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

Författare

Andrea Grespi

Lunds universitet

Alfred Larsson

Leiden Institute of Chemistry

Giuseppe Abbondanza

Chalmers, Fysik, Kemisk fysik

J. Manidi

Politecnico di Milano

J. Eidhagen

Alleima Tube AB

E. Lira

Lunds universitet

A. Ti

Lunds universitet

M. Ramakrishnan

Max IV-laboratoriet

Justus Just

Max IV-laboratoriet

Jinshan Pan

Kungliga Tekniska Högskolan (KTH)

L. R. Merte

Lunds universitet

Malmö universitet

Edvin Lundgren

Lunds universitet

Journal of the Electrochemical Society

0013-4651 (ISSN) 1945-7111 (eISSN)

Vol. 173 7 076502

Ämneskategorier (SSIF 2025)

Materialkemi

Atom- och molekylfysik och optik

DOI

10.1149/1945-7111/ae5bcf

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Senast uppdaterat

2026-04-24