Phase evolution studies of sol–gel derived lead zirconate titanate (PZT) nanopowder using X-ray diffraction and X-ray photoelectron spectroscopy

Abstract

We report here the formation of single phase lead zirconate titanate (PZT) nanopowder with composition Pb(Zr0.52Ti0.48)O3 and average crystallite size 12–20 nm, synthesized by sol–gel process. The phase evolution of PZT gel powder, heat treated at temperatures 550, 650 and 800°C was monitored by X-ray diffraction (XRD) and X-ray photo-electron spectroscopy (XPS). The high resolution XPS spectra of Pb4f, Zr3d, Ti2p and O1s show that PZT with pure perovskite structure is obtained at 800°C while at lower temperatures pyrochlore phase co-exists with perovskite phase. The XRD results also support this analysis. We have also identified the pyrochlore phase using XPS by analyzing the corresponding variations in the FWHM values, peak positions and the separation between the spin doublets of Pb, Zr and Ti associated with it. The composition of the final powder obtained with pure perovskite structure is calculated and is close to the designed value.