Olivine-type lithium iron phosphate (LiFePO4) powders were synthesized applying three different methods: solid state reaction at high temperature, ultrasonic spray pyrolysis, and sonochemical treatment. The samples were characterized by X-ray powder diffraction (XRPD). Particle morphologies of the obtained powders were determined by scanning electron microscopy (SEM). It was found that structural and microstructural parameters of this material were strongly dependent on the synthesis conditions. We present here the results obtained upon optimization of each procedure for designing this cathode material.