Synthesis and characterization of pseudo-ternary Pb(Fe<Subscript>1/2</Subscript>Nb<Subscript>1/2</Subscript>)O<Subscript>3</Subscript>-PbZrO<Subscript>3</Subscript>-PbTiO<Subscript>3</Subscript> ferroelectric ceramics via a B-site oxide mixing route

Perovskite phase formation and dielectric/ferroelectric properties of the pseudo-ternary Pb(Fe_1/2Nb_1/2)O₃-PbZrO₃-PbTiO₃ (PFN-PZ-PT) ferroelectric ceramics have been investigated as promising materials for multi-layer ceramic capacitors. Complete solid solution with pure perovskite phase can be formed in this system in the whole composition range studied using conventional solid-state reaction method via a B-site oxide mixing route. Crystal lattice of the ceramics obtained shrinkages with the increase of the concentration of Pb(Fe_1/2Nb_1/2)O₃ (PFN) and expands with the increase of the content of PbZrO₃ (PZ). With the increase of the concentration of PbTiO₃ (PT), crystal structure of PFN-PZ-PT changes from pseudo-cubic ferroelectric phase to tetragonal one while retains the fraction of PFN as constant. A morphotropic phase boundary (MPB) forms at the composition of 42 mol% PT regardless of whatever concentration of PFN, and the content of PFN affects little on the composition of MPB. The preliminary phase diagram of the PFN-PZ-PT system is determined by X-ray diffraction (XRD) measurements combining with dielectric/ferroelectric characterization. Dielectric measurements indicate that the value of dielectric maximum (ɛ_m) and the temperature where ɛ_m appears (T_m) increase with the increase of the concentration of PT. However, PFN exhibits opposite effects, i.e., ɛ_m increases with the increase of the concentration of PFN accompanied by the decrease of T_m.     

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Structural and electrical properties of 0.56Pb(Ni1/3Nb2/3)O3-0.10Pb(Zn1/3Nb2/3)O3-0.34PbTiO3 ceramics prepared by different ceramic processings

The ternary system of 0.56Pb(Ni_1/3Nb_2/3)O₃-0.10Pb(Zn_1/3Nb_2/3)O₃-0.34PbTiO₃ (0.56PNN-0.10PZN-0.34PT) ceramics were prepared by conventional solid-state reaction method via straight mixed oxide method, columbite precursor method and B-site oxide mixing route. X-ray diffraction (XRD) measurement demonstrated that both the tetragonal and rhombohedral phases coexist in the B-site oxide mixing route prepared ceramics accompanied by the largest content of perovskite phase of 95.18%. The 0.56PNN-0.10PZN-0.34PT ceramics prepared by the straight mixed oxide method and the B-site oxide mixing route exhibit rather homogeneous microstructure. As a comparison, in the columbite precursor method prepared ceramics nebulous granules and octahedral or other polyhedral morphology grains are observed. All the sintered ceramics exhibit diffused ferroelectric phase transition where the dielectric response peaks are broad, diffused and strongly frequency dependent. However, the temperature of dielectric maximum (T_m) increases greatly from 398.0 K of the 0.56PNN-0.10PZN-0.34PT ceramics prepared by the B-site oxide mixing route to 423.3 K of the ones prepared by the straight mixed oxide method. Saturated and symmetric P-E hysteresis loops are observed in all the sintered ceramics, where the B-site oxide mixing route prepared ceramics exhibit large value of remanent polarization (P_r) of 17.13 μC/cm² and the least value of coercive field (E_c) of 11.99 kV/cm. Piezoelectric constant (d₃₃) exhibits the largest value of 449 pC/N for the ceramics prepared by the B-site oxide mixing route. Such results are related to the phase composition, density and porosity of the ceramics.     

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