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In Situ Quantification of a Wetted Surface Area during Scanning Electrochemical Cell Microscopy Using Retraction

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This study introduces a new method using retraction curves to accurately measure the working electrode surface area during scanning electrochemical cell microscopy (SECCM) in real-time. This technique improves quantitative analysis of local current density values.

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Area of Science:

  • Electrochemistry
  • Surface Science
  • Analytical Chemistry

Background:

  • Scanning electrochemical cell microscopy (SECCM) is a powerful technique for local electrochemical analysis.
  • Accurate determination of the working electrode surface area is crucial for quantitative SECCM measurements.
  • Current methods for surface area determination are often time-consuming or provide averaged values.

Purpose of the Study:

  • To develop and validate a novel in situ methodology for estimating the working electrode surface area during SECCM using retraction curves.
  • To compare the accuracy of the retraction curve method with traditional ex situ techniques.
  • To investigate the influence of experimental parameters on the estimated wetted surface area.

Main Methods:

  • Measuring current as a function of pipet displacement in the z-direction during SECCM.
  • Identifying droplet detachment point to estimate droplet contact diameter.
  • Utilizing goniometry and silanized pipet measurements to confirm droplet spreading effects.
  • Comparing in situ retraction curve measurements with ex situ correlative image analysis.

Main Results:

  • Retraction curves provide real-time estimation of the wetted electrode surface area at each measurement point.
  • Estimated surface areas using retraction curves were smaller than ex situ droplet footprint measurements due to post-retraction droplet spreading.
  • The retraction curve method showed good agreement with true wetted surface areas after surface cleaning and was more accurate than pipet aperture estimations.
  • Experimental parameters like approach separation, retraction rates, and probe diameter were analyzed for their effect on droplet contact size.

Conclusions:

  • Retraction curves offer a reliable and accurate in situ method for determining working electrode surface area in SECCM.
  • This technique overcomes limitations of ex situ methods and provides more precise local current density values.
  • The findings enhance the quantitative capabilities of SECCM for surface analysis.