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2. Li _2.9 Fe _0.9 Zr _0.1 Cl ₆ as Redox-Active Catholyte for Solid-State Li-Ion Batteries

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3. Polymorphism in Weberite Na ₂ Fe ₂ F ₇ and its Effects on Electrochemical Properties as a Na-Ion Cathode

   https://doi.org/10.1021/acs.chemmater.3c00233  

   Foley, Emily E; Wu, Vincent C; Jin, Wen; Cui, Wei; Yoshida, Eric; Manche, Alexis; Clément, Raphaële J (May 2023, Chemistry of Materials)

   Weberite-type sodium transition metal fluorides (Na2M2+Mʹ3+F7) have emerged as potential high performance sodium intercalation cathodes, with predicted energy densities in the 600-800 Wh/kg range and fast Na-ion transport. One of the few weberites that has been electrochemically tested is Na2Fe2F7, yet inconsistencies in its reported structure and electrochemical properties have hampered the establishment of clear structure-property relationships. In this study, we reconcile structural characteristics and electrochemical behavior using a combined experimental-computational approach. First principles calculations reveal the inherent metastability of weberite-type phases, the close energetics of several Na2Fe2F7 weberite polymorphs, as well as their predicted (de)intercalation behavior. We find that as-prepared Na2Fe2F7 samples inevitably contain a mixture of polymorphs, with local probes such as solid-state nuclear magnetic resonance and Mössbauer spectroscopy providing unique insights into the distribution of Na and Fe local environments. Polymorphic Na2Fe2F7 exhibits a respectable initial capacity yet steady capacity fade, a consequence of the transformation of the Na2Fe2F7 weberite phases to the more stable perovskite-type NaFeF3 phase upon cycling, as revealed by ex situ synchrotron X-ray diffraction and solid-state NMR. Overall, these findings highlight the need for greater control over weberite polymorphism and phase stability through compositional tuning and synthesis optimization. 

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