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Cathodic regeneration of a clean and ordered Cu(100)-(1×1) surface from an air-oxidized and disordered electrode: An operando STM study

Kim, Youn-Geun and Soriaga, Manuel P. (2014) Cathodic regeneration of a clean and ordered Cu(100)-(1×1) surface from an air-oxidized and disordered electrode: An operando STM study. Journal of Electroanalytical Chemistry, 734 . pp. 7-9. ISSN 1572-6657. https://resolver.caltech.edu/CaltechAUTHORS:20141001-103653915

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Abstract

In work related to the electrocatalysis of the CO_2 reduction reactions, we recently reported in This Journal the structure and composition of a Cu(100) electrode surface, pre-dosed at low levels of O_(2(g)) to simulate a Cu electrocatalyst unprotected from air, before and after immersion in alkaline electrolyte at fairly negative potentials to ascertain if an oxide-to-metal reduction reaction can be effected; experimental measurements were based upon ex situ techniques, low-energy electron diffraction (LEED) and Auger electron spectroscopy (AES). It was found that the mildly oxided surface remained ordered and could be cathodically reduced back to a well-ordered oxide-free Cu(100); the quality of the LEED pattern and AES spectrum was less than ideal, however, due to small amounts of base electrolyte remnant in the emersed layer. In this Short Communication, we present results from operando electrochemical scanning tunneling microscopy (EC-STM) that not only confirm the earlier observations but, more importantly, depict more accurately the actual electrocatalysis conditions. An as-received commercially oriented Cu(100) disk that had not been protected from air was observed to consist of narrow terraces encrusted with highly disordered oxides. Cyclic voltammetry and coulometry showed that the oxidized surface consisted of five monolayers of CuO and quarter of a monolayer of Cu_2O. Upon complete cathodic reduction of the interfacial oxides, the surface was found to have reverted to a single-crystalline Cu(100)-(1×1) structure. It may thus be inferred that, under the conditions of electrochemical CO_2 reduction, the Cu catalyst would exist as a zerovalent metal.


Item Type:Article
Related URLs:
URLURL TypeDescription
http://dx.doi.org/10.1016/j.jelechem.2014.09.010DOIArticle
http://www.sciencedirect.com/science/article/pii/S1572665714003889PublisherArticle
ORCID:
AuthorORCID
Kim, Youn-Geun0000-0002-5936-6520
Soriaga, Manuel P.0000-0002-0077-6226
Additional Information:© 2014 Elsevier B.V. Received 2 August 2014, Accepted 9 September 2014, Available online 19 September 2014. This material is based upon work performed by the Joint Center for Artificial Photosynthesis, a DOE Energy Innovation Hub, supported through the Office of Science of the U.S. Department of Energy under Award No. DE-SC0004993. There is no conflict of interest among the authors.
Group:JCAP
Funders:
Funding AgencyGrant Number
Department of Energy (DOE)DE-SC0004993
Subject Keywords:Operando electrochemical scanning tunneling microscopy; Copper electrocataysts for co2 reduction; Cathodic regeneration of ordered Cu(hkl) from oxided surfaces; Air-oxidized copper electrocatalyst surfaces; In Situ electrochemical scanning tunneling microscopy
Record Number:CaltechAUTHORS:20141001-103653915
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20141001-103653915
Official Citation:Youn-Geun Kim, Manuel P. Soriaga, Cathodic regeneration of a clean and ordered Cu(100)-(1×1) surface from an air-oxidized and disordered electrode: An operando STM study, Journal of Electroanalytical Chemistry, Volume 734, 15 November 2014, Pages 7-9, ISSN 1572-6657, http://dx.doi.org/10.1016/j.jelechem.2014.09.010. (http://www.sciencedirect.com/science/article/pii/S1572665714003889)
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:50142
Collection:CaltechAUTHORS
Deposited By: Ruth Sustaita
Deposited On:01 Oct 2014 18:12
Last Modified:03 Oct 2019 07:20

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