Potential of vibro-milling technique for preparation of electroceramic nanopowders

The potential of the vibro-milling technique as a simple method to obtain usable quantities of single-phase electroceramic powders with nanosized particles was examined. A detailed study considering the role of both milling time and firing condition on phase formation and particle size of the final product was performed. The calcination temperature for the formation of the desired phase was lower when longer milling times have been applied. More importantly, by employing an appropriate choice of the milling time and calcination condition, high purity electroceramic nanopowders have been successfully prepared with a simple solid-state reaction method.     

Phase Formation and Magnetic Properties of Bismuth Ferrite–Lead Titanate Multiferroic Composites

In this study, phase formation and the magnetic properties of bismuth ferrite–lead titanate multiferroic composites were investigated. Multiferroic composites consisting of antiferromagnetic bismuth ferrite (BiFeO₃ or BF) and ferroelectric lead titanate (PbTiO₃ or PT) were synthesized by the solid-state sintering method. The presence of pure phase in these composites was confirmed by X-ray diffraction (XRD). The microstructure and magnetic properties were investigated by means of a scanning electron microscope (SEM) and vibrating sample magnetometer (VSM), respectively. Structural transformation from rhombohedral in pure BF to mixed-phase between rhombohedral and tetragonal when added with 50 wt% PT has been revealed from XRD analysis. The magnetic properties are generally seen to reduce with an increase in the content of the PT phase. Interestingly, the M–H hysteresis loop measurements indicated that the composites exhibited superparamagnetic behavior at room temperature for all compositions, a noticeable contradiction to the magnetic behavior earlier reported for the BF–PT solid–solution.     

Indirect Measurement of Energy Density of Soft PZT Ceramic Utilizing Mechanical Stress

This paper reports on an indirect measurement of energy density of soft PZT ceramic utilizing mechanical stress. The method works analogous to the Olsen cycle and allows for a large amount of electro-mechanical energy conversion. A maximum energy density of 350 kJ/m³/cycle was found under 0–312 MPa and 1–20 kV/cm of applied mechanical stress and electric field, respectively. The obtained result is substantially higher than the results reported in previous studies of PZT materials utilizing a direct piezoelectric effect.     

MPB Phase Transition and Microstructure of (1 – x)PMN–xPZT Activated by 0.05BZN Ceramics

The relaxor ferroelectric materials can be found in morphotropic phase boundary (MPB) existing between tetragonal and cubic phase. Since the MPB shifts to other phases by adding ceramics composition. [(1 – x)Pb(Mg_1/3 Nb_2/3)O₃–x Pb(Zr_0.52Ti_0.48)O₃] were doped by 0.05Ba(Zn_1/3 Nb_2/3)O₃ when x = 0.4, 0.3, and 0.2 ceramics, which prepared by using a two–step sintering process. The MPB transitions were studied by the use of XRD. The samples, at x = 0.4, were in MPB and then gradually shifted to cubic phase at x = 0.2. The microstructure of samples fracture found that the largest grain size of 4.51 μm for x = 0.2. This study using TEM technique which demonstrated a crystalline morphology with the largest crystal size about 1.293 μm at x = 0.3. These results also revealed that not only the ferroelectric phase shifted to relaxor behavior with decreasing PZT contents in PMN–PZT system but also activated by BZN, which led to the presence of the relaxor behavior.     

Piezoelectric properties of low temperature sintering in Pb(Zr,Ti)O3–Pb(Zn,Ni)1/3Nb2/3O3 ceramics for piezoelectric transformer applications

In this study, in order to develop low-temperature sintering ceramics for a multilayer piezoelectric transformer application, we explored CuO and Bi₂O₃ as sintering aids at low temperature (900 °C) sintering condition for Sb, Li and Mn-substituted 0.8Pb(Zr_0.48Ti_0.52)O₃–0.16Pb(Zn_1/3Nb_2/3)O₃–0.04Pb(Ni_1/3Nb_2/3)O₃ ceramics. These substituted ceramics have excellent piezoelectric and dielectric properties such as d₃₃  347 pC/N, k_p  0.57 and Q_m  1469 when sintered at 1200 °C. The addition of CuO decreased the sintering temperature through the formation of a liquid phase. However, the piezoelectric properties of the CuO-added ceramics sintered below 900 °C were lower than the desired values. The additional Bi₂O₃ resulted in a significant improvement in the piezoelectric properties. The composition Sb, Li and Mn-substituted 0.8Pb(Zr_0.48Ti_0.52)O₃–0.16Pb(Zn_1/3Nb_2/3)O₃–0.04Pb(Ni_1/3Nb_2/3)O₃ + 0.5 wt% CuO + 0.5 wt% Bi₂O₃ showed the value of k_p = 0.56, Q_m = 1042 (planar mode), d₃₃ = 350 pC/N, when it was sintered at 900 °C for 2 h. These values indicated that the newly developed composition might be suitable for multilayer piezoelectric transformer application.     

