High-Vacuum Scanning Electron Microscopy Characterization of Electrochemical Reactions

Electrochemical reactions like HER and ORR are vital for fuel cells and electrolyzers but studying them under environmental conditions limits spatial and temporal resolution. This work introduces a high-vacuum-compatible electrochemical cell that allows in situ SEM observation of electrochemical processes. The system overcomes vacuum challenges, maintains electrochemical stability, and enables electron beam interaction with the reaction environment.ObjectivesThe study aims to develop a high-vacuum electrochemical cell for real-time SEM observation of electrochemical reactions. The system sustains low-pressure reactions while regulating hydrogen and oxygen evolution. A non-MOF-based gas management system integrates metal hydrides and Zr-based alloys to control gases. SEM-based signals are extracted using BSE, REELS, and SE to analyze surface interactions.Materials & MethodsThe cell features a single working electrode and a microfluidic system for stable ion transport. An electron-transparent SiN window enables SEM imaging while maintaining vacuum integrity. Gas evolution is regulated with metal hydrides for hydrogen control and Zr alloys for oxygen capture. Capillary channels and microporous membranes optimize gas diffusion and maintain signal clarity.ConclusionThis study introduces a high-vacuum electrochemical cell for real-time nanoscale observation of electrochemical reactions. It bridges atmospheric studies with high-resolution SEM imaging. Future research will enhance membrane sealing and electrochemical stability for energy conversion and storage applications.ReferencesYoshida K., Sasaki Y., Kuwabara A., & Ikuhara Y. (2022). Reliable electrochemical setup for in situ observations with an atmospheric SEM. J. Microsc., DOI: 10.1093/jmicro/dfac028de Jonge N., & Ross F.M. (2011). Electron microscopy of specimens in liquid. Nat. Nanotechnol., DOI: 10.1038/NNANO.2011.161Tortora L., & Bussetti G. (2023). Surface and Interface Modification of Graphite and Graphene-Based Materials for Energy and Sensor Applications. Molecules, mdpi.com/journal/molecules This site uses cookies for statistics and to improve your navigation and web applicat