A parallel line probe for spatially selective electrochemical NMR spectroscopy.

Autor: Luo R; Magnetic Resonance Research Center, Institute for Molecules and Materials, Radboud University, Nijmegen, the Netherlands., Janssen HJWG; Magnetic Resonance Research Center, Institute for Molecules and Materials, Radboud University, Nijmegen, the Netherlands., Kentgens APM; Magnetic Resonance Research Center, Institute for Molecules and Materials, Radboud University, Nijmegen, the Netherlands., Zhao EW; Magnetic Resonance Research Center, Institute for Molecules and Materials, Radboud University, Nijmegen, the Netherlands. Electronic address: evanwenbo.zhao@ru.nl.
Jazyk: angličtina
Zdroj: Journal of magnetic resonance (San Diego, Calif. : 1997) [J Magn Reson] 2024 Apr; Vol. 361, pp. 107666. Date of Electronic Publication: 2024 Mar 24.
DOI: 10.1016/j.jmr.2024.107666
Abstrakt: In situ NMR is a valuable tool for studying electrochemical devices, including redox flow batteries and electrocatalytic reactors, capable of detecting reaction intermediates, metastable states, time evolution of processes or monitoring stability as a function of electrochemical conditions. Here we report a parallel line detector for spatially selective in situ electrochemical NMR spectroscopy. The detector consists of 17 copper wires and is doubly tuned to 1 H/ 19 F and X nuclei ranging from 63 Cu (106.1 MHz) to 7 Li (155.5 MHz). The flat geometry of the parallel line detector allows its insertion into a high electrode surface-to-volume electrochemical flow reactor, enabling a detector-in-a-reactor design. This integrated device is named "eReactor NMR probe". Combined with B 1 -selective pulse sequences, selective detection of the nuclei at the electrode-electrolyte interface, that is within a distance of 800 μm from the electrode surface, has been achieved. The selective detection of 7 Li and 19 F nuclei is demonstrated using two electrolytes, LiCl and LiBF 4 solutions, respectively. A good B 1 homogeneity with an 810° to 90° pulse intensity ratio of 68-72 % was achieved. Using electrochemical plating of lithium metal as a model reaction, we further demonstrated the operando functionality of the probe. The new eReactor NMR probe offers a general method for studying flow electrochemistry, and we envision applications in a wide range of environmentally relevant energy systems, for example, Li metal batteries, electrochemical ammonia synthesis, carbon dioxide capture and reduction, redox flow batteries, fuel cells, water desalination, lignin oxidation etc.
Competing Interests: Declaration of competing interest R. Luo, H. J. W. G. Janssen, A. P. M. Kentgens, E. W. Zhao together with Radboud Innovation (Radboud University Nijmegen) filed a patent application to protect intellectual property embedded within this report and its relation to the use of the eReactor NMR probe.
(Copyright © 2024 The Author(s). Published by Elsevier Inc. All rights reserved.)
Databáze: MEDLINE
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