LiMn2O4 powders were synthesized by ultrasonic spray pyrolysis. By varying the cooling conditions. two samples of powders were obtained: quenched in water (Q) and spontaneously cooled to room temperature (SC). The crystal structure of the as-prepared powders was revealed by X-ray powder diffraction. Structure refinements confirm that SC sample crystallizes in Fd3m space group, while Q sample crystallizes in I4(1)/amd space group. Particle morphology was determined by scanning electron microscopy. Electrochemical intercalation and deintercalation were examined in galvanostatic regime.