Scanning Electrochemical Microscopy

Bard, Allen J.; Mirkin, Michael V.

doi:10.1201/b11850

Cited by 258 publications

(59 citation statements)

References 15 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…In traditional electrochemical imaging approaches, the electrochemical current is recorded at a fixed potential of interest and, typically, only one or a few images are recorded. [1][2][3] Dynamic imaging was reported by Wipf 4,5 and Schuhmann 6 by combining scanning electrochemical microscopy (SECM) with time-dependent techniques, such as cyclic voltammetry (CV) and potential pulse methods, although this type of approach has not been widely adopted and has not been used to gain information on heterogeneous electrode surface activity, having employed rather large probe electrodes.…”

Section: Introductionmentioning

confidence: 99%

Voltammetric Scanning Electrochemical Cell Microscopy: Dynamic Imaging of Hydrazine Electro-oxidation on Platinum Electrodes

et al. 2015

View full text Add to dashboard Cite

(2015) Voltammetric scanning electrochemical cell microscopy : dynamic imaging of hydrazine electro-oxidation on platinum electrodes. Analytical Chemistry Permanent WRAP url: http://wrap.warwick.ac.uk/67791 Copyright and reuse:The Warwick Research Archive Portal (WRAP) makes this work of researchers of the University of Warwick available open access under the following conditions. Copyright © and all moral rights to the version of the paper presented here belong to the individual author(s) and/or other copyright owners. To the extent reasonable and practicable the material made available in WRAP has been checked for eligibility before being made available.Copies of full items can be used for personal research or study, educational, or not-forprofit purposes without prior permission or charge. Provided that the authors, title and full bibliographic details are credited, a hyperlink and/or URL is given for the original metadata page and the content is not changed in any way. Publisher's statement:This document is the Accepted Manuscript version of a Published Work that appeared in final form in Analytical Chemistry copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see link to Published Work, http://pubs.acs.org/page/policy/articlesonrequest/index.html]The version presented here may differ from the published version or, version of record, if you wish to cite this item you are advised to consult the publisher's version. Please see the 'permanent WRAP url' above for details on accessing the published version and note that access may require a subscription. Abstract:Voltammetric scanning electrochemical cell microscopy (SECCM) incorporates cyclic voltammetry measurements in the SECCM imaging protocol, by recording electrochemical currents in a wide potential window at each pixel in a map. This provides much more information compared to traditional fixed potential imaging. Data can be represented as movies (hundreds of frames) of current (over a surface region) at a series of potentials and are highly revealing of subtle variations in electrode activity. Furthermore, by combining SECCM data with other forms of microscopy, e.g. scanning electron microscopy and electron backscatter diffraction data, it is possible to directly relate the current-voltage characteristics to spatial position and surface structure. In this work we use a 'hopping mode', where the SECCM pipet probe is translated towards the surface at a series of positions until meniscus contact. Small amounts of residue left on the surface, upon probe retraction, demark the precise area of each measurement. We use these techniques to study hydrazine oxidation on a polycrystalline platinum substrate in air and in a deaerated environment. In both cases, the detected faradaic current shows a structural dependence on the surface crystallographic orientation. Significantly, in the presence of oxygen (aerated solution) the electrochemical current decreases strongly for alm...

show abstract

Section: Introductionmentioning

confidence: 99%

Voltammetric Scanning Electrochemical Cell Microscopy: Dynamic Imaging of Hydrazine Electro-oxidation on Platinum Electrodes

et al. 2015

View full text Add to dashboard Cite

show abstract

“…When deployed as the tip in scanning electrochemical microscopy (SECM), these electrodes have enabled the measurement of pH with high spatial resolution at interfaces. [11][12][13][14] The scale on which pH electrodes can be made has advanced in recent years to the micro 15,16 and nano scale. 17,18 SECM pH probes employing a variety of metal/metal oxides have been reported previously.…”

