Synthesis and sintering of PZT ceramics

Lead zirconate powder, with Zr/Ti ratio of 50/50 was prepared by polymeric precursor method and doped with 3, 5 and 7 mol% of Sr+2 Or Ba+2, as well as by 0.2 to 5 mol% of Nb+5. The powder was calcined at 750 degrees C by 4 hours and milled during 1.5 h in isopropilic alcohol. Powders were characterized by surface area measurements (BET method), by infrared spectroscopy and by X-ray diffraction to characterize the crystal structure. Isostatically pressed samples were sintered in a dilatometer furnace by using a constant heating rate of 10 degrees C/min from ambient to 1200 degrees C. Synthetic air and air with water vapor were used as atmospheres. Both Sr+2 and Ba+2 substitute Pb+2 and favor the formation of rhombohedral phase. Otherwise, Nb+5 substitute preferentially Zr+4 favoring tetragonal phase. The concentration of dopants and the atmosphere influence the densification and the microstructure of the PZT, which alters the dielectric and piezoelectric properties of the ceramics.

Microstructure of organometallic derived PLZT ceramics

The PLZT powders with the formula Pb0.905La0.095(Zr0.65Ti0.35)(0.976)O-3+3.5 wt.% PbO were prepared by the organometallic precursor method (Pechini and partial oxalate processes). The microstructure of sintered 9.5/65/35 PLZT ceramics obtained from a partial oxalate procedure shows that the outstanding feature of this microstructure is its fairly uniform grains of about 1.8 mum. The microstructure of sintered PLZT ceramics obtained by the Pechini process consists of uniform small randomly- oriented grains tightly bonded together in the central part of the sample with,a grain size of about 1.2 mum. Cubic and elongated grains are formed at the sample's border. The microstructures of hot pressed PLZT ceramics obtained from both processes are dense and rather uniform. After a double stage of hot pressing (2 plus 20 h) the microstructure of PLZT is fully dense, uniform and homogeneous with a grain size of approximately 2.5 mum. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

AC impedance study of Ni, Fe, Cu, Mn doped ceria stabilized zirconia ceramics

Doped zirconia has been used in electronic applications in the cubic crystalline phase. Ceria-stabilized tetragonal zirconia presents high toughness and can also be applied as solid electrolytes. The tetragonal phase of zirconia can be stabilized at room temperature with ceria in a broad range of composition. However, CeO2-ZrO2 has low sinterability. so it is important to investigate the effect of sintering dopants. In this study the effect of iron, copper. manganese and nickel was investigated. The dopants such as iron and copper lowered the sintering temperature from 1600 degreesC down to 1450 degreesC, with a percentage of tetragonal phase retained at room temperature higher than 98% and also with an increase of the electrical conductivity. The electrical conductivity was measured using impedance spectroscopy. The grain boundary contribution was determined and the activation energy associated with the ionic conduction was 1.04 eV. The dopants can also promote a grain boundary cleanliness verified by blocking effect measurement. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Microstructural and electric properties of bismuth-layered structured ceramics - SrBi2(Ta1-xNbx)O-9

Ceramic samples of SrBi2(Nb1-xTax)O-9 (0 less than or equal to x less than or equal to 1) were prepared by the solid state reaction method in order to investigate their structural and electrical features as well as obtain useful information to improve the properties of SrBi2(Nb1-xTax)O-9 as a thin film. The X-ray diffraction patterns and the scanning electronic microscopy photomicrographs show no secondary phases but the formation of a solid-state solution for all the composition. The ac conductivity of the samples, measured at 25 degreesC and 100 kHz frequency, decreases with the increase of Ta content. Such results were explained by intrinsic conductivity of pure components.

Low-voltage varistor based on (Sn,Ti)O-2 ceramics

A description is given of the nonohmic behavior obtained in (SnxTi1-x)O-2-based systems. A matrix founded on (SnxTi1-x)O-2-based systems doped with Nb2O5 leads to a low-voltage varistor system with nonlinear coefficient values of similar to9. The presence of the back-to-back Schottky-type barrier is observed based on the voltage dependence of the capacitance. When doped with CoO, the (SnxTi1-x)O(2)(.)based system presents higher nonlinear coefficient values (>30) than does the SnO2-based varistor system.

