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Following the Electrochemical Oxidation of Au(111) in Real-Time Using Surface Optical Reflectance and Total-Reflection X-Ray Absorption Spectroscopy

Grespi, A. LU orcid ; Larsson, A. LU orcid ; Abbondanza, G. LU ; Manidi, J. ; Eidhagen, J. ; Lira, E. LU ; Ti, A. LU orcid ; Ramakrishnan, M. LU ; Just, J. LU orcid and Pan, J. LU , et al. (2026) In Journal of the Electrochemical Society 173(7).
Abstract

Under electrochemical polarization, many electrocatalysts can undergo oxidation that alters their reactivity and can lead to restructuring and dissolution. In this context, the structure-property relationships of electrocatalysts, as well as their kinetics and dynamic behaviour, are still poorly understood. This knowledge gap mainly relies on the limitations of many traditional spectroscopic and structure determination methods, which cannot be easily coupled in situ with electrochemical methods. In this work, we performed cyclic voltammetry (CV) combined with 2D surface optical reflectance (2D-SOR) and total reflection X-ray absorption spectroscopy (RefleXAFS) in a single operando experiment, to directly follow the electro-oxidation and... (More)

Under electrochemical polarization, many electrocatalysts can undergo oxidation that alters their reactivity and can lead to restructuring and dissolution. In this context, the structure-property relationships of electrocatalysts, as well as their kinetics and dynamic behaviour, are still poorly understood. This knowledge gap mainly relies on the limitations of many traditional spectroscopic and structure determination methods, which cannot be easily coupled in situ with electrochemical methods. In this work, we performed cyclic voltammetry (CV) combined with 2D surface optical reflectance (2D-SOR) and total reflection X-ray absorption spectroscopy (RefleXAFS) in a single operando experiment, to directly follow the electro-oxidation and reduction of a Au(111) model electrode. Our results show that the surface in 0.05 M H2SO4 forms a self-limiting Au3+ oxide or hydroxide film around 1.5 VRHE during the anodic scan in the CV (2 mV s−1), with a thickness of ∼5 Å estimated from the 2D-SOR measurements. The film is then rapidly reduced during the cathodic scan around 1.1 VRHE.

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organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
cyclic voltammetry, electrocatalysis, operando surface optical reflectance, operando total reflection X-ray absorption spectroscopy, oxidation
in
Journal of the Electrochemical Society
volume
173
issue
7
article number
076502
publisher
IOP Publishing
external identifiers
  • scopus:105035803321
ISSN
0013-4651
DOI
10.1149/1945-7111/ae5bcf
language
English
LU publication?
yes
additional info
Publisher Copyright: © 2026 The Author(s). Published on behalf of The Electrochemical Society by IOP Publishing Limited.
id
cafcadac-3ad3-47e9-87c8-53c3f35b759a
date added to LUP
2026-04-29 13:40:35
date last changed
2026-05-05 08:28:01
@article{cafcadac-3ad3-47e9-87c8-53c3f35b759a,
  abstract     = {{<p>Under electrochemical polarization, many electrocatalysts can undergo oxidation that alters their reactivity and can lead to restructuring and dissolution. In this context, the structure-property relationships of electrocatalysts, as well as their kinetics and dynamic behaviour, are still poorly understood. This knowledge gap mainly relies on the limitations of many traditional spectroscopic and structure determination methods, which cannot be easily coupled in situ with electrochemical methods. In this work, we performed cyclic voltammetry (CV) combined with 2D surface optical reflectance (2D-SOR) and total reflection X-ray absorption spectroscopy (RefleXAFS) in a single operando experiment, to directly follow the electro-oxidation and reduction of a Au(111) model electrode. Our results show that the surface in 0.05 M H<sub>2</sub>SO<sub>4</sub> forms a self-limiting Au<sup>3+</sup> oxide or hydroxide film around 1.5 V<sub>RHE</sub> during the anodic scan in the CV (2 mV s<sup>−1</sup>), with a thickness of ∼5 Å estimated from the 2D-SOR measurements. The film is then rapidly reduced during the cathodic scan around 1.1 V<sub>RHE</sub>.</p>}},
  author       = {{Grespi, A. and Larsson, A. and Abbondanza, G. and Manidi, J. and Eidhagen, J. and Lira, E. and Ti, A. and Ramakrishnan, M. and Just, J. and Pan, J. and Merte, L. R. and Lundgren, E.}},
  issn         = {{0013-4651}},
  keywords     = {{cyclic voltammetry; electrocatalysis; operando surface optical reflectance; operando total reflection X-ray absorption spectroscopy; oxidation}},
  language     = {{eng}},
  month        = {{04}},
  number       = {{7}},
  publisher    = {{IOP Publishing}},
  series       = {{Journal of the Electrochemical Society}},
  title        = {{Following the Electrochemical Oxidation of Au(111) in Real-Time Using Surface Optical Reflectance and Total-Reflection X-Ray Absorption Spectroscopy}},
  url          = {{http://dx.doi.org/10.1149/1945-7111/ae5bcf}},
  doi          = {{10.1149/1945-7111/ae5bcf}},
  volume       = {{173}},
  year         = {{2026}},
}