We report the successful electrochemical intercalation of F-ions into a densely packed perovskite oxide from a liquid electrolyte at room temperature. Using galvanostatic oxidation and electrochemical impedance spectroscopy coupled with operando X-ray diffraction, we show that roughly 0.5 equivalents of F-ions can be inserted onto the vacant A-site of the perovskite ReO3. Density functional theory calculations indicate that the intercalated phase is thermodynamically unfavorable compared to other less densely packed polymorphs of ReO3F. Pairing X-ray spectroscopy, neutron total scattering measurements, and magic-angle spinning 19F NMR confirms a rapid decomposition of the product on removal from the cell but nevertheless, these results clearly demonstrate that small anions like fluoride can be intercalated into solids as readily as alkali cations at room temperature, which opens new opportunities to electrochemically fluorinate many new materials.

中文翻译：

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氧化物钙钛矿的电化学氧化氟化

我们报告了在室温下从液体电解质中成功地将F离子电化学嵌入到紧密堆积的钙钛矿氧化物中的过程。使用恒电流氧化和电化学阻抗谱结合操作X射线衍射，我们显示大约0.5当量的F离子可以插入钙钛矿ReO3的空位A上。密度泛函理论计算表明，与ReO3F的其他密度较小的多晶型物相比，插层相在热力学上不利。配对的X射线光谱，中子总散射测量和幻角旋转19F NMR证实了从细胞中去除后产物的快速分解，但是，