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Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope (AFM-SECM)
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Subparticle Operando Imaging for Probing Electrocatalytic Intermediates and Cation Effects.

Haotian Meng1, Hanxiao Fan1, Jin Xie1

  • 1Department of Materials Science and Engineering, National University of Singapore, Singapore 117575, Singapore.

Journal of the American Chemical Society
|May 11, 2026
PubMed
Summary
This summary is machine-generated.

Single-molecule imaging reveals how copper hydride (Cu-H*) intermediates behave at the nanoscale during electrocatalysis. Electrolyte composition significantly impacts reaction dynamics and efficiency, offering insights for designing better catalysts.

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Area of Science:

  • Electrocatalysis
  • Surface Chemistry
  • Nanotechnology

Background:

  • Surface-bound metal-hydride intermediates are crucial in electrocatalysis but challenging to study due to their transient nature.
  • Conventional methods average signals, masking nanoscale dynamics and heterogeneity.

Purpose of the Study:

  • To directly visualize and quantify the nanoscale dynamics of electrocatalytic intermediates on individual copper nanoplates.
  • To understand the influence of electrolyte composition and particle structure on intermediate behavior and catalytic activity.

Main Methods:

  • Operando single-molecule super-resolution imaging was used to track copper hydride (Cu-H*) intermediates.
  • Systematic variation of electrolyte cation identity and concentration was performed.
  • Analysis included single- and subparticle measurements, spatial correlation, and particle size dependence.

Main Results:

  • Catalytic activity is structure-dependent (corner > edge > basal), linked to interfacial solvation.
  • Reactivity shows a biphasic dependence on particle size, indicating kinetic and transport regimes.
  • Negative catalytic cooperativity was observed between surface sites, driven by competition for proton and water access.
  • Increasing cation size suppressed activity, while ionic strength showed a biphasic effect.

Conclusions:

  • Operando imaging provides a measurable descriptor for Cu-H* intermediates, linking nanoscale structure to solvation.
  • Mechanistic insights are gained for rational electrolyte design in aqueous electrocatalysis.
  • The approach is extensible to other intermediates and electrocatalytic reactions.