Characterization of Ferroelectric Ceramics Using XRD, TEM, and XPS

Abstract

Ferroelectric ceramic samples of PbTiO3, prepared by a modified oxide-mixing technique, were examined by x-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques for crystalline and microstructural characterization. XRD clearly revealed only a monophasic perovskite of tetragonal symmetry for the reference PbTiO3, whichwas established to possess both a–a- and a–c-type 90◦ domains. The inclination was approximately 2◦ between the two different domains, as observed by high-resolution TEM. Inductively coupled plasma (ICP) analysis, electron probe microanalysis (EPMA), and x-ray photoelectron spectroscopy (XPS) were employed and the ensuing chemical composition results are discussed. The approximate molar ratios of Pb:Ti were 1:1, 1:1.5, and 1:0.8 as obtained by ICP analysis, EPMA, and XPS, respectively. Corrections for the sensitivity factor (SCorr) for Pb 4f, Ti 2p and the substitution of the matrix factors for FTi,Pb, FPb,Ti have been taken into account in obtaining the Pb:Ti ratio of 1:1 by XPS quantification. The sensitivity factor (SKratos) given by the instrumental maker was compared with the theoretical one (STheo) and the result is also discussed.