Preparation and characterization of Pb(Zr_0.52Ti_0.48)O₃ ceramics from high-energy ball milling powders

Ultra-fine Pb(Zr_0.52Ti_0.48)O₃ powder has been synthesized from the commercial PbO, TiO₂ and ZrO₂ powders using the high-energy ball milling technique in air at room temperature without any post-annealing. The synthesized powders milling for different hours are characterized using XRD, SEM, TEM and Raman spectra. XRD patterns and Raman spectra show that the perovskite phase of PZT can be formed from the mixture of the starting materials after milling for 20 h. The grain sizes of the powders have been estimated from the XRD patterns and TEM images to be approximately ~ 10 nm. The relationship between the microstructure of the PZT powders and the milling hours has been discussed. The PZT ceramics are derived for the synthesized powders by sintering the green pellets at 1100 °C for 1 h. The dielectric properties of the PZT samples are comparable with those of the same composition PZT prepared by other methods, but the high-energy ball milling process is much easier than other reported methods. The high-energy ball milling method offers a very attractive advantage of avoiding the loss of volatile elements, such as Pb, Bi, in the procedure of synthesis of nano-powders with their uniform compositions.