Glycine-assisted sol-gel-synthesized multiple-doped spinels, LiMn0.25Ni0.25Mn1.5O4 (M = Cr, Fe, and Co) have been studied as 5 V cathode materials. The sol-gel technique provides homogencity, high purity, lower processing temperature, controlled particle size. and morphology. The synthesized samples were subjected to physical characterization studies. viz., thermogravimetric and differential thermal analysis. X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and electrochemical charge-discharge studies. Galvanostatic charge-discharge studies of the samples reveal that LiFe0.25Ni0.25Mn1.5O4 using glycine as a chelating agent delivers a stable capacity of 120 mAh g(-1) even after 20 cycles when cycled between 3 and 5 V. (C) 2009 The Electrochemical Society.