Publication date: 22nd July 2026
The combination of electrochemistry and near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) offers unique opportunities for probing electrochemical interfaces under realistic conditions. However, truly operando measurements at solid-liquid interfaces remain highly challenging. A key difficulty is the need to follow the evolution of electrolyte-derived elements, here chlorine, while they redistribute across different chemical environments. In particular, the Cl signal must be distinguished as it evolves from solvated perchlorate species in the electrolyte toward possible intercalated states within the electrode structure, despite strong signal attenuation and overlapping interfacial contributions.
Here, we present the recent implementation of an electrochemical NAP-XPS platform developed at the Physics Department at Politecnico di Milano and discuss its potential for operando investigations. Highly oriented pyrolytic graphite (HOPG) in perchloric acid solutions is used as a model system to explore the experimental limitations associated with operando measurements. Ex situ and quasi-operando experiments, including partial immersion and electrochemical treatments, allow discrimination between immersed regions, dry surface areas and the meniscus region, while providing insight into wettability, defect-mediated reactivity and ion intercalation phenomena.
These results highlight the intrinsic complexity of operando NAP-XPS at electrochemical interfaces and establish a methodological framework for tracking ion transfer and intercalation processes under realistic electrochemical conditions, with meniscus-controlled measurements playing a central role in the development of reliable operando methodologies.
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