Low temperature fabrication and impedance spectroscopy of PMN-PT ceramics

Single phase perovskite 0.9Pb(Mg1/3Nb2/3)O-3-0.1(PbTiO3) ceramics were prepared using the columbite precursor method after optimizing the synthesis conditions. X-ray diffraction (XRD) studies were carried out to verify the phase formation at each processing step. Scanning electron microscopy (SEM) was employed to observe the microstructure of the sintered ceramics. Impedance and modulus spectroscopic data were used to gain an insight into the electrical properties of the samples and with a view to observing the relaxations in them. (C) 1999 Elsevier Science Ltd.

Microstructural, dielectric, pyroelectric and ferroelectric studies on partially grain-oriented SrBi2Ta2O9 ceramics

Partially grain-oriented (48%) ceramics of strontium bismuth tantalate (SrBi2Ta2O9) have been fabricated via conventional sintering. The grain-orientation factor of the ceramics was determined, as a function of both the sintering temperature and duration of sintering using X-ray powder diffraction (XRD) techniques. Variations in microstructural features (from acircular to plate like morphology) as a function of sintering temperature of the pellets were monitored by Scanning Electron Microscopy (SEM). The dielectric constant and loss measurements as functions of both frequency and temperature have been carried out along the directions parallel and perpendicular to the pressing axis. The anisotropy (epsilon(rn)/epsilon(rp)) associated was found to be 2.21. The effective dielectric constant of the samples with varying porosity was predicted using different dielectric mixture formulae. The grain boundary and grain interior contributions to the dielectric properties were rationalized using the impedance spectroscopy. The pyroelectric coefficient for strontium bismuth tantalate ceramic was determined along the parallel and perpendicular directions to the pressing axis and found to be -23 muC/m(2)K and -71 muC/m(2)K, respectively at 300 K. The ferroelectric properties of these partially grain-oriented ceramics are superior in the direction perpendicular to the pressing axis to that in the parallel direction.

Characterization of lithium borate–bismuth tungstate glasses and glass-ceramics by impedance spectroscopy

Transparent glasses in the system (1−x)Li2B4O7–xBi2WO6 (0≤x≤0.35) were prepared via melt quenching technique. Differential thermal analysis was employed to characterize the as-quenched glasses. Glass-ceramics with high optical transparency were obtained by controlled heat-treatment of the glasses at 720 K for 6 h. The amorphous nature of the as-quenched glass and crystallinity of glass-ceramics were confirmed by X-ray powder diffraction studies. High resolution transmission electron microscopy (HRTEM) shows the presence of nearly spherical nanocrystallites of Bi2WO6 in Li2B4O7 glass matrix. Capacitance and dielectric loss measurements were carried out as a function of temperature (300–870 K) in the frequency range 100 Hz–40 MHz. Impedance spectroscopy employed to rationalize the electrical behavior of glasses and glass-ceramics suggest the coexistence of electronic and ionic conduction in these materials. The thermal activation energies for the electronic conduction and ionic conduction were also estimated based on the Arrhenius plots.

Structural and dielectric properties of Bi2NbxVi−xO5.5 ceramics

Bi2Nbx V1−xO5.5 ceramics with x ranging from 0.01 to 0.5 have been prepared. The crystal system transforms from an orthorhombic to tetragonal at x 3= 0.1 and it persists until x = 0.5. Scanning electron microscopic (SEM) investigations carried out on thermally etched Bi2NbxV1−xO5.5 ceramics confirm that the grain size decreases markedly (18 μm to 4 μm) with increasing x. The shift in the Curie temperature (725 K) toward lower temperatures, with increasing x, is established by Differential Scanning Calorimetry (DSC). The dielectric constants as well as the loss tangent (tan δ) decrease with increasing x at room temperature.

Transmission electron microscopy study of domain structures in ferroelectric SrBi2Nb2O9 ceramics

A transmission electron microscopy study has been carried out on the domain structures of SrBi2Nb2O9 (SBN) ferroelectric ceramics which belong to the Aurivillius family of bismuth layered perovskite oxides. SBN is a potential candidate for Ferroelectric Random access memory (FeRAM) applications. The 90° ferroelectric domains and antiphase boundaries (APBs) were identified with dark field imaging techniques using different superlattice reflections which arise as a consequence of octahedral rotations and cationic shifts. The 90° domain walls are irregular in shape without any faceting. The antiphase boundaries are less dense compared to that of SrBi2Ta2O9(SBT). The electron microscopy observations are correlated with the polarization fatigue nature of the ceramic where the domain structures possibly play a key role in the fatigue- free behavior of the Aurivillius family of ferroelectric oxides.

Physical chemistry of mixed conducting zirconia ceramics

Suivant la pression partielle d'oxygène, la zircone peut être conducteur ionique ou électronique. Mise au point de méthodes de mesures de f.é.m. permettant de s'affranchir des sources d'erreur introduites par ces propriétés.

