Microstructure and electric properties of Pr-doped Pb(Zr0.52Ti0.48)O3 ceramics

Improving the piezoelectric activity of lead zirconate titanate (PZT) ceramics is of great importance for practical applications. In this study, the influence of Pr³⁺ doping on the ferroelectric phase composition, microstructure, and electric properties on the A-site of (Pb_1-1.5xPr_x)(Zr_0.52Ti_0.48)O₃ is extensively investigated. A dense and fine microstructural sample is obtained with the introduction of Pr³⁺. The results show that the morphotropic phase boundary (MPB) moves to the rhombohedral phase region. The rhombohedral and tetragonal phases exhibit an ideal coexistence in the 4 mol.% Pr³⁺ doped (PPZT4) samples. Lead vacancy and the reduction of the potential energy barrier are considered to be the key mechanisms for donor doping, which is upheld by the Pr³⁺ doping. Combining the I-E hysteresis loops with the P-E hysteresis loops, it becomes apparent that both contribution maximums of the domain switching and residual polarisation are in PPZT4. Moreover, the thermal aging resistance of PZT is improved by doping, and the temperature stability is optimised from 83% in PZT to 96% in PPZT4. Hence, an appropriate amount of Pr³⁺ doping can effectively improve the piezoelectric activity of PZT ceramics in the MPB area and optimise the performance stability of the material under application temperatures.     

Thermal treatment effect on the magnetoelectric properties of (Ni0.5Zn0.5)Fe2O4/Pt/Pb(Zr0.3Ti0.7)O3 heterostructured thin films

Magnetoelectric (ME) property modulation in heterostructured (Ni_0.5Zn_0.5)Fe₂O₄/Pt/Pb(Zr_0.3Ti_0.7)O₃ (NZFO/Pt/PZT) thin films on platinized Si substrate by thermal annealing condition variation was studied. In an attempt to prevent interfacial reaction between NZFO and PZT layers during high temperature annealing, thin Pt layer was deposited which can serve as inter-diffusion barrier as well as electrode. The ferroelectric, magnetic, and ME properties of the heterostructured film were noticeably modulated due to microstructural evolution and clamping relaxation developed during thermal annealing process. Room temperature ME voltage coefficient of the heterostructured thin films was enhanced with increasing annealing temperature and reached to 29 mV/cm·Oe when annealed at 650 °C.     

Crystal structure,polarization properties and reverse nonlinearity of solid solutions of the KNN-PZT system in a wide range of external influences

Experimental research of the crystal structure, polarization properties, and reverse nonlinearity of ceramic solid solutions of the (1-x) (Na_0·5K_0.5)NbO₃-xPb(Ti_0·5Zr_0.5)O₃ (KNN-PZT) quasi-binary system with 0.0 = x ≤ 1.0 in a wide range of external influences (temperatures, strength of dc/ac fields) has been done. Based on the X-ray structural data, an x-T diagram of the system has been constructed, and correlations of the behavior of the macroproperties of solid solutions with the features of their phase states with the temperature change have been established. It has been concluded that it is advisable to use the proposed compositions when designing microelectronic devices operating in various extreme conditions.     

PZT components derived from polysulphone spinning process

The present paper deals with the development of lead zirconate titanate (PZT) fibres, pearls and fibre fragments, for their use as active phase in piezocomposites. As new a approach, the green ceramic components are shaped by polysulphone spinning, allowing for effective and flexible forming over a wide range of different geometries and sizes. The correlation between processing parameters, e.g. the slurry composition, nozzle size and operation velocity, and the resultant shape of ceramic components is analysed. Sintered piezoceramic parts show a dense microstructure. Performance data are evaluated on PZT/epoxy composites. Measurement results of strain, polarisation and piezoelectric coupling are given and discussed. The developed PZT components are seen as key for the creation of smart and lightweight structural components. Further, free formed PZT components open new design approaches for sensing and actuating devices and ultrasound transducers.     

High piezoelectric sensitivity and hydrostatic figures of merit in unidirectional porous ferroelectric ceramics fabricated by freeze casting

High performance lead zirconate titanate (PZT) ceramics with aligned porosity for sensing applications were fabricated by an ice-templating method. To demonstrate the enhanced properties of these materials and their potential for sensor and hydrophone applications, the piezoelectric voltage constants (g₃₃ and g₃₁), hydrostatic parameters (d_h, g_h, ?d₃₃/d₃₁, d_h·g_h and d_h·g_h/tanδ) and AC conductivity as a function of the porosity in directions both parallel and perpendicular to the freezing temperature gradient were studied. As the porosity level was increased, PZT poled parallel to the freezing direction exhibited the highest d_h, ?d₃₃/d₃₁ and figures of merit d_h·g_h, d_h·g_h/tanδ compared to the dense and PZT poled perpendicular to the freezing direction. The g_h, g₃₃ and g₃₁ coefficients were highest for the PZT poled perpendicular to the freezing direction; the g_h was 150%–850% times higher than dense PZT, and was attributed to the high piezoelectric activity and reduced permittivity in this orientation. This work demonstrates that piezoelectric ceramics produced with aligned pores by freeze casting are a promising candidate for a range of sensor applications and the polarisation orientation relative to the freezing direction can be used to tailor the microstructure and optimise sensitivity for sensor and hydrostatic transducer applications.     

