705 resultados para sintering


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An experimental and theoretical study of the ferroelectric and piezoelectric behavior of PZT doped with barium is presented. Ab initio perturbed ion calculations was carried out. The properties, such as remnant polarization, coercive field and the coupling factor of the PZT at constant sintering temperature was compared with the Zr4+/Ti4+ ions dislocation energy and the lattice interaction energy. An agreement between the experimental and theoretical results, with a decrease of the interaction energy and an inversion of the energy stability from tetragonal to rhombohedral phase was observed. (C) 1999 Kluwer Academic Publishers.

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Strontium titanate (SrTiO3) thin films were prepared by dip-coating Si(111) single-crystal substrates in citrate solutions of ethylene glycol, considering several citric acid/ethylene glycol (CA/EG) ratios. Measurements of intrinsic viscosity indicate that increasing the amount of EG increases the precursors' polymeric chains and increases the weight loss. After deposition the substrates were dried on a hotplate (approximate to 150 degrees C); this was followed by heat treatment at temperatures ranging from 500 to 700 degrees C using heating and cooling rates of 1 degrees C min(-1). SEM and optical microscopy investigations of the sintered films obtained from different CA/EG ratios indicate that there is a critical thickness above which the films present cracks. This critical thickness for SrTiO3 films deposited on the Si(111) substrate is about 150 nm, Measurements of crack spacing as a function of film thickness indicate that the origin of cracks cannot be explained by the elastic behavior of the film but rather by the viscoelastic relaxation of the film during pyrolysis and sintering. Copyright (C) 1999 John Wiley & Sons, Ltd.

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Tin oxide, SnO2. is a very used compound in industry and one of its uses is as varistor. For the current requirements of the technology is necessary a strict control of the chemical purity and the particle size of the raw material; for that reason the great interest that exists at the moment to develop synthesis methods that allow to get these requirements. In this work, ceramic powders of the Sn-Co-Nb-Ti-Al system using the controlled precipitation and polymeric precursor (Pechini) methods were synthesized. The raw material obtained was characterized using X-ray diffraction (XRD), thermal analysis (DTA/FG) and scanning electron microscopy (SEM). The sintering samples shown a good varistor behavior with non-linear coefficient (alpha) values similar to 22, and Er 2083 V/cm(2). (c) 2007 Elsevier Ltd. All rights reserved.

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The structural evolution of aerogels prepared from TEOS sono-hydrolysis was studied as a function of the temperature of heat treatment up to 1100 degreesC by means of small angle X-ray scattering (SAXS) and density measurements. The mass fractal structure of the original wet sonogel (with scattering exponent alpha similar to 2.2) apparently transforms to a surface fractal structure in a length scale lesser than similar to1.5 nm, upon the process resulting in aerogel. Such a structural transformation is interpreted by the formation of new particles with characteristic dimension of similar to1.5 nm, with rough boundaries or electronic density fluctuations (or ultra-micropores) in their interior. The structural arrangement of these particles seem to preserve part of mass fractal characteristics of the original wet sonogel, now in a length scale greater than similar to1.5 nm. The electronic density heterogeneities in the particles start to be eliminated at around 800 degreesC and, at 900 degreesC, the particles become perfectly homogeneous, so the structure can be described as a porous structure with a porosity of similar to68% with similar to9.0 nm mean size pores and similar to4.3 nm mean size solid particles. Above 900 degreesC, a vigorous viscous flux sintering process sets in, eliminating most of the porosity and increasing rapidly the bulk density in an aerogel-glass transformation. (C) 2003 Elsevier B.V. All rights reserved.

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Bismuth titanate, Bi(4)Ti(3)O(12) (BIT) nanosized powders have been successfully synthesized via high energy mechanochemical activation. The phase formation of BIT, crystal structure, microstructure, crystallite size and specific surface area were followed by XRD, scanning electron microscopy (SEM) and the BET specific surface area measurements. The BIT milled 2 h shows the orthorhombic crystalline structure with small amount of amorphous phase. The microstructure of Bi(4)Ti(3)O(12) ceramics sintered at 1000 degrees C for 12h exhibit plate-like grain structure.