Section: Introductionmentioning

confidence: 99%

Fabrication and Characterization of Dual Function Nanoscale pH-Scanning Ion Conductance Microscopy (SICM) Probes for High Resolution pH Mapping

et al. 2013

View full text Add to dashboard Cite

(2013) Fabrication and characterization of dual function nanoscale pH-scanning ion conductance microscopy (SICM) probes for high resolution pH mapping. Analytical Chemistry, Volume 85 (Number 17). pp. 8070-8074 Permanent WRAP url: http://wrap.warwick.ac.uk/57249 Copyright and reuse:The Warwick Research Archive Portal (WRAP) makes this work of researchers of the University of Warwick available open access under the following conditions. Copyright © and all moral rights to the version of the paper presented here belong to the individual author(s) and/or other copyright owners. To the extent reasonable and practicable the material made available in WRAP has been checked for eligibility before being made available.Copies of full items can be used for personal research or study, educational, or not-forprofit purposes without prior permission or charge. Provided that the authors, title and full bibliographic details are credited, a hyperlink and/or URL is given for the original metadata page and the content is not changed in any way. Publisher's statement:This document is the Accepted Manuscript version of a Published Work that appeared in final form in Analytical Chemistry copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work http://dx.doi.org/10.1021/ac401883n The version presented here may differ from the published version or, version of record, if you wish to cite this item you are advised to consult the publisher's version. Please see the 'permanent WRAP url' above for details on accessing the published version and note that access may require a subscription. AbstractThe easy fabrication and use of nanoscale dual function pH-scanning ion conductance microscopy (SICM) probes is reported. These probes incorporate an iridium oxide coated carbon electrode for pH measurement and an SICM barrel for distance control, enabling simultaneous pH and topography mapping. These pH-SICM probes were fabricated rapidly from laser pulled theta quartz pipets, with the pH electrode prepared by in-situ carbon filling of one of the barrels by the pyrolytic decomposition of butane, followed by electrodeposition of a thin layer of hydrous iridium oxide. The other barrel was filled with an electrolyte solution and Ag/AgCl electrode as part of a conductance cell for SICM. The fabricated probes, with pH and SICM sensing elements typically on the 100 nm scale, were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy and various electrochemical measurements. They showed a linear super-Nernstian pH response over a range of pH (pH 2-10). The capability of the pH-SICM probe was demonstrated by detecting both pH and topographical changes during the dissolution of a calcite microcrystal in aqueous solution. This system illustrates the quantitative nature of pH-SICM imaging, because the dissolution process changes the crystal height and interfacial pH (compared to bulk) and each is sensitive to the rate. Both measurements reve...

show abstract

“…32 First, is the possibility of mapping topography and reactivity simultaneously in exactly same location (unlike double-barrel combined SECM-SICM probes) 10,33 and without need for special apparatus as required, for example, for shear force-SECM, 34 SECM-atomic force microscopy (AFM) 35,36 and intermittent contact-SECM. 37 SECM alone has the issue that topography and activity are not easily separated.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Interfacial Reactivity and Topography Mapping with Scanning Ion Conductance Microscopy

et al. 2016

View full text Add to dashboard Cite

Scanning ion conductance microscopy (SICM) is a powerful technique for imaging the topography of a wide range of materials and interfaces. In this report we develop the use and scope of SICM, showing how it can be used for mapping spatial distributions of ionic fluxes due to (electro)chemical reactions occurring at interfaces. The basic idea is that there is a change of ion conductance inside a nanopipette probe when it approaches an active site, where the ionic composition is different to that in bulk solution, and this can be sensed via the current flow in the nanopipette with an applied bias. Careful tuning of the tip potential allows the current response to be sensitive to either topography or activity, if desired. Furthermore, the use of a distance modulation SICM scheme allows reasonably faithful probe positioning using the resulting AC response, irrespective of whether there is a reaction at the interface that changes the local ionic composition. Both strategies (distance modulation or tuned bias) allow simultaneous topographyactivity mapping with a single channel probe. The application of SICM reaction imaging is demonstrated on several examples, including voltammetric mapping of electrocatalytic reactions on electrodes and high-speed electrochemical imaging at rates approaching 4 s per image frame.These two distinct approaches provide movies of electrochemical current as a function of potential with hundreds of frames (images) of surface reactivity, to reveal a wealth of spatiallyresolved information on potential (and time) -dependent electrochemical phenomena. The experimental studies are supported by detailed finite element method modeling that places the technique on a quantitative footing.

show abstract

Scanning Electrochemical Microscopy

Cited by 258 publications

References 15 publications

Voltammetric Scanning Electrochemical Cell Microscopy: Dynamic Imaging of Hydrazine Electro-oxidation on Platinum Electrodes

Voltammetric Scanning Electrochemical Cell Microscopy: Dynamic Imaging of Hydrazine Electro-oxidation on Platinum Electrodes

Fabrication and Characterization of Dual Function Nanoscale pH-Scanning Ion Conductance Microscopy (SICM) Probes for High Resolution pH Mapping

Simultaneous Interfacial Reactivity and Topography Mapping with Scanning Ion Conductance Microscopy

Contact Info

Product

Resources

About