Perovskite lead hafnate (PbHfO3, PH) nanoparticles that were free from halides and organics were synthesized via the oxidant peroxo method. Stoichiometric amounts of hafnium nitrate (HfO(NO3)(2)) and lead nitrate (PbHfO3) were dissolved in a diluted hydrogen peroxide (H2O2) aqueous solution, which was slowly added to a solution of H2O2 and ammonia (NH3) (pH 11). The lead-hafnium precipitate obtained was filtered and washed, to eliminate all nitrate ions. The precipitate was dried, ground, and calcined at temperatures of 400degrees-900degreesC. A tetragonal intermediate phase was identified using X-ray diffractometry and Raman spectroscopy during the calcination process, followed by the crystallization of the orthorhombic PH phase at similar to700degreesC.