操作掠入射X射线散射下薄膜的电化学：避开电解质散射用于高保真时间分辨研究
Electrochemistry of thin films with operando grazing incidence X-ray scattering: bypassing electrolyte scattering for high fidelity time resolved studies
摘要：
电活性聚合物薄膜在电化学应用中的操作期间经历重复的可逆结构变化。虽然同步辐射X射线散射是强大的独立和非原位有机薄膜的表征，原位结构表征一直未得到充分利用-在很大程度上是由于支持电解质散射所产生的并发症。这极大地阻碍了与应用相关的结构属性关系的发展。因此，我们已经开发了一种新的方法，在原位和operando X射线表征，分离的入射和散射的X射线光束路径的电解质。作为一个概念的证明，我们证明了在原位的弱散射，有机混合离子-电子导体薄膜在水性电解质环境中的结构变化，使访问以前未探索的变化，在π-π峰和扩散散射原位，同时捕获的溶剂溶胀薄膜结构，这是在以前的非原位研究无法访问。这些原位测量提高了对结构变化的灵敏度，捕获了不可能的非原位微小变化，并且具有多模态潜力，例如组合拉曼测量，其也用于验证电池的真实原位/操作条件。最后，我们研究了新的方向，使这个operando细胞的设计和比较最先进的测量。
英文摘要：
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 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, we have developed a new methodology for in situ and operando X-ray characterization that separates the incident and scattered X-ray beam path from the electrolyte. As a proof of concept, we demonstrate the in situ structural changes of weakly-scattering, organic mixed ionic-electronic conductor thin films in an aqueous electrolyte environment, enabling access to previously unexplored changes in the pi-pi peak and diffuse scatter in situ, while capturing the solvent swollen thin film structure which was inaccessible in previous ex situ studies. These in situ 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, we examine new directions enabled by this operando cell design and compare state of the art measurements.
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