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Electroactive polymer thin films undergo repeated reversible structuralchange during operation in electrochemical applications. While synchrotronX-ray scattering is powerful for the characterization of stand-alone andex-situ organic thin films, in situ structural characterization has beenunderutilized--in large part due to complications arising from supportingelectrolyte scattering. This has greatly hampered the development ofapplication relevant structure property relationships. Therefore, we havedeveloped a new methodology for in situ and operando X-ray characterizationthat separates the incident and scattered X-ray beam path from the electrolyte.As a proof of concept, we demonstrate the in situ structural changes ofweakly-scattering, organic mixed ionic-electronic conductor thin films in anaqueous electrolyte environment, enabling access to previously unexploredchanges in the pi-pi peak and diffuse scatter in situ, while capturing thesolvent swollen thin film structure which was inaccessible in previous ex situstudies. These in situ measurements improve the sensitivity to structuralchanges, capturing minute changes not possible ex situ, and have multimodalpotential such as combined Raman measurements that also serve to validate thetrue in situ/operando conditions of the cell. Finally, we examine newdirections enabled by this operando cell design and compare state of the artmeasurements.

Electrochemistry of thin films with operando grazing incidence X-ray  scattering: bypassing electrolyte scattering for high fidelity time resolved  studies