Surface Enhanced Infrared Spectroelectrochemistry using a Microband Electrode

Publication: Canadian Journal of Chemistry4 November 2021https://doi.org/10.1139/cjc-2021-0183

Abstract

The successful use of a microband electrode printed on a silicon internal reflection element to perform time resolved infrared spectroscopy is described. Decreasing the critical dimension of the microband electrode to several hundred micrometers provides a sub-microsecond time constant in a Kretschmann configured spectroelectrochemical cell. The high brilliance of synchrotron sourced infrared radiation has been combined with a specially designed horizontal attenuated total reflectance (ATR) microscope to focus the infrared beam on the microband electrode. The first use of a sub-microsecond time constant working electrode for ATR surface enhanced infrared absorption spectroscopy (ATR-SEIRAS) is reported. Measurements show that the advantage afforded by the high brilliance of the synchrotron source is at least partially offset by increased noise from the experimental floor. The test system was the potential induced desorption of an adsorbed monolayer of 4-methoxypyridine as measured using step-scan interferometry. Based on diffusion considerations alone, the expected time scale of the process was less than 10 microseconds but was experimentally measured to be three orders of magnitude slower. A defect-mediated dissolution of the condensed film is speculated to be the underlying cause of the unexpected slow kinetics.

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Received: 7 July 2021
Published online: 4 November 2021

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Tyler A. Morhart
University of Saskatchewan, 7235, Department of Chemistry, Saskatoon, Saskatchewan, Canada
Canadian Light Source Inc, 117197, Saskatoon, Saskatchewan, Canada
Kaiyang Tu
University of Saskatchewan, 7235, Department of Chemistry, Saskatoon, Saskatchewan, Canada
Canadian Light Source Inc, 117197, Saskatoon, Saskatchewan, Canada
Stuart Read
Canadian Light Source Inc, 117197, Saskatoon, Saskatchewan, Canada
Scott M Rosendahl
Canadian Light Source Inc, 117197, Department of Chemistry, Saskatoon, Saskatchewan, Canada
Garth Wells
Canadian Light Source Inc, 117197, Department of Chemistry, Saskatoon, Saskatchewan, Canada
Sven Achenbach
University of Saskatchewan, 7235, Department of Electrical and Computer Engineering, Saskatoon, Saskatchewan, Canada
Ian J Burgess ian.burgess@usask.ca
University of Saskatchewan, 7235, Department of Chemistry, Saskatoon, Saskatchewan, Canada

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