Innovative method to produce large-area freestanding functional ceramic foils

Using thick and thin films instead of bulk functional materials presents tremendous advantages in the field of flexible electronics and component miniaturization. Here, a low-cost method to grow and release large-area, microscale thickness, freestanding, functional, ceramic foils is reported. It uses evaporation of sodium chloride to silicon wafer substrates as sacrificial layers, upon which functional lead titanate zirconate ceramic films are grown at 710?°C maximum temperature to validate the method. The freestanding, functional foils are then released by dissolution of the sacrificial sodium chloride in water and have the potential to be integrated into low-thermal stability printed circuits and flexible substrates. The optimization of the sodium chloride layer surface quality and bonding strength with the underlying wafer is achieved thanks to pre-annealing treatment.     

Direct processing of PbZr0.53Ti0.47O3 films on glass and polymeric substrates

This work reports on direct crystallization of PbZr_0.53Ti_0.47O₃ (PZT) thin films on glass and polymeric substrates, using pulsed thermal processing (PTP). Specifically, xenon flash lamps deliver pulses of high intensity, short duration, broadband light to the surface of a chemical solution deposited thin film, resulting in the crystallization of the film. Structural analysis by X-ray diffraction (XRD) and transmission electron microscopy show the existence of perovskite structure in nano-sized grains (≤5 nm). Local functional analysis by band excitation piezoelectric spectroscopy and electrostatic force microscopy confirm the presence of a ferroelectric phase and retention of voltage-written polarization for multiple days. Based on structural and functional analyses, strategies are discussed for optimization of pulse voltage and duration for the realization of crystalline ferroelectric thin films. For ∼200 nm-thick PZT films on glass substrates, 500 μs-long pulses were required for crystallization, starting with 100 pulses at 350 V, 10 or 25 pulses at 400 V and in general lower number of pulses at higher voltages (resulting in higher radiant energy). Overall power densities of >6.4 kW/cm² were needed for appearance of peaks corresponding to the perovskite phase in the XRD. Films on glass processed at 350–400 V had a higher degree of 111-oriented perovskite grains. Higher applied radiant energy (through increased pulse voltage or count) resulted in more random and/or partially 001-oriented films. For ∼1 μm-thick PZT films on polymeric substrates, 10 to 25 250 μs-long pulses at voltages ranging between 200 to 250 V, corresponding to power densities of ∼2.8 kW/cm², were optimal for maximized perovskite phase crystallization, while avoiding substrate damage.     

Ferroelastic domain switching and R-curve behavior in lead zirconate titanate (Zr/Ti = 52/48)-based ferroelectric ceramics

In this work, ferroelastic domain switching and R-curve behavior in lead zirconate titanate (Nb/Ce co-doped Pb(Zr_0.52Ti_0.48)O₃, ab. PZT-NC)-based ferroelectric ceramics were investigated, using the indentation-strength-in-bending (ISB) method. Firstly, Vickers indentation test examined the notable fracture anisotropy of PZT-NC ceramics between the poling direction and its perpendicular direction, and the crack open displacement (COD) profiles in the two directions were also theoretically calculated from the indentation fracture mechanics. And then two kinds of ferroelastic domain switching modes (in-plane and out-of-plane) were used for explaining such anisotropic propagation behavior of indentation cracks. The subsequent three-point bending test illustrated the dependence of fracture strength on indentation load and the rising crack growth resistance curves (R-curves) in two directions. The resulted R-curves were fitted by the Hill's type Growth Function successfully, giving the reasonable values of crack extension exponential (n), plateau fracture toughness (K_max), and initial fracture toughness (K_ini). The in-plane ferroelastic domain switching was identified as a more significant toughening mechanism for PZT-NC ceramics than the out-of-plane switching due to more switchable domains.     

High pressure EIGA preparation and 3D printing capability of Ti—6Al—4V powder

Ti—6Al—4V alloy powder was processed by electrode induction melting gas atomization (EIGA) at high gas pressure (5.5–7.0 MPa). The effects of atomizing gas pressure on the powder characteristics and the microstructure, along with the mechanical properties of the as-fabricated block by laser melting deposition (LMD), were investigated. The results indicate that the diameters of powders are distributed in a wide range of sizes from 1 to 400 μm, and the median powder size (d₅₀) decreases with increasing gas pressure. The powders with a size fraction of 100–150 μm obtained at gas pressures of 6.0 and 6.5 MPa have better flowability. The oxygen content is consistent with the change trend of gas pressure within a low range of 0.06%–0.20%. Specimens fabricated by LMD are mainly composed of α+β grains with a fine lamellar Widmanstatten structures and have the ultimate tensile strength (UTS) and yield strength of approximately 1100 and 1000 MPa, respectively. Furthermore, the atomized powders have a favorable 3D printing capability, and the mechanical properties of Ti—6Al—4V alloys manufactured by LMD typically exceed those of their cast or wrought counterparts.     

Microstructure and strengthening mechanism of Mg—5.88Zn—0.53Cu—0.16Zr alloy solidified under high pressure

Mg—5.88Zn—0.53Cu—0.16Zr (wt.%) alloy was solidified at 2—6 GPa using high-pressure solidification technology. The microstructure, strengthening mechanism and compressive properties at room temperature were studied using SEM and XRD. The results showed that the microstructure was refined and the secondary dendrite spacing changed from 35 μm at atmospheric pressure to 10 μm at 6 GPa gradually. Also, Mg(Zn,Cu)₂ and MgZnCu eutectic phases were distributed in the shape of network, while under high pressures the second phases (Mg(Zn,Cu)₂ and Mg₇Zn₃) were mainly granular or strip-like. The solid solubility of Zn and Cu in the matrix built up over increasing solidification pressure and reached 4.12% and 0.32% respectively at 6 GPa. The hardness value was HV 90 and the maximum compression resistance was 430 MPa. Therefore, the grain refinement strengthening, the second phase strengthening and the solid solution strengthening are the principal strengthening mechanisms.