Bismuth–vanadium oxyfluoride (Bi2VO5F) has been synthesized using a simple, solid-state reaction process at different sintering temperatures. The structure and performance of the samples have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and galvanostatic charge/discharge experiments. The results show that bismuth–vanadium oxyfluoride belongs to a tetragonal crystal system with space group I4mm. The sample that was synthesized at 550°C (P550) exhibits relatively good electrochemical properties. Sample P550 shows a high, initial discharge capacity of 222mAhg−1 at a rate of 100mAg−1 between 1.4 and 3.5V. Sample P550 also shows acceptable electrochemical cycling properties. After the first cycle, the discharge specific capacity remains between 106 and 155mAhg−1, which plateaus between 2.1 and 1.9V during the first 15 cycles.