Effect of different ethylene glycol (ethylene glycol, polyethylene glycol-400 and polyethylene glycol-4000) precursors on the Pechini process for the synthesis of nano-crystalline LiNi0.5Co0.5VO4 powders was investigated. The structural coordination of as-prepared and calcined polymeric intermediates was investigated by FTIR analysis. Thermal behavior of the polymeric intermediates was studied by DSC thermograms. Effect of different ethylene glycols on the microstructure of polymeric intermediates was identified by SEM analysis. The inverse spinel phase of the obtained LiNi0.5Co0.5VO4 powders was confirmed by comparing the X-ray diffraction spectra with JCPDS data and the crystallite size was calculated using XRD data and Scherrer's formula. The lowest crystallite size was found to be 49 mu for the calcined polymeric intermediate, at 450degreesC for 12 h, prepared with ethylene glycol (EG). (C) 2004 Published by Elsevier B.V.