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

Autor(es)

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

• Tipo de documento: Artigo Científico
• Fonte: Analytical Chemistry; v. 95, n. 44, p. 9-pg., 2023-10-26.

Resumo

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)

• Processo FAPESP: 20/07955-0 - Desenvolvimento e caracterização de células eletroquímicas microfluídicas para medidas de imageamento por difração coerente de Bragg in situ
• Beneficiário: Heloísa Vampré Nascimento Gomes
• Modalidade de apoio: Bolsas no Brasil - Iniciação Científica
• Processo FAPESP: 17/11986-5 - Geração e Armazenamento de Novas Energias: trazendo desenvolvimento tecnológico para o país
• Beneficiário: Ana Flávia Nogueira
• Modalidade de apoio: Auxílio à Pesquisa - Programa Centros de Pesquisa em Engenharia
• Processo FAPESP: 21/02678-0 - Estudos fundamentais na área de eletroquímica no nível de nanopartículas individuais usando técnicas baseadas em luz síncrotron
• Beneficiário: Rafael Alcides Vicente
• Modalidade de apoio: Bolsas no Brasil - Doutorado
• Processo FAPESP: 20/04431-0 - Utilização de óxidos de perovskitas para a geração contínua e simultânea de energia e/ou portadores densos de energia
• Beneficiário: Pablo Sebastián Fernández
• Modalidade de apoio: Auxílio à Pesquisa - Programa BIOEN - Regular