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K 3 FeF 6 was synthesized through a simple hydrothermal reaction for a novel cathode material of lithium-ion batteries. From the SEM and TEM images, the synthesized K 3 FeF 6 particle are about 30-50 nm after high energy ball milling. K 3 FeF 6 electrode delivers a high reversible capacity of 212.6 mAh g −1 and it maintained 131 mAh g −1 after 30 cycles. Additionally, in rate performance test, when the current density returns back to the 10 mA g −1 again, the full recovery of the capacity exhibits its superior rate performance. The electrochemical redox mechanism, herein studied through Ex-situ XRD of K 3 FeF 6 electrodes at different polarization voltages, shows the satisfactory reversibility of structure.

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