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Scanning Electrochemical Cell Microscopy (SECCM) in aprotic solvents : practical considerations and applications
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Bentley, Cameron Luke, Kang, Minkyung and Unwin, Patrick R. (2020) Scanning Electrochemical Cell Microscopy (SECCM) in aprotic solvents : practical considerations and applications. Analytical Chemistry, 92 (17). pp. 11673-11680. doi:10.1021/acs.analchem.0c01540 ISSN 0003-2700.
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WRAP-Scanning-Electrochemical-Cell-Microscopy-(SECCM)-aprotic-solvents-Bentley-2020.pdf - Accepted Version - Requires a PDF viewer. Download (1528Kb) | Preview |
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Official URL: http://dx.doi.org/10.1021/acs.analchem.0c01540
Abstract
Many applications in modern electrochemistry, notably electrosynthesis and energy storage/conversion take advantage of the “tunable” physicochemical properties (e.g., proton availability and/or electrochemical stability) of non-aqueous (e.g., aprotic) electrolyte media. This work develops general guidelines pertaining to the use of scanning electrochemical cell microscopy (SECCM) in aprotic solvent electrolyte media to address contemporary structure−electrochemical activity problems. Using the simple outer-sphere Fc0/+ process (Fc = ferrocene) as a model system, high boiling point (low vapor pressure) solvents give rise to highly robust and reproducible electrochemistry, whereas volatile (low boiling point) solvents need to be mixed with suitable low melting point supporting electrolytes (e.g., ionic liquids) or high boiling point solvents to avoid complications associated with salt precipitation/crystallization on the scanning (minutes to hours) timescale. When applied to perform microfabrication — specifically the electrosynthesis of the conductive polymer, polypyrrole — the optimized SECCM set up produces highly reproducible arrays of synthesized (electrodeposited) material on a commensurate scale to the employed pipet probe. Applying SECCM to map electrocatalytic activity — specifically the electro-oxidation of iodide at polycrystalline platinum — reveals unique (i.e., structure-dependent) patterns of surface activity, with grains of specific crystallographic orientation, grain boundaries and areas of high local surface misorientation identified as potential electrocatalytic “hot spots”. The work herein further cements SECCM as a premier technique for structure−function−activity studies in (electro)materials science and will open up exciting new possibilities through the use of aprotic solvents for rational analysis/design in electrosynthesis, microfabrication, electrochemical energy storage/conversion and beyond.
Item Type: | Journal Article | |||||||||||||||
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Subjects: | Q Science > QD Chemistry | |||||||||||||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | |||||||||||||||
Library of Congress Subject Headings (LCSH): | Electrochemistry, Chemistry, Analytic, Nanotechnology, Scanning electrochemical microscopy | |||||||||||||||
Journal or Publication Title: | Analytical Chemistry | |||||||||||||||
Publisher: | American Chemical Society | |||||||||||||||
ISSN: | 0003-2700 | |||||||||||||||
Official Date: | 1 September 2020 | |||||||||||||||
Dates: |
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Volume: | 92 | |||||||||||||||
Number: | 17 | |||||||||||||||
Page Range: | pp. 11673-11680 | |||||||||||||||
DOI: | 10.1021/acs.analchem.0c01540 | |||||||||||||||
Status: | Peer Reviewed | |||||||||||||||
Publication Status: | Published | |||||||||||||||
Reuse Statement (publisher, data, author rights): | 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 http://dx.doi.org/10.1021/acs.analchem.0c01540 | |||||||||||||||
Access rights to Published version: | Restricted or Subscription Access | |||||||||||||||
Date of first compliant deposit: | 22 June 2020 | |||||||||||||||
Date of first compliant Open Access: | 11 June 2021 | |||||||||||||||
RIOXX Funder/Project Grant: |
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