A new low-temperature synthetic route has been developed and demonstrated for the production of spinel LiMn2O4 as a cathode material for Li-ion batteries. The process involves the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. The material resulting from hydrothermal treatment is a spinel-structured Li0.92LiMn2O4 with reasonable crystallinity. It exhibits promising electrochemical behavior in nonaqueous liquid electrolyte. The influence of hydrothermal temperature and the effect of glucose in determining the final structural integrity and electrochemical performance have also been systemically explored. Furthermore, the capacity degradation of low-temperature synthesized spinels was studied by cyclic voltammetry and X-ray diffraction. This capacity fading can be mainly attributed to the factors of structural degradation and loss of active materials. (c) 2005 The Electrochemical Society.