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Hard X-ray Photoelectron Spectroscopy Probing Fe Segregation during the Oxygen Evolution Reaction.

Filippo Longo1,2, Pedro Javier Lloreda-Jurado3, Jorge Gil-Rostra3

  • 1Chemical Energy Carriers and Vehicle Systems Laboratory, Empa - Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, 8600 Dübendorf, Switzerland.

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|October 17, 2024
PubMed
Summary

Iron-Nickel (NiFe) electrocatalysts show high activity for water splitting. This study reveals that iron segregation to the surface, influenced by catalyst porosity, forms inactive phases, impacting overall performance.

Keywords:
Fe surface segregationHAXPESNiFe-oxyhydroxidenanostructured thin film catalystsnondestructive in-depth chemical profilesoxygen evolution reaction

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Area of Science:

  • Electrochemistry
  • Materials Science
  • Surface Science

Background:

  • Nickel-Iron (NiFe) electrocatalysts are highly active for alkaline oxygen evolution reaction (OER) in water splitting.
  • Understanding the Ni-Fe interplay and surface phenomena is critical for designing efficient water-splitting electrodes.
  • Electrochemical reactions induce complex surface changes like oxide formation and species segregation, hindering rational design.

Purpose of the Study:

  • To develop and apply a method for quantifying chemical depth profiling using XPS/HAXPES.
  • To investigate the surface reconstruction of NiFe electrodes with varying porosities during OER.
  • To elucidate the role of porosity in iron segregation and its impact on electrocatalyst performance.

Main Methods:

  • Quantitative chemical depth profiling using X-ray photoelectron spectroscopy (XPS) and hard X-ray photoelectron spectroscopy (HAXPES).
  • Application of the developed method to two NiFe electrodes with distinct porosities.
  • In-situ analysis of surface reconstruction during electrochemical oxygen evolution reaction.

Main Results:

  • Iron (Fe) segregates to the surface under ambient conditions, forming an inactive FeO phase.
  • Catalyst porosity significantly influences the Fe segregation process and electrode performance.
  • Higher porosity in nanostructured samples leads to increased Fe diffusion and suppression of the active NiFe-oxyhydroxide phase.

Conclusions:

  • Surface chemistry of multielement systems is dynamic and depends on applied potential, electrolyte, and bulk properties.
  • Porosity is a critical factor in NiFe electrocatalyst design, affecting Fe surface segregation and OER activity.
  • HAXPES provides crucial insights into subsurface properties influencing surface behavior.