Spinel LiMn2O4 andLiCr(x)Mn(2-x)O(4) (x = 0.00-0.20) have been synthesized by a soft chemistry method using adipic acid as the chelating agent. This technique offers better homogeneity, preferred surface morphology, reduced heat-treatment conditions, sub-micron sized particles, and better crystallinity. The synthesized spinet materials are characterized by X-ray diffraction, scanning electron microscopy, cyclic voltammetry, and charge-discharge testing. It is found that chromium substitution alleviates capacity fading in the 4-V region and improves the structural stability of LiMn2O4 spinet upon repeated cycling. (C) 2004 Published by Elsevier B.V.