Relaxor behavior of K0.5La0.5Bi2Nb2O9 ceramics

K0.5La0.5Bi2Nb2O9, a relaxor, was synthesized and the structural studies confirmed it to be an n = 2 member of the Aurivillius oxides. The ½{h00} and ½{hk0} types of superlattice reflections in the electron diffraction patterns reflected the presence of ordered polar regions. A broad dielectric peak with frequency dependent dielectric maximum temperature was observed. The dielectric relaxation obeyed the Vogel-Fulcher relation wherein Ea = 0.04 eV, Tf = 428 K,and ωo = 1010 Hz. The diffuseness parameter γ = 2.003 established the relaxor nature and it was attributed to the A-site cationic disorder. The piezoelectric d31 coefficient was 0.5 pC/N at 300 K and 2 pC/N at 480 K.

Ferro electriclike and pyroelectric behavior of CaCu3Ti4O12 ceramics

A ferroelectriclike hysteresis loop was obtained at room temperature for CaCu3Ti4O12 (CCTO) ceramic. The remnant polarization and coercive field for 1100 °C/5 h sintered CaCu3Ti4O12 ceramics were 0.063 μC/cm2 and 195 V/cm, respectively. Remnant polarization increased while the coercive field decreased with increase in sintering temperature/duration, implying that these were microstructural dependent. The observation of the hysteresis loop for CCTO ceramic was corroborated by its pyroelectric behavior, and the pyroelectric current at room temperature was −0.0028 nA. These findings were attributed to the presence of mixed-valent Ti ions, apart from off center displacement of Ti ions in TiO6 octahedra.

Relaxor characteristics of layered Ba1-(3/2)xLaxBi2Nb2O9 ceramics

Barium lanthanum bismuth niobate Ba1−(3/2)xLaxBi2Nb2O9 (x = 0, 0.05, 0.1, and 0.15) powders have been prepared via solid state reaction route. The monophasic layered perovskite nature of each composition of these was confirmed by x-ray diffraction studies. A continuous decrease in the lattice parameter c of parent BaBi2Nb2O9 with increase in La3+ doping level was noteworthy. A decrease in dielectric constant maximum (εm), a shift in dielectric anomaly to lower temperatures (from 488 to 382 K), and an increase in the diffuseness (γ) (from 1.58 to 1.84) of dielectric anomaly were encountered on increasing x from 0 to 0.15. Vogel-Fulcher analyses showed a decrease in freezing temperature (Tf) (from 157 to 40 K) and an increase in the activation energy (0.53 to 1.12 eV) for frequency dispersion with increase in La3+ content. A downward shift in the peak position of the pyroelectric coefficient with increasing La3+ doping level was observed. The observed changes in the above physical properties were attributed to the increase in A-site chemical heterogeneity as a result of aliovalent La3+ doping on Ba2+ sites and associated A-site vacancy formation.

Improved microwave dielectric properties of (Mg1-(x+y)CaxLay)(Ti1-yAly)O3 ceramics

Phase-singular solids of the composition, (Mg1−(x+y) Cax Lay)(Ti1−yAly)O3 (x = 0 to 0.88; y = 0.05 to 0.35) having the cubic perovskite-type structure were prepared by the substitution of La3+ and Al3+ in equivalent quantities which brought about complete miscibility between MgTiO3 and CaTiO3. These ceramics showed relative permittivities of 16.5 to 50 (at 6 GHz) with increasing Ca content, high Q values of 10 000 to 30 000 and retained near-zero temperature coefficients in permittivity at optimum y values. Their dielectric characteristics are better accountable in terms of the positional disorder rather than the tolerance factor of perovskite structure.

Effect of calcium stoichiometry on the dielectric response of CaCu3Ti4O12 ceramics

CaxCu3Ti4O12 (x=0.90, 0.97, 1.0, 1.1 and 1.15) polycrystalline powders with variation in calcium content were prepared via the oxalate precursor route. The structural, morphological and dielectric properties of the ceramics fabricated using these powders were studied using X-ray diffraction, scanning electron microscope along with energy dispersive X-ray analysis, transmission electron microscopy, electron spin resonance (ESR) spectroscopy and impedance analyzer. The X-ray diffraction patterns obtained for the x = 0.97, 1.0 and 1.1 powdered ceramics could be indexed to a body-centered cubic perovskite related structure associated with the space group Im3. The ESR studies confirmed the absence of oxygen vacancies in the ceramics that were prepared using the oxalate precursor route. The dielectric properties of these suggest that the calcium deficient sample (x = 0.97) has a reduced dielectric loss while retaining the high dielectric constant which is of significant industrial relevance. (C) 2012 Elsevier Ltd. All rights reserved.