Two types of LiMn₂O₄ particles were synthesized from metallic nitrates and acetates by ultrasonic spray pyrolysis. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis revealed that the starting precursor solution influenced the particle morphology, i.e., the nitrate precursor solution led to the formation of porous particles, and the acetate led to the formation of hollow particles. No differences in crystal phase or crystallinity between the two types of LiMn₂O₄s were detected by X-ray diffraction (XRD) analysis. It was found that the morphology and microstructure of the particles were important factors in determining their electrochemical properties.