Detection of electrocatalytical and -chemical processes by means of in situ flow NMR spectroscopy

Research output: Contribution to journalResearch articleContributedpeer-review

Contributors

  • Anastasia Vyalikh - , Professor (rtd.) for Surface Physics, Institute of Solid State and Materials Physics, TUD Dresden University of Technology, Freiberg University of Mining and Technology (Author)
  • Wolfram Münchgesang - , Freiberg University of Mining and Technology, Fraunhofer Institute for Wind Energy System IWES Leuna (Author)
  • Juan Jesús Velasco-Vélez - , Max Planck Institute for Chemical Energy Conversion, Fritz Haber Institute of the Max Planck Society, Autonomous University of Barcelona (Author)

Abstract

In situ studies of electrochemical processes using NMR offer valuable information on reaction mechanisms, kinetics, and species identification, making it a powerful tool in electrochemistry research. In this study, we present the design of an in situ redox-flow NMR cell that allows for a continuous flow of liquid (electrolyte) or gas, application of electrical voltage, and recording of NMR signals. The utility of this setup is demonstrated through two case studies: electrochemical copper deposition on a gold electrode and the electrochemical conversion of carbon dioxide into hydrocarbon products. Specifically, the presence of multicarbon products containing C–C bonds generated during the electrochemical reduction reaction is confirmed in the 2H NMR spectra in the latter example. These findings highlight the ability of the in situ redox-flow NMR cell to directly monitor reaction intermediates and products, thereby enabling the elucidation of reaction mechanisms for the efficient and selective production of valuable hydrocarbon products through the conversion of CO2 into value-added chemicals. In contrast to other reported in situ NMR cells, the presented cell is suitable for multiple uses, and allows detecting NMR signals not only from exhaust products but also from those formed on the catalyst surface.

Details

Original languageEnglish
Article number107736
JournalElectrochemistry Communications
Volume163
Publication statusPublished - Jun 2024
Peer-reviewedYes

Keywords

ASJC Scopus subject areas

Keywords

  • CO, Copper electrodeposition, Electroreduction, Flow NMR, In situ NMR