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Single-phase three-dimensional vanadium oxide (V 4 O 9 ) was synthesized by reduction of V 2 O 5 using a gas stream of ammonia/argon (NH 3 /Ar). The as-synthesized oxide, prepared by this simple gas reduction method was subsequently electrochemically transformed into a disordered rock salt type-"Li3.7V4O9" phase while cycling over the voltage window 3.5 to 1.8 V versus Li. The Li-deficient phase delivers an initial reversible capacity of ∼260 mAhg -1 at an average voltage of 2.5 V vs. Li + /Li 0 . Further cycling to 50 cycles yields a steady 225 mAhg -1 . Ex situ X-ray diffraction studies confirmed that (de) intercalation phenomena follows a solid-solution electrochemical reaction mechanism. As demonstrated, the reversibility and capacity utilization of this V 4 O 9 is found to be superior to battery grade, micron-sized V 2 O 5 cathodes in lithium cells., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2023 Senguttuvan, Lee, Key and Johnson.)