Abstract
A Spectro electrochemical cell is described that enables confocal Raman microscopy studies of electrode-supported films. the confocal probe volume (∼1 μm3) was treated as a fixed-volume reservoir for the observation of potential-induced changes in chemical composition at microscopic locations within an ∼20 μm thickness layer of a redox polymer cast onto a 3 mm diameter carbon disk electrode. using a Raman system with high collection efficiency and wavelength reproducibility, spectral subtraction achieved excellent rejection of background interferences, opening opportunities for measuring within micrometer-scale thickness redox films on widely available, low-cost, and conventional carbon disk electrodes. the cell performance and spectral difference technique are demonstrated in experiments that detect transformations of redox-active molecules exchanged into electrode-supported ionomer membranes. then in situ measurements were sensitive to changes in the film oxidation state and swelling/deswelling of the polymer framework in response to the uptake and discharge of charge-compensating electrolyte ions. the studies lay a foundation for confocal Raman microscopy as a quantitative in situ probe of processes within electrode-immobilized redox polymers under development for a range of applications, including electrosynthesis, energy conversion, and chemical sensing.
Recommended Citation
J. Xu et al., "In Situ Confocal Raman Microscopy of Redox Polymer Films on Bulk Electrode Supports," ACS Measurement Science Au, vol. 3, no. 2, pp. 127 - 133, American Chemical Society, Apr 2023.
The definitive version is available at https://doi.org/10.1021/acsmeasuresciau.2c00064
Department(s)
Chemistry
Publication Status
Open Access
Keywords and Phrases
confocal; polymer-modified electrode; Raman microscopy; redox polymer; thin film
International Standard Serial Number (ISSN)
2694-250X
Document Type
Article - Journal
Document Version
Final Version
File Type
text
Language(s)
English
Rights
© 2025 American Chemical Society, All rights reserved.
Creative Commons Licensing
This work is licensed under a Creative Commons Attribution 4.0 License.
Publication Date
19 Apr 2023
Comments
National Science Foundation, Grant CBET-1921075