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Interfacial electrochemical methods focus on the phenomena occurring at the boundary between an electrode and a solution, as opposed to bulk methods that concentrate on the solution's overall properties. These interfacial methods are classified as either static or dynamic based on the presence of a nonzero current in the electrochemical cell and the consistency of analyte concentrations. Static methods, such as potentiometry, measure the cell's potential without any significant current...
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Interfacial pH measurements during CO2 reduction on gold using a rotating ring-disk electrode.

Xuan Liu1, Mariana C O Monteiro1, Marc T M Koper1

  • 1Leiden Institute of Chemistry, Leiden University, 2300 RA Leiden, The Netherlands. m.koper@lic.leidenuniv.nl.

Physical Chemistry Chemical Physics : PCCP
|January 12, 2023
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Understanding interfacial pH is key to controlling electrochemical CO2 reduction. This study maps pH changes near the electrode, revealing buffer capacity

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Area of Science:

  • Electrochemistry
  • Surface Science
  • Chemical Engineering

Background:

  • Electrochemical CO2 reduction (CO2R) control is limited by poor understanding of reaction mechanisms and kinetics.
  • Interfacial pH is a critical, yet poorly understood, parameter in proton-coupled reactions like CO2R.

Purpose of the Study:

  • To investigate and map interfacial pH variations during electrochemical CO2 reduction.
  • To correlate interfacial pH changes with reaction mechanisms and electrolyte effects.

Main Methods:

  • Utilized a sensitive pH sensor integrated with the rotating ring-disk electrode (RRDE) technique.
  • Employed functionalized gold electrodes for real-time detection of hydroxide ions (OH-) generated during CO2R.
  • Conducted scan rate-dependent voltammetry and chronopotentiometry to analyze homogeneous reactions and buffer effects.

Main Results:

  • Mapped interfacial pH from 7 to 12 with increasing current density, noting a sharp rise at -0.5 V vs. RHE.
  • Confirmed homogeneous reactions reach equilibrium within measurement timescales, enabling calculation of interfacial species concentrations.
  • Demonstrated that weakly hydrated alkali metal cations reduce pH gradients and that electrolyte buffer capacity is crucial for suppressing pH variations.

Conclusions:

  • Interfacial pH significantly influences CO2R and can be mapped using advanced electrochemical techniques.
  • Electrolyte buffer capacity and cation hydration play vital roles in moderating interfacial pH gradients.
  • This work provides crucial insights for optimizing CO2R through control of interfacial electrochemical conditions.