Effect of processing route on the phase formation and properties of Bi4Ti3O12 ceramics

Our efforts were directed to the preparation of bismuth titanate-Bi4Ti3O12 (BIT) by two procedures: mechanically assisted synthesis and polymeric precursor method to display a variety of their advantages. To follow the nucleation and phase formation of BIT, XRD and Rietveld refinement analysis were used and it was shown that Bi4Ti3O12 ceramic can been successfully prepared from nano-sized powders obtained by both methods. The ferroelectric properties were determined and the loops from BIT obtained by polymeric precursor method were not fully saturated with a remnant polarization of 20 mu C/cm(2) and coercitive field of 1500 kV/cm. BIT obtained from powders prepared by mechanically assisted synthesis shows a remnant polarization of 0.65 mu C/cm(2) and coercitive field of 1050 kV/cm. The grain morphology may be the factor causing the observed differences. (C) 2005 Published by Elsevier Ltd and Techna Group S.r.l.

WO3 and ZnO-doped SnO2 ceramics as insulating material

SnO2 ceramics doped with ZnO and WO3 were prepared by mixed oxide method. The effect of ZnO and WO3 additives could be explained by the substitution of Sn4+ by Zn2+ and W6+. The addition of WO3 inhibits the grain growth due to the segregation of SnZnWO8 and ZnWO6 at the grain boundaries without strong influence on the densification process. The electrical characterization (log E x log J) shows that the ternary system SnO2-ZnO-WO3 exhibits a very high resistivity of around 10(14) Omega M. Independently of the WO3 concentration, the electrical conductivity of the Sn02-ZnO-WO3 system is always lower than that of the undoped tin dioxide. (C) 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Er3+ and Eu3+ containing transparent glass ceramics in the system PbGeO3-PbF2-CdF2

Glasses with composition 60PbGeO(3)-10PbF(2)-30CdF(2) (mol%) have been obtained in the bulk form with a high stability against crystallization. After doping them with 0.5 mol% of Er3+ or Eu3+ and appropriate heat treatment transparent glass ceramics could be obtained. Electronic spectroscopy, X-ray diffraction and transmission electron microscopy measurements have been made. beta-PbF2: Er3+/Eu3+ Single crystals, 5-10 nm in size, are detected in the otherwise transparent composite medium, the size of the particles and absence of clustering allowing for the increased transparency of the final materials. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Effects of powder preparation and sintering procedure on microstructure and dielectric properties of PLZT ceramics

PLZT ceramics belong to one of the very important groups of functional materials that make a basis for the production of a large range of electronic devices. The microstructure and properties of ceramics depend on the powder preparation and thermal processing conditions. Various techniques have been used to obtain chemically homogeneous and fine starting powders. PLZT powders have been prepared by two different production routes: by a modified Pechini method, using a polymeric precursor method (PMM) and by a partial oxalate method. A two-step sintering process, including a hot pressing, was carried out at 1100 and 1200degreesC Distinct phases obtained during the sintering process have been investigated by SEM and EDS techniques and dielectric properties such as permittivity and dielectric loss were measured in a frequency range from 1 to 20 kHz.. A significant difference in microstructure and dielectric properties, depending on powder origin and sintering procedure, has been noticed.

Hyperfine interaction measurements on ceramics: PZT revisited

The solid solution of PbZr1-xTixO3, known as lead-zirconate titanate (PZT), was probably one of the most studied ferroelectric materials, especially due to its excellent dielectric, ferroelectric and piezoelectric properties. The highest piezoelectric coefficients of the PZT are found near the morphotropic phase boundary (MPB) (0.46 <= x <= 0.49), between the tetragonal and rhombohedral regions of the composition-temperature phase diagram. Recently, a new monoclinic phase near the MPB was observed, which can be considered as a bridge between PZT's tetragonal and rhombohedral phases. This work is concerned with the study of the structural properties of the ferroelectric PZT (Zr/Ti = 52/48, 53/47) by hypertine interaction (HI) measurements obtained from experiments performed by using the nuclear spectroscopy time differential perturbed angular correlation (TDPAC) in a wide temperature range. (c) 2006 Elsevier B.V. All rights reserved.

