Abstract Lithium iron phosphate LiFePO 4 (LFP) is one of the promising new cathode materials for next generation lithium secondary batteries. Various synthesis strategies have been proposed to create LiFePO 4 particles with maximum efficiency. The spray pyrolysis is a suitable synthesis technique which allows to direct the particle formation in multiple ways. LiFePO 4 has successfully been synthesized by ultrasonic and nozzle spray pyrolysis. The obtained products were characterized by means of XRD and SEM analysis. Furthermore, the mechanism of the particle formation was investigated.