A Combined Raman Spectroscopy and Atomic Force Microscopy System for In Situ and Real-Time Measures in Electrochemical Cells

Gianlorenzo Bussetti; Marco Menegazzo; Sergei Mitko; Chiara Castiglioni; Matteo Tommasini; Andrea Lucotti; Luca Magagnin; Valeria Russo; Andrea Li Bassi; Martina Siena; Alberto Guadagnini; Samuele Grillo; Davide Del Curto; Lamberto Duò

doi:10.3390/ma16062239

A Combined Raman Spectroscopy and Atomic Force Microscopy System for In Situ and Real-Time Measures in Electrochemical Cells

Materials (Basel). 2023 Mar 10;16(6):2239. doi: 10.3390/ma16062239.

Affiliations

¹ Department of Physics, Politecnico di Milano, 20133 Milan, Italy.
² NT-MDT BV, Hoenderparkweg 96 b, 7335 GX Apeldoorn, The Netherlands.
³ Department of Chemistry, Materials and Chemical Engineering, Politecnico di Milano, 20133 Milan, Italy.
⁴ Department of Energy, Politecnico di Milano, 20133 Milan, Italy.
⁵ Department of Civil and Environmental Engineering, Politecnico di Milano, 20133 Milan, Italy.
⁶ Department of Electronics, Information and Bioengineering, Politecnico di Milano, 20133 Milan, Italy.
⁷ Department of Architecture and Urban Studies, Politecnico di Milano, 20133 Milan, Italy.

Abstract

An innovative and versatile set-up for in situ and real time measures in an electrochemical cell is described. An original coupling between micro-Raman spectroscopy and atomic force microscopy enables one to collect data on opaque electrodes. This system allows for the correlation of topographic images with chemical maps during the charge exchange occurring in oxidation/reduction processes. The proposed set-up plays a crucial role when reactions, both reversible and non-reversible, are studied step by step during electrochemical reactions and/or when local chemical analysis is required.

Keywords: HOPG intercalation; Raman spectroscopy; in situ AFM; solid–liquid interface.

Grants and funding

G. Bussetti acknowledges funding by: Fondazione CARIPLO (grant 2020-0977). A. Li Bassi and V. Russo acknowledge funding by: Funder: Project funded under the National Recovery and Resilience Plan (NRRP), Mission 4 Component 2 Investment 1.3—Call for tender No. 1561 of 11.10.2022 of Ministero dell’Università e della Ricerca (MUR); funded by the European Union–NextGenerationEU Award Number: Project code PE0000021, Concession Decree No. 1561 of 11.10.2022 adopted by Ministero dell’Università e della Ricerca (MUR), CUP D43C22003090001, Project title “Network 4 Energy Sustainable Transition—NEST”.