Following the Electrochemical Oxidation of Au(111) in Real-Time Using Surface Optical Reflectance and Total-Reflection X-Ray Absorption Spectroscopy
Journal article, 2026
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.
operando surface optical reflectance
electrocatalysis
oxidation
cyclic voltammetry
operando total reflection X-ray absorption spectroscopy
Author
Andrea Grespi
Lund University
Alfred Larsson
Leiden Institute of Chemistry
Giuseppe Abbondanza
Chalmers, Physics, Chemical Physics
J. Manidi
Polytechnic University of Milan
J. Eidhagen
Alleima Tube AB
E. Lira
Lund University
A. Ti
Lund University
M. Ramakrishnan
MAX IV Laboratory
Justus Just
MAX IV Laboratory
Jinshan Pan
Royal Institute of Technology (KTH)
L. R. Merte
Lund University
Malmö university
Edvin Lundgren
Lund University
Journal of the Electrochemical Society
0013-4651 (ISSN) 1945-7111 (eISSN)
Vol. 173 7 076502Subject Categories (SSIF 2025)
Materials Chemistry
Atom and Molecular Physics and Optics
DOI
10.1149/1945-7111/ae5bcf