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Transition metal hydroxides are key electrocatalysts for oxygen evolution. This study reveals how their nanoscale structure and cobalt oxidation states dynamically change during operation, linking bulk transformations to surface catalytic activity.

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Area of Science:

  • Materials Science
  • Electrochemistry
  • Nanotechnology

Background:

  • Transition metal (oxy)hydroxides are promising electrocatalysts for the oxygen evolution reaction.
  • Material properties dynamically evolve with applied voltage via ion insertion redox reactions.
  • The far-from-equilibrium catalytic state complicates direct observation.

Purpose of the Study:

  • To establish a link between oxygen evolution activity and the local nanoscale structure of single-crystalline β-Co(OH)2 platelet particles.
  • To understand the dynamic transformations occurring during electrocatalysis.

Main Methods:

  • Operando scanning probe and X-ray microscopy techniques.
  • Correlative microscopy to link chemical, physical, and electronic nanoscale structure.
  • Analysis of single-crystalline β-Co(OH)2 platelet particles.

Main Results:

  • Particles swell to form an α-CoO2H1.5·0.5H2O-like structure (Co +2.5) at pre-catalytic voltages.
  • Interlayer water and protons de-intercalate to form contracted β-CoOOH (Co +3) during oxygen evolution.
  • Electrochemical current is restricted to edge facets, correlating with local Co +3 concentration and Tafel behavior.

Conclusions:

  • Demonstrates the link between bulk ion-insertion and surface catalytic activity in electrocatalysts.
  • Heterogeneous bulk transformations are coupled to localized surface activity.
  • Operando microscopy reveals dynamic nanoscale changes crucial for catalytic function.