Williams, Cara G., Edwards, Martin A., Colley, Anna L., Macpherson, Julie V. and Unwin, Patrick R.. (2009) Scanning micropipet contact method for high-resolution imaging of electrode surface redox activity. Analytical Chemistry, Vol.81 (No.7). pp. 2486-2495. ISSN 0003-2700

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Abstract

A scanning micropipet contact method (SMCM) is described which promises wide-ranging application in imaging and quantifying electrode activity at high spatial resolution. In SMCM, a moveable micropipet probe (diameter 300 nm to 1 mu m) containing an electroactive species in electrolyte solution is brought to a sample electrode surface so that the liquid meniscus makes contact. The micropipet contains a reference-counter electrode, and the sample is connected as the working electrode to make a two-electrode voltammetric measurement. SMCM thus makes possible highly localized electrochemical experiments, and furthermore, heterogeneous electrode surfaces may be investigated without the substrate being completely immersed in solution. This opens up the possibility of making measurements on a wide range of electrode materials without having to encapsulate the electrode. Furthermore, the electrode/solution contact can be made rapidly and briefly, which is useful for situations where the electrode would be unstable for longer periods (e.g., due to corrosion or surface adsorption). For heterogeneously active surfaces the technique is particularly powerful as it allows defined areas to be targeted and individual sites to be probed. To exemplify the approach, the electroactivity of basal plane highly oriented pyrolytic graphite (HOPG) and two types of aluminum alloy were investigated. SMCM measurements indicate that basal plane HOPG shows much greater activity than present consensus. Measurements of chemically heterogeneous aluminum alloy surfaces with SMCM allow variations in redox activity to be mapped with high spatial resolution.

Item Type:	Journal Article
Subjects:	Q Science > QD Chemistry Q Science > QH Natural history > QH301 Biology
Divisions:	Faculty of Science > Chemistry
Library of Congress Subject Headings (LCSH):	Micropipettes, Atomic force microscopy, Electrodes, Electrochemistry, Charge exchange, Nanotubes, Oxidation-reduction reaction
Journal or Publication Title:	Analytical Chemistry
Publisher:	American Chemical Society
ISSN:	0003-2700
Official Date:	1 April 2009
Volume:	Vol.81
Number:	No.7
Number of Pages:	10
Page Range:	pp. 2486-2495
Identification Number:	10.1021/ac802114r
Status:	Peer Reviewed
Publication Status:	Published
Access rights to Published version:	Restricted or Subscription Access
Funder:	Engineering and Physical Sciences Research Council (EPSRC), Novelis, GlaxoSmithKline
URI:	http://wrap.warwick.ac.uk/id/eprint/28229

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