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In the development of low cost, sustainable, and energy-dense batteries,chloride-based compounds are promising catholyte materials for solid-statebatteries owing to their high Na-ion conductivities and oxidative stabilities.The ability to further improve Na-ion conduction, however, requires anunderstanding of the impact of long-range and local structural features ontransport in these systems. In this study, we leverage different synthesismethods to control polymorphism and cation disorder in Na-Y-Zr-Cl solidelectrolytes and interrogate the impact on Na-ion conduction. We demonstratethe existence of a more conductive P2$_1$/n polymorph of Na$_2$ZrCl$_6$ formedupon ball milling. In Na$_3$YCl$_6$, the R$\bar{3}$ polymorph is shown to bemore conductive than its P2$_1$/n counterpart owing to the presence ofintrinsic vacancies and disorder on the Y sublattice. Transition metal orderingin the Na$_{2.25}$Y$_{0.25}$Zr$_{0.75}$Cl$_6$ composition strongly impactsNa-ion transport, where a greater mixing of Y$^{3+}$ and Zr$^{4+}$ on thetransition metal sublattice facilitates ion migration through partialactivation of Cl rotations at relevant temperatures. Overall, Na-ion transportsensitively depends on the phases and transition metal distributions stabilizedduring synthesis. These results are likely generalizable to other halidecompositions and indicate that achieving control over the synthetic protocoland resultant structure is key in the pursuit of improved catholytes for highvoltage solid-state sodium-ion batteries.

Synthetic control of structure and conduction properties in Na-Y-Zr-Cl solid electrolytes