Nanoscale Raman Fingerprints of Electrochemically Intercalated Graphite Blisters

Gianlorenzo Bussetti^a, Marco Menegazzo^a, Elia Mazzoletti^a, Rossella Yivlialin^a, Lamberto Duò^a, Chiara Castiglioni^a, Andrea Li Bassi^a, Valeria Russo^a, Emmanuel Maisonhaute^b

^apolitecnico di milano, Piazza Leonardo da Vinci, Milan, Italy

^bSorbonne Université, Institut Parisien de Chimie Moléculaire, UMR 8232 CNRS, France

Proceedings of MATSUS Fall 2026 Conference (MATSUSFall26)

C1 Multiscale Insights into Solid–Liquid Interfaces for Sustainable Energy Technologies

Palma, Spain, 2026 October 26th - 30th

Organizers: Marco Fontana, Elena Magnano, Silvia Nappini and Francesca Risplendi

Oral, Gianlorenzo Bussetti, presentation 391
Publication date: 22nd July 2026

Electrochemical intercalation in layered materials is a key process in energy storage and surface science, enabling the formation of confined phases, local strain, and chemical heterogeneities at the nanoscale [1]. In highly oriented pyrolytic graphite (HOPG), intercalation leads to the formation of blister-like nanostructures that host trapped species and display complex mechanical, structural, and electronic behaviours [2,3]. In this work, individual HOPG blisters are investigated through a multimodal nanoscale approach combining atomic force microscopy (AFM), scanning tunnelling microscopy (STM), Raman spectroscopy, and tip-enhanced Raman spectroscopy (TERS). This combination enables the correlation of topographic, mechanical, atomic-scale, and vibrational information across both the blister body and its highly structured edge regions. AFM and STM reveal the morphology, stiffness, and surface features of the intercalation-induced structures, while Raman and TERS provide spatially resolved spectroscopic fingerprints with enhanced sensitivity to local strain, disorder, and confined molecular species. Particular attention is devoted to blister borders and coalescence regions, where interlayer deformation and chemical confinement are expected to be most pronounced. Local changes in the Raman G-band response and TERS spectra highlight the heterogeneous nature of these nanostructures and suggest the possible encapsulation of gaseous species such as CO, CO₂, and O₂. These findings establish a meaningful analogy between electrochemically generated graphite blisters and gas-filled bubbles in two-dimensional materials. Overall, this study demonstrates that the integration of scanning probe microscopy with advanced Raman techniques is a powerful strategy to unravel the physicochemical complexity of intercalated stratified systems at the nanoscale, with implications for electrochemical interfaces, surface science, and energy-related layered materials.

References:

[1] Goss, C.A. et al Imaging the Incipient Electrochemical Oxidation of Highly Oriented Pyrolytic Graphite. Anal Chem 1993, 65, 1378–1389

[2] Bussetti, et al. A Combined Raman Spectroscopy and Atomic Force Microscopy System for In Situ and Real-Time Measures in Electrochemical Cells. Materials 2023, 16, 2239

[3] Menegazzo, M. et al; Stiffness and Mechanical Manipulation of Blisters Grown on Electrochemically Intercalated Graphite. Electrochim Acta 2024, 488, 144201

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