee: Ana Flávia Nogueira
• Support Opportunities: Research Grants - Research Centers in Engineering Program
• FAPESP's process: 21/02678-0 - Fundamental studies in the field of electrochemistry at the level of single nanoparticles using synchrotron-based techniques
• Grantee: Rafael Alcides Vicente
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 20/04431-0 - Perovskite oxides for the continuous and/or simultaneous production of energy and/or dense energy carriers
• Grantee: Pablo Sebastián Fernández
• Support Opportunities: Program for Research on Bioenergy (BIOEN) - Regular Program Grants