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Hopping Intermittent Contact-Scanning Electrochemical Microscopy (HIC-SECM): Visualizing Interfacial Reactions and Fluxes from Surfaces to Bulk Solution

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    Hopping Intermittent Contact-Scanning Electrochemical Microscopy (HIC-SECM): Visualizing Interfacial Reactions and Fluxes from Surfaces to Bulk Solution
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    † Department of Chemistry, University of Warwick, Coventry, U.K. CV4 7AL
    ‡ Molecular Organization and Assembly in Cells (MOAC) Doctoral Training Centre (DTC), University of Warwick, Coventry, U.K. CV4 7AL
    *E-mail: [email protected]
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    Analytical Chemistry

    Cite this: Anal. Chem. 2013, 85, 5, 2937–2944
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    https://doi.org/10.1021/ac303642p
    Published February 4, 2013
    Copyright © 2013 American Chemical Society
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    Abstract

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    Hopping intermittent contact-scanning electrochemical microscopy (HIC-SECM) is introduced as a powerful new technique for the quantitative visualization of redox activity and concentration at and above a surface of interest. HIC-SECM combines a hopping imaging mode, in which data are acquired at a tip as a function of distance (z) from the surface, at a series of x, y pixels across the surface, using the principles of intermittent contact to provide a nonelectrochemical means of determining when the tip and the substrate come into contact. The implementation of HIC-SECM is described, and SECM feedback measurements in three-dimensional (3D) space over a gold band array are presented. To demonstrate the generality of the methodology, flux imaging is also carried out over a Pt-disk ultramicroelectrode (UME) in the feedback mode and substrate generation/tip collection mode. The type of information that can be extracted from the data sets acquired include x-y current maps at a well-defined tip–substrate separation (parallel to the surface), x-z current maps (normal to the surface), 3D x-y-z profiles, approach curves at particular spots on the surface of interest, and surface topography. Moreover, because HIC-SECM utilizes an oscillating probe, alternating current data are also obtained that greatly enhances the information content compared to other types of electrochemical imaging. Furthermore, interfacial fluxes are ubiquitous in chemistry and allied areas, and HIC-SECM opens up the possibility of detailed flux visualization in three dimensions for many physicochemical processes.

    Copyright © 2013 American Chemical Society

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    Measured oscillation amplitude at three z distances as a function of x-y position, collected in the HIC-SECM scan of gold bands on glass. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Analytical Chemistry

    Cite this: Anal. Chem. 2013, 85, 5, 2937–2944
    Click to copy citationCitation copied!
    https://doi.org/10.1021/ac303642p
    Published February 4, 2013
    Copyright © 2013 American Chemical Society
    Request reuse permissions

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