Niobium doped Bi4Ti3O12 ceramics obtained by the polymeric precursor method

Pure and niobium doped bismuth titanate ceramics (Bi4Ti3-xNbxO12 (BTN)), with x ranging from 0 to 0.4 were prepared by the polymeric precursor method. X-ray diffraction showed no secondary phases. Increasing niobium content leads to more resistive ceramics. The shape and size of the grains are strongly influenced by the niobiurn added to the system. The dielectric constant is not influenced by the niobium addition while hysteresis loops are significantly narrowed. (c) 2006 Elsevier B.V All rights reserved.

Comparison of two bond strength testing methodologies for bilayered all-ceramics

Objectives. This study compared the shear bond strength (SBS) and microtensile (MTBS) testing methodologies for core and veneering ceramics in four types of all-ceramic systems.Methods. Four different ceramic veneer/core combinations, three of which were feldspathic and the other a fluor-apatite to their respectively corresponding cores, namely leucitereinforced ceramic ((IPS)Empress, Ivoclar), low leucite-reinforced ceramic (Finesse, Ceramco), glass-infiltrated alumina (In-Ceram Alumina, Vita) and lithium disilicate ((IPS)Empress 2, Ivoclar) were used for SBS and MTBS tests. Ceramic cores (N = 40, n = 10/group for SBS test method, N=5blocks/group for MTBS test method) were fabricated according to the manufacturers' instructions (for SBS: thickness, 3 mm; diameter, 5 mm and for MTBS: 10 mm x 10 mm x 2 mm) and ultrasonically cleaned. The veneering ceramics (thickness: 2 mm) were vibrated and condensed in stainless steel moulds and fired onto the core ceramic materials. After trying the specimens in the mould for minor adjustments, they were again ultrasonically cleaned and embedded in PMMA. The specimens were stored in distilled water at 37 degrees C for 1 week and bond strength tests were performed in universal testing machines (cross-head speed: 1mm/min). The bond strengths (MPa +/- S.D.) and modes of failures were recorded.Results. Significant difference between the two test methods and all-ceramic types were observed (P < 0.05) (2-way ANOVA, Tukey's test and Bonferroni). The mean SBS values for veneering ceramic to lithium disilicate was significantly higher (41 +/- 8 MPa) than those to low leucite (28 +/- 4 MPa), glass-infiltrated (26 +/- 4 MPa) and leucite-reinforced (23 +/- 3 MPa) ceramics, while the mean MTBS for low leucite ceramic was significantly higher (15 +/- 2 MPa) than those of leucite (12 +/- 2 MPa), glass-infiltrated (9 +/- 1 MPa) and lithium disilicate ceramic (9 +/- 1 MPa) (ANOVA, P < 0.05).Significance. Both the testing methodology and the differences in chemical compositions of the core and veneering ceramics influenced the bond strength between the core and veneering ceramic in bilayered all-ceramic systems. (c) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Use of impedance spectroscopy in the study of the effect of Cr concentration on the electrical properties of SnO2-based ceramics

This paper reports a study of influence of Cr concentration on the electrical properties and microstructure of SnO2-based powders doped with Mn and Nb, prepared by an organic route (Pechini method). All the samples were compacted into discs and sintered at 1300 degrees C for 3h, resulting in ceramics with relative density varying between 78% and 98%. The powders were characterized by X-ray diffraction analysis. Impedance spectroscopy characterization indicated that the conductivity decreases as Cr concentration increases, probably due to Cr segregation at grain boundaries, which reduces grain size, increasing the number of resistive boundaries.

Study of potassium additive on the phase formation and ferroelectric properties of 0.9PMN-0.1PT ceramics

A recent and innovative method to include Ti into the columbite precursor has permitted to synthesize 0.9PMN-0.1PT powders with high homogeneity. The present work describes this methodology, named modified columbite method, showing that the reaction between MN(T)and PbO at 800 degrees C for 2 h results in perovskite single-phase. The crystal structure alterations in the columbite and perovskite phases obtained by this methodology and the effects of potassium doping were investigated by the Rietveld method. Changes in the powder morphology, density and weight loss during the sintering process were also studied. Conclusively, potassium does not affect significantly the perovskite amount, but reduces the particle and grain sizes. This dopant also changes the relaxor behavior of 0.9PMN-0.1 PT ceramic, reducing the dielectric loss and enhancing the diffuseness of the phase transition. (C) 2005 Published by Elsevier Ltd and Techna Gronp S.r.l.