Journal
SMALL
Volume 17, Issue 42, Pages -Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/smll.202103213
Keywords
electrochemistry; grazing incidence wide-angle X-ray scattering; in situ; operando; organic mixed ionic-electronic conductors; polymers
Categories
Funding
- National Science Foundation
- NSF [DMR-1751308]
- TomKat Center for Sustainable Energy at Stanford University
- U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory [DE-AC02-06CH11357]
- U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences [DE-AC02-76SF00515]
- SHyNE Resource [NSF ECCS-2025633, NSF DMR-1720139]
- MRSEC program of the National Science Foundation [DMR-1720139]
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This study presents a new methodology for in situ/operando X-ray characterization of electroactive polymer thin films in electrochemical applications. The method effectively separates electrolyte scattering, improves sensitivity to structural changes, and has multimodal potential.
Electroactive polymer thin films undergo repeated reversible structural change during operation in electrochemical applications. While synchrotron X-ray scattering is powerful for the characterization of stand-alone and ex situ organic thin films, in situ/operando structural characterization has been underutilized-in large part due to complications arising from supporting electrolyte scattering. This has greatly hampered the development of application relevant structure property relationships. Therefore, a new methodology for in situ/operando X-ray characterization that separates the incident and scattered X-ray beam path from the electrolyte is developed. As a proof of concept, the operando structural characterization of weakly-scattering, organic mixed conducting thin films in an aqueous electrolyte environment is demonstrated, accessing previously unexplored changes in the pi-pi peak and diffuse scatter, while capturing the solvent swollen thin film structure which is inaccessible in previous ex situ studies. These in situ/operando measurements improve the sensitivity to structural changes, capturing minute changes not possible ex situ, and have multimodal potential such as combined Raman measurements that also serve to validate the true in situ/operando conditions of the cell. Finally, new directions enabled by this in situ/operando cell design are examined and state of the art measurements are compared.
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