Single-phase marićite, NaFePO4, was synthesized from a mixture of monosodium phosphate and iron oxalate at 750 °C and atmospheric pressure. Thermal treatment of synthetic marićite in air led to its oxidative decomposition into Na3Fe23+(PO4)3 NASICON and α-Fe2O3, which started at temperatures slightly below 225 °C. Intergrowth of the two reaction products is found to occur at the nanoscale without identified crystallographic relationship with the marićite precursor. Electrochemical activity of the reaction product is confirmed with the reversible insertion of one Na at 2.55 V versus Na+/Na0.

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