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In-situ and operando Grazing Incidence XAS: a novel set-up and its application to model Pd electrodes for alcohols oxidation

  • Enrico Berretti , Andrea Giaccherini , Vincenzo Dell’Aquila , Francesco Di Benedetto , Giordano Montegrossi , Giovanni Orazio Lepore , Massimo Innocenti , Francesco D’Acapito , Francesco Vizza EMAIL logo and Alessandro Lavacchi
Published/Copyright: March 8, 2024
Pure and Applied Chemistry
From the journal Pure and Applied Chemistry Volume 96 Issue 4

Abstract

In this article, we present an in-situ and operando time-resolved X-ray Absorption Spectroscopy (XAS) technique which exploits a combination of Grazing Incidence XAS (GIXAS) and Fixed Energy X-ray Absorption Voltammetry (FEXRAV), the Grazing Incidence FEXRAV (GI-FEXRAV). A case-study is also outlined. Palladium ultra-low loadings were deposited above Au polycrystalline iso-oriented substrates adopting three different deposition methods: surface-controlled electrochemical methods, direct electrodeposition, and physical vapour deposition (PVD). These catalytical surfaces were prepared for the investigation by GI-FEXRAV of the Pd oxidation/dissolution phenomenon that could occur when the metal is used in the anodic compartment of Direct Alcohol Fuel Cells (DAFCs) or in electrochemical reformers. Moreover, we report a robust, low cost and versatile procedure to obtain wide and flat iso-oriented gold substrates that can mimic monocrystalline gold (1 1 1) in the electrochemical response. The use of GI-FEXRAV for the operando characterization of the catalysts, in conjunction with the designed experimental cell and our flexible Au-based electrochemical substrates show an invaluable potential in the operando study of fundamental phenomena in heterogeneous electrocatalysis model systems and, due to its versatility, paves the way to further studies on a wide selection of electrochemical systems.

Keywords: Avogadro Colloquia 2022; electrocatalysis; fuel cells; palladium; surface chemistry; XAS
Corresponding author: Francesco Vizza, Institute for the Chemistry of Organometallic Compounds, CNR-ICCOM, Via Madonna del Piano n.10, Sesto Fiorentino, 50019, Italy, e-mail:
Article note: A collection of invited papers based on presentations at Avogadro Colloquia 2022, 15th – 16th December 2022.

Funding source: POR H2 AdP MMES/ENEA

Award Identifier / Grant number: Mission 2, Component 2, Investment 3.5

Funding source: Made in Italy – Circular and Sustainable (MICS) Extended Partnership

Funding source: Ministero dell’Università e della Ricerca

Award Identifier / Grant number: PRIN 2022 2022NW4P2T

Funding source: European Synchrotron Radiation Facility

Award Identifier / Grant number: EXP CH-6101, EXP MA-3431

Funding source: Ministero dell’Istruzione, dell’Università e della Ricerca

Award Identifier / Grant number: PRIN 2017 n.2017YH9MRK

Acknowledgments

Authors wanted to thank PRIN 2017 Project “Novel Multilayered and Micro-Machined Electrode Nano-Architectures for Electrocatalytic Applications (Fuel Cells and Electrolyzers)” (N° 2017YH9MRK) funded by Italian Ministry MUIR. Authors wanted to acknowledge the European Synchrotron Radiation Facility (ESRF) for provision of synchrotron radiation beamtime for EXP MA-3431 and CH-6101. Thanks are due also to the Made in Italy – Circular and Sustainable (MICS) Extended Partnership funded by the European Union Next-Generation EU (Piano Nazionale di Ripresa e Resilienza (PNRR) - Missione 4, Componente 2, Investimento 1.3 – D.D. 1551.11-10-2022, PE00000004), to the European Union – NextGeneration EU from the Italian Ministry of Environment and Energy Security POR H2 AdP MMES/ENEA with involvement of CNR and RSE, PNRR – Mission 2, Component 2, Investment 3.5 “Ricerca e sviluppo sull’idrogeno”. L.A.1.1.24, and to Ministero della Università e Ricerca PRIN 2022 2022NW4P2T (FUTURO) for financial support. Authors wanted also to acknowledge Carlo Bartoli from the CNR-ICCOM workshop for its help in developing the operando EC cells concept.

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Published Online: 2024-03-08
Published in Print: 2024-04-25

© 2024 IUPAC & De Gruyter

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Preface
  4. Avogadro Colloquia in Rome on “Vision and Opportunities of a Sustainable Hydrogen Society”
  5. Conference papers
  6. H2 in the energy transition
  7. Watching atoms at work during reactions
  8. Hydrogen production and conversion to chemicals: a zero-carbon puzzle?
  9. Rethinking chemical production with “green” hydrogen
  10. Hydrogen as an energy carrier: constraints and opportunities
  11. Shaping the future of green hydrogen: De Nora’s electrochemical technologies for fueling the energy transition
  12. In-situ and operando Grazing Incidence XAS: a novel set-up and its application to model Pd electrodes for alcohols oxidation
  13. Hydrogen storage and handling with hydrides
  14. Advanced polymer electrolyte membrane water electrolysis for power to gas applications
  15. Inkjet printed acrylate-urethane modified poly(3,4-ethylenedioxythiophene) flexible conductive films
  16. Cu(II) complexes using acylhydrazones or cyclen for biocidal antifouling coatings
  17. Randomly cross-linked amphiphilic copolymer networks of n-butyl acrylate and N,N-dimethylacrylamide: synthesis and characterization
  18. Roles of electrostatics and intermolecular electronic motions in the structural and spectroscopic features of hydrogen- and halogen-bonded systems
  19. The accurate assessment of the chemical speciation of complex systems through multi-technique approaches
https://doi.org/10.1515/pac-2023-1013
Keywords for this article
Avogadro Colloquia 2022; electrocatalysis; fuel cells; palladium; surface chemistry; XAS

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Preface
  4. Avogadro Colloquia in Rome on “Vision and Opportunities of a Sustainable Hydrogen Society”
  5. Conference papers
  6. H2 in the energy transition
  7. Watching atoms at work during reactions
  8. Hydrogen production and conversion to chemicals: a zero-carbon puzzle?
  9. Rethinking chemical production with “green” hydrogen
  10. Hydrogen as an energy carrier: constraints and opportunities
  11. Shaping the future of green hydrogen: De Nora’s electrochemical technologies for fueling the energy transition
  12. In-situ and operando Grazing Incidence XAS: a novel set-up and its application to model Pd electrodes for alcohols oxidation
  13. Hydrogen storage and handling with hydrides
  14. Advanced polymer electrolyte membrane water electrolysis for power to gas applications
  15. Inkjet printed acrylate-urethane modified poly(3,4-ethylenedioxythiophene) flexible conductive films
  16. Cu(II) complexes using acylhydrazones or cyclen for biocidal antifouling coatings
  17. Randomly cross-linked amphiphilic copolymer networks of n-butyl acrylate and N,N-dimethylacrylamide: synthesis and characterization
  18. Roles of electrostatics and intermolecular electronic motions in the structural and spectroscopic features of hydrogen- and halogen-bonded systems
  19. The accurate assessment of the chemical speciation of complex systems through multi-technique approaches
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