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Mapping Electrochemical Heterogeneity at Gold Surfaces: A Second Harmonic Imaging Study.

Igor Nahalka1, Gregor Zwaschka2, R Kramer Campen2,3

  • 1Laboratory for fundamental BioPhotonics (LBP), Institute of Bio-engineering (IBI), and Institute of Materials Science (IMX), School of Engineering (STI), and Lausanne Centre for Ultrafast Science (LACUS), École Polytechnique Fédérale de Lausanne (EPFL), CH-1015, Lausanne, Switzerland.

The Journal of Physical Chemistry. C, Nanomaterials and Interfaces
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Summary

This study maps gold electrode surfaces during electrocatalysis using optical second harmonic imaging. It reveals how surface structure heterogeneity influences reactivity and potential-induced restructuring in nanocatalysts.

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Area of Science:

  • Surface science
  • Electrochemistry
  • Materials science

Background:

  • Designing efficient catalysts necessitates correlating surface structure and composition with reactivity across diverse length scales.
  • Existing research primarily focuses on single crystals, with limited understanding of heterogeneous catalysts used in practical applications.
  • Heterogeneous catalysts require methods for mapping structure-function relationships during electrochemical processes.

Purpose of the Study:

  • To map the surface of gold nanocrystalline and polycrystalline electrodes during electrooxidation.
  • To quantify surface reconstruction during potential cycling using advanced imaging techniques.
  • To correlate surface heterogeneity with electrochemical reactivity.

Main Methods:

  • Utilized optical second harmonic imaging combined with cyclic voltammetry.
  • Employed a wide-field microscope for real-time imaging of approximately 100 μm diameter areas with submicron resolution.
  • Analyzed pixel-wise voltage dependence of the second harmonic signal to identify surface domain characteristics.

Main Results:

  • Uncovered heterogeneity in the second harmonic signal across the gold electrode surface.
  • Quantified domains exhibiting a positive quadratic dependence of second harmonic intensity with bias, attributed to electronic polarization.
  • Identified areas with a negative quadratic dependence, correlating with higher roughness, prone to restructuring, and showing significant changes during cyclic voltammetry.

Conclusions:

  • Optical second harmonic imaging effectively maps surface heterogeneity and potential-induced restructuring in nanocatalysts.
  • Specific surface domains with higher roughness exhibit distinct electrochemical behavior and restructuring.
  • The findings provide insights into structure-reactivity relationships crucial for designing advanced electrocatalysts.