Sol-gel assisted spinel LiCrxNiyMn2-x-yO4 (0 < x < 0.4 and 0 < y < 0.4) has been synthesized. The thermal study of the precursor was carried out by thermogravimetric and differential thermal analyses. Furthermore, the material has been subjected to X-ray diffraction, scanning electron microscopy, Fourier transform IR spectroscopy analysis, X-ray photoelectron spectroscopy, cyclic voltammetry studies, and electrochemical charge-discharge studies. The X-ray diffraction of LiCrxNiyMn2-x-yO4 matches well with the Joint Committee on Powder Diffraction Standard card no. 35-782, confirming the formation of a single-phase spinel. Charge-discharge studies were carried out between 3 and 5 V to understand the electrochemical behavior of the undoped and doped spinels. LiCr0.25Ni0.25Mn1.5O4 calcined at 850 degrees C possesses a particle size of around 70 nm and exhibits an initial discharge capacity of 105 mAh g(-1) stabilizing at 98 mAh g(-1) over the investigated 20 cycles. However, maleic acid derived LiCr0.25Ni0.25Mn1.5O4 delivers a stable higher discharge capacity of similar to 115 mAh g(-1) over the investigated 20 cycles and is a promising 5 V cathode material.