Site of incorporation and solubility for Fe ions in acceptor-doped PZT ceramics

Pb ( Zr 0.54 Ti 0.46 ) O 3 ceramic samples with composition near the morphotropic phase boundary have been investigated. Samples have been nominally doped with 0.5 and 1.0 mol % Fe atoms and studied by electron paramagnetic resonance (EPR), transmission electron microscopy (TEM), and Mössbauer spectroscopy. EPR and Mössbauer measurements indicated the creation of Fe–O vacancy dipoles in the grains and a solubility limit of less than 1 mol % for the Fe atoms in the PZT lattice. TEM studies revealed a dense sample with homogeneous microstructure and a second crystalline phase at the triple pockets with Pb excess. In the case of the 1 mol % Fe:PZT sample, beside the components Pb, Zr, and Ti even Fe was determined in these pockets with higher concentration as in the grains.