Simple setup for in situ electrochemical electron paramagnetic resonance spectroscopy to study organic energy-storage materials
File(s)
Published version
OA Location
Author(s)
Type
Journal Article
Abstract
The design and application of a cost-effective, customisable electrochemical cell suitable for in situ X-band (9–10 GHz) Electron Paramagnetic Resonance (EPR) experiments is demonstrated. The cell is optimized for investigating electrochemical parameters of redox-active polymer films at room temperature using polar organic electrolytes. The polymer film to be studied is directly deposited onto the surface of a platinum wire acting as the working electrode. The three-electrode cylindrical cell design with mutual arrangement of the electrodes, inspired by the “ultramicroelectrode concept”, provides enhanced electrochemical response by minimizing ohmic drop while maintaining flexibility for a wide range of experimental setups. The cell performance is demonstrated using a redox conducting polymeric cathode material for organic radical batteries, namely poly[N,N″-bis(3-(4-oxy(2,2,6,6-tetramethylpiperidin-1-oxyl)butoxy)salicylidene)ethylenediiminato nickel(II)], as a test material. Continuous-wave EPR experiments using a portable benchtop spectrometer at a fixed magnetic field allow detecting the material's state of charge, initialisation of oxidation and reduction processes, as well as estimating electrochemical properties. The cell design presented here enables potentiostatic, galvanostatic, and potentiodynamic measurement modes, while offering the possibility of customisation through 3D printing and the use of various electrode materials.
Date Issued
2026-02-01
Date Acceptance
2025-12-15
Citation
Journal of Magnetic Resonance, 2026, 383
ISSN
1090-7807
Publisher
Elsevier
Journal / Book Title
Journal of Magnetic Resonance
Volume
383
Copyright Statement
© 2025 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
License URL
Identifier
https://www.ncbi.nlm.nih.gov/pubmed/41422694
PII: S1090-7807(25)00182-X
Subjects
Cheap setup
Cyclic voltammetry
Electron paramagnetic resonance spectroscopy
In situ technique
In-tube electrochemical cells
Organic battery materials
Spectroelectrochemistry
Publication Status
Published
Coverage Spatial
United States
Article Number
108010
Date Publish Online
2025-12-18