Li-ion batteries have received attention as rechargeable power sources for room temperature consumer applications since the commercialization of Sony’s lithium-ion cell in 1990 [1–8]. New lithiated transition-metal oxides, such as LiNiVO4 and LiCoVO4 have been recently proposed as cathode materials for modern rechargeable batteries [9, 10]. These materials are very attractive for their use in the so-called Li ion or rockingchair batteries due to their theoretical capacity of about 148 mA hg−1 and their high potential of 4.8 V vs. Li+/Li [11, 12]. Therefore, the preparation of LiMVO4 (M Ni, Co) for battery applications has been of considerable interest [13–16]. Solid-state reactions are often used to prepare LiMVO4, but they are not economical owing to the amount of energy (high temperature) and long reaction time required. In order to overcome these drawbacks, in the present work, we describe a simple procedure for the preparation of bulk quantities of nanosized particles of high crystalline LiNi0.5Co0.5VO4 at a low temperature of 450 ◦C. LiNi0.5Co0.5VO4 sample was prepared first by dissolving stoichiometric quantities of Li2CO3, Ni2(OH)2CO3, Co(Ac)2 and NH4VO3in de-ionized water. During vigorous stirring and ultrasonic treatment, saturated citric acid solution and polyethylene glicol solution were added, which gave off a great deal of gas, and a brown xerogel was obtained after being heated at 80–100 ◦C. The as-obtained xerogel was heated at 450 ◦C for 4 h, accompanied by obvious combustion, which ultimately gave rise to a brown powder. Thermal analyses of the precursor complex were performed using a Netzsch STA 449C DSC-TG apparatus. Experiment was carried out under ambient atmosphere with a heating rate of 10 ◦C/min. Xray diffraction (XRD) experiments were done on a HZG4/B-PC X-ray diffractrometer with Co Kα radiation and graphite monochrometer. Fourier transform infrared (FTIR) absorption spectra were recorded using a 60-SXB IR spectrometer with a resolution of 4 cm−1. The measuring wavenumber range is 300–3900 cm−1. Transmission electron microscopic (TEM) images were collected by employing a JEM-100CX II transmission electron microscope at 80 kV. The metal contents were determined by inductively coupled plasmaatomic emission spectroscopy (PLASMA 300) with the accuracy of ±0.1%. The cathode preparation and the cell test were similar to that described in Ref. 15.