Spinel LiMn2O4 particles with fine sizes and regular morphologies were successfully synthesized by ultrasonic spray pyrolysis at the severe preparation conditions from a spray solution with citric acid and ethylene glycol. The as-prepared particles with spherical shapes, porous structures and micron sizes turned into LiMn2O4 particles with submicron size and narrow size distribution at the post-treatment temperature of 800 degrees C. The discharge capacities of the particles prepared from the spray solution with citric acid and ethylene glycol changed from 90 to 127 mAh/g when the post-treatment temperature was changed from 700 to 1 1000 degrees C. The LiMn2O4 particles had maximum discharge capacities at the post-treatment temperature of 800 degrees C. The discharge capacity of the LiMn2O4 particles dropped from 127 to 108 mAh/g by the 30th cycle.