LiMn2O4-based spinels are of great interest as positive electrode materials for lithium-ion batteries. The single-phase LiMn2O4 nanoparticles have been synthesized by a novel sol-gel thermolysis process using poly vinyl alcohol (PVA) with three different combustion fuels such as urea, hexamine and citric acid to know the effect on structure, particle size and electrochemical properties of LiMn2O4 nanoparticles. Among the three combinations. the polymeric gel precursor obtained by using PVA-urea has generate complete crystallization at lower temperature than other two combinations are confirmed by TG/DTA analysis. But all the three combinations generate phase pure LiMn2O4 nanoparticles are confirmed by XRD studies. The particle size and electrochemical properties are confirmed by TEM analysis and charge/discharge studies, respectively. It reveals that LiMn2O4 obtained by using PVA-urea has smaller nanoparticles and better electrochemical performance than the nanoparticles obtained by using other two combinations such as PVA-hexamine and PVA-citric acid. (c) 2006 Elsevier B.V. All rights reserved.