Phase formation,electrical properties and morphotropic phase boundary of 0.95Pb(ZrxTi1−x)O3–0.05Pb(Mn1/3Nb2/3)O3 ceramics

Ferroelectric ceramics in specific composition of 0.95Pb(Zr_xTi_1?x)O₃–0.05Pb(Mn_1/3Nb_2/3)O₃ or PZT–PMnN (with x=0.46, 0.48, 0.50, 0.52, and 0.54) have been investigated in order to identify the morphotropic phase boundary (MPB) composition. The effects of Zr/Ti ratio on phase formation, dielectric and ferroelectric properties of the specimens have also been investigated and discussed. X-ray diffraction patterns indicate that the MPB of the tetragonal and rhombohedral phase lies in x=0.52. The crystal structure of PZT–PMnN appeared to change gradually from tetragonal to rhombohedral phase with increasing Zr content. The dielectric and ferroelectric properties measurements also show a maximum value (ε_r, tan δ and P_r) at Zr/Ti=52/48, while the transition temperature decreases with increasing Zr content.     

Influence of calcination conditions on phase formation and particle size of indium niobate powders synthesized by the solid-state reaction

A wolframite-type phase of indium niobate, InNbO₄, has been synthesized by a solid-state reaction via a rapid vibro-milling technique. The formation of the InNbO₄ phase in the calcined powders has been investigated as a function of calcination conditions by TG-DTA and XRD techniques. Morphology, particle size and chemical composition have been determined via a combination of SEM and EDX techniques. Single-phase InNbO₄ powders have been obtained successfully for calcination condition of 900 °C for 4 h or 950 °C for 2 h with heating/cooling rates of 30 °C/min. Higher temperatures and longer dwell times clearly favoured particle growth and the formation of large and hard agglomerates.     

Processing and properties of Pb(Mg1/3Nb2/3)O3–PbTiO3-based ceramics

Ceramic compositions of a combination between lead magnesium niobate, Pb(Mg_1/3Nb_2/3)O₃, and lead titanate, PbTiO₃, were fabricated using the Mg₄Nb₂O₉ precursor technique. Their electrical properties with respect to temperature and frequency were examined and the effect of sintering conditions on phase formation, densification, microstructure and electrical properties of the ceramics were examined. It has been found that optimisation of sintering conditions can lead to a highly dense and pyrochlore-free PMN–PT ceramics. The gradual decrease of the physical properties of the sintered ceramics was related to the gradual decrease of density and inhomogeneous microstructure. The results also revealed that for the lower concentration of lead titanate, a relaxor behaviour is noticed with a high electrostrictive effect, which was almost hysteretic free. However, higher amount of lead titanate led to a normal ferroelectric behaviour.     

The fabrication of lead titanate ceramics by a two-stage sintering technique

In this work, a two-stage sintering technique, which began with an initial heating at lower temperature and followed by higher temperature sintering, was employed in the production of PbTiO₃ ceramics. Effects of designed sintering conditions on phase formation, densification, microstructure and dielectric properties of the ceramics were characterized via X-ray diffraction (XRD), Archimedes method, scanning electron microscopy (SEM) and dielectric measurement, respectively. The potentiality of a two-stage sintering technique as a low-cost and simple ceramic fabrication to obtain highly dense and pure lead titanate ceramics was demonstrated. It has been found that, under suitable conditions, the perovskite phase of densified PT ceramics with reasonable dielectric properties may be achieved with equivalent to those obtained from a single-stage sintering technique.     

Stress-dependent ferroelectric properties of Pb(Zr1/2Ti1/2)O3–Pb(Zn1/3Nb2/3)O3 ceramic systems

Effects of compressive stress on the ferroelectric properties of ceramics in PZT–PZN systems were investigated. (1 − x)Pb(Zr_1/2Ti_1/2)O₃(xPb(Zn_1/3Nb_2/3)O₃ or (1 − x)PZT–(x)PZN (x = 0.1–0.5) ceramics were prepared by a conventional mixed-oxide method. The ferroelectric properties under compressive stress of the PZT–PZN ceramics were observed at stress levels up to 170 MPa using a compressometer in conjunction with a modified Sawyer–Tower circuit. It was found that with increasing compressive stress the area of the ferroelectric hysteresis (P–E) loops, the saturation polarization (P_sat), the remanent polarization (P_r), and the coercive field (E_c) decreased. These results were interpreted through the non-180° ferroelectric domain switching processes.