Double doped spinel LiCo (x) Ni (y) Mn2-x-y O-4 (x = y = 0.25) have been synthesised via sol-gel method using different chelating agents viz., acetic acid, maleic acid and oxalic acid to obtain 5 V positive electrode material for use in lithium rechargeable batteries. The sol-gel route endows lower processing temperature, lesser synthesis time, high purity, better homogeneity, good control of particle size and surface morphology. Physical characterizations of the synthesized powder were carried out using thermo-gravimetric and differential thermal analysis (TG/DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The electrochemical behaviour of the calcined samples has been carried out by galvanostatic charge/discharge cycling studies in the voltage range 3-5 V. The XRD patterns reveal crystalline single-phase spinel product. SEM photographs indicate micron sized particles with good agglomeration. The charge-discharge studies show LiCo0.25Ni0.25Mn1.5O4 synthesized using oxalic acid to be as a promising cathode material as compared to other two chelating agents and delivers average discharge capacity of 110 mA h g(-1) with low capacity fade of 0.2 mA h g(-1) per cycle over the investigated 15 cycles.