In order to obtain dense PbNb2O6-based piezoelectric ceramics with a single orthorhombic ferroelectric phase, Ba, and excess Ti were doped into PbNb2O6 ceramics with the composition of Pb0.92Ba0.08Nb2O6–0.25 wt% TiO2 via a conventional solid-state reaction method. The ceramics were sintered at 1210°–1300°C. The effects of sintering temperature on the crystallite structure, microstructure, and dielectric and piezoelectric properties were studied in detail. All ceramics had shown a high relative density (>94%) and a single orthorhombic phase. The lattice parameters, grain size, and shape varied with changing sintering temperature. All ceramics exhibited a typical characteristic in ferroelectrics with normal paraelectric–ferroelectric phase transition at the Curie temperature. With increasing sintering temperature from 1210° to 1300°C, the Curie temperature decreased from 554° to 523°C, while the maximum dielectric constant increased. The change in dielectric properties with changing sintering temperature is associated with a competing effect among internal stress, porosity, and grain size. The ceramic sintered at 1260°C possesses an excellent piezoelectric constant (d33=82 pC/N), low mechanical quality factor (Qm=20.52), low dielectric loss (tan δ=0.0062), and high Curie temperature (Tc=535°C), presenting a high potential to be used in high-temperature applications as piezoelectric transducers.

Microstructure, Dielectric, and Piezoelectric Properties of Pb0.92Ba0.08Nb2O6–0.25 wt% TiO2 Ceramics: Effect of Sintering Temperature

Ferroelectric orthorhombic lead metaniobate (PbNb2O6) is known to be metastable with respect to the thermodynamically stable nonferroelectric rhombohedral polymorph. The high-temperature tetragonal to low temperature rhombohedral phase transition is reconstructive and thereby sluggish; ferroelectric PbNb2O6 is obtained by quenching from the stable phase field of the tetragonal polymorph. We report on the stabilization of the ferroelectric tungsten bronze polymorphs of PbNb2O6 by minor chemical substitution in the series [(1 - x) PbNb2O6-xBiTiNbO(6)], [(1 - x)PbNb2O6-xNa(0.5)Bi(0.5)Nb(2)O(6)], [(1 - x)PbNb2O6-xK(0.5)Bi(0.5)Nb(2)O(6)], and [(1 - x)PbNb2O6-xCaTiO(3)]. The high- temperature tungsten bronze polymorph is entropy stabilized with respect to the stable rhombohedral polymorph, and we propose that the tungsten bronze is further entropy stabilized by chemical substitution, reducing the transition temperature of the rhombohedral polymorph and further disfavoring the kinetics of the undesired phase transition. Optimized solid-state synthesis and processing to obtain dense ceramics were developed for the solid solutions, and the dielectric, ferroelectric, and piezoelectric properties of the PbNb2O6 solid solutions are reported. Curie temperature is suppressed with chemical substitution in all the systems. Lattice cell parameters display systematic variation with composition, reducing the molar volume, and the lattice parameter ratio 2b/a with increasing degree of substitution, reflecting a suppression of the polarization along the (010) direction due to chemical substitution. The piezoelectric properties improved with increasing substitution level probably due to the ease of poling of the materials with lower T-c. However, some improvements seen with 2% CaTiO3 were not accompanied by T-c decrease.

Solid Solutions of Lead Metaniobate—Stabilization of the Ferroelectric Polymorph and the Effect on the Lattice Parameters, Dielectric, Ferroelectric, and Piezoelectric Properties

Microstructure and dielectric properties of Pb0.94La0.06Nb2O6 ceramics

A high piezoelectric transition temperature is indicated for present orthorhombic samples of lead meta-niobate (PbNb2O6) by the high value of the temperature (Tm) at which the real part (ϵ′) of electrical permittivity peaks. It is 573 to 580°C. The imaginary component (ϵ″) increases sharply at these temperatures. Cooling run after heating to 700°C gives changed values of ϵ′ and ϵ″ and Tm. Present work reports impedance spectroscopy (up to 700°C over 20 Hz to 5.5 MHz) and Differential Scanning Calorimetry or DSC on the pure orthorhombic phase, and, for the first time, on the pure rhombohedral phase. DSC shows an endothermic dip across Tm during heating and an exothermic peak during cooling for the orthorhombic sample only.

Dielectric and Thermal Investigations on PbNb2O6 in Pure Piezoelectric Phase and Pure Non-Piezoelectric Phase

Environment-friendly lead-free perovskites have gained immense interest in the scientific community now a days. Here, we report the synthesis of PbNb2O6 using the sol-gel auto-combustion method, where Pb is substituted with Ca, which reduced its toxicity and improved its energy storage capacity. XRD analysis confirmed the formation of a rhombohedral phase for parent composition which transformed to the orthorhombic phase when Pb is completely replaced by Ca. Depending on the relative concentrations of Pb and Ca, the intermediate compositions exhibited dual phases. The crystallite size of all the compositions is in the range of 26–53 nm. Platelet-like morphology, besides particle agglomeration, has been observed for Ca-free composition. However, as the Ca concentration increased, a rod-like morphology appeared with a significant reduction in particle size. The presence of all elements according to their stoichiometric compositions is confirmed by energy dispersive X-ray spectroscopy. The presence of all downward peaks in the FTIR spectra in the range of 400–1000 cm−1 are associated with the stretching and bending of Nb–O bonds, except for one peak which appeared at 432.13 cm−1 and originates from the Pb–O bond. Dielectric analysis revealed that Ca substitution improved the dielectric constant of PbNb2O6 over wide frequency range. Even a frequency of 1 MHz, the value of dielectric constant is remarkably high with a small value of tangent loss. These properties demonstrate the potential of Pb-free perovskites for energy storage applications. 

Tuning the dielectric properties of PbNb2O6 perovskite through calcium substitution

The effect of microstructure on dielectric and piezoelectric properties of PbNb2O6 was studied to examine the possibility of using powder with the low-temperature rhombohedral form for the preparation of piezoelectric PbNb2O6 ceramics. Dense, fine-grained PbNb2O6 ceramics with good piezoelectric property with the maximum kt value of 0.315 were obtained by rapid heating and isothermal soaking at 1250°C of powders with particle size between 0.7 and 1.0 μm. The use of coarse powder resulted in the development of large grains and pores caused by exaggerated grain growth induced by phase transformation from the low- to high-temperature forms. Isothermal soaking at 1300°C resulted in the formation of a duplex structure. These structural defects reduced the piezoelectric property.

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低温相粉体を用いた緻密な圧電性 PbNb2O6 の作製

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低温相粉体を用いた緻密な圧電性 PbNb2O6 の作製

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低温相粉体を用いた緻密な圧電性 PbNb2O6 の作製

李鎬誠