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In this work, the effect of the substrate microstructure on the formation of SnO2 membranes and of the sintering conditions on their porosity have been analysed. Samples have been prepared by colloidal suspensions cast on alumina or kaolin substrates. Supported membranes have been characterized by Hg porosimetry, MEV, XRD and N-2 adsorption-desorption isotherms. The results show that the narrower pore size distribution of alumina substrate allowed to prepare membranes more homogeneous and free of cracks than that supported on kaolin. The crystallite and pore sizes of the membranes could be controlled by adjusting the temperature of sintering, allowing materials with adequate microstructure with application for ultrafiltration process.

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The dielectric properties and loss of Bi1.5ZnSb1.5O7 a poor-semiconducting ceramic were investigated by impedance spectroscopy, in the frequency range from 5 Hz to 13 MHz. Electric measurements were performed from 100 to 700 degreesC. Pyrochlore type phase was synthesized by the polymeric precursor method. Dense ceramic with 97% of the theoretical density was prepared by sintering via constant heating rate. The dielectric permittivity dependence as a function of frequency and temperature showed a strong dispersion at frequency lower than 10 kHz. The losses (tan delta) exhibit slight dependence with the frequency at low temperatures presenting a strong increase at temperatures higher than 400 degreesC. A decrease of the loss magnitude occurs with increasing frequency. Relaxation times were extracted using the dielectric functions Z(omega) and M(omega). The plots of the relaxation times tau(Z'), and tau(M) as a function of temperature follow the Arrhenius law, where a single slope is observed with activation energy values equal to 1.38 and 1.37 eV, respectively. (C) 2003 Elsevier Ltd. All rights reserved.

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In this study, the effect of bismuth content on the crystal structure, morphology and electric properties of barium-bismuth-tantalate (BBT) ceramics was explored with the aid of X-ray diffraction (XRD), scanning electron microcopy (SEM), dielectric properties and ferroelectric hysteresis loops. BaBi2Ta2O9 (BBT) ceramics have been successfully prepared by the solid-state reaction. The BBT phase was crystallized at 900 degreesC for 2 h. The excess of bismuth controls the grain size, affecting the density of the material. Measurements of dieletric constant and dieletric losses confirm that the material is a ferroeletric with a Curie temperature around 77 degreesC. The dieletric constant measured at room temperature was 400, with a dielectric loss of 0.03. Both the phase-transition behaviour and ferroelectric properties, such as spontaneous polarization (P-s), showed a dependence on Bi content. (C) 2004 Elsevier B.V. All rights reserved.

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A nonisothermal study of the kinetics of the nanoporosity elimination in monolithic silica xerogels, prepared from acid and ultrasound catalyzed hydrolysis of tetraethylortosilicate (TEOS), has been carried out by means of in situ linear shrinkage measurements performed with different heating rates. The study could be applied up to almost alpha similar to 0.6 of the volume fraction alpha of eliminated pores. The activation energy was found increasing from about 3.2 x 10(2) kJ/mol for alpha similar to 0.06 up to about 4.4 x 10(2) kJ/mol for alpha. similar to 0.44. The sintering process accompanying the nanopore elimination in this set of xerogels is in agreement with a viscous flux sintering process with the hydroxyl content diminishing with the volume fraction of eliminated pores. All the volume fraction of eliminated pores versus temperature (T) curves can be matched onto a unique curve with an appropriate rescaling of the T axis, independent of the heating rate. This scaling property suggests that the path of sintering seems the same, regardless of the heating rate; the difference is that the rate is faster at higher temperature.

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Variations on the microstructure development and on the electrical properties of SnO2-based varistors are discussed on the basis of the oxygen vacancies created or annihilated by the presence of different additives. Electron paramagnetic resonance (EPR) analysis of sintered samples evidenced a substantial increase in the paramagnetic oxygen vacancies concentration when Nb2O5 is added to the SnO2 center dot Co3O4 system. on the other hand, the observed diminution in the concentration of such species after the addition of Fe2O3 indicates solid solution formation. The quantification of paramagnetic oxygen vacancies allowed to confirm the proposed substitutions taking place in the lattice during sintering. These findings are supported by scanning electron microscopy, by density measurements and by current density versus electric field curves. The characterization of secondary phases through EDS assisted SEM and TEM is also reported in this work.

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An investigation was made to discover how the addition of Cr2O3 affects the microstructural heterogeneity and nonohmic features of the SnO2(Co-x, Mn1-x)O-based varistor system, with x varying from 0 to 1. The presence of Cr2O3 was found to strongly increase the nonohmic features when x = 1. However, the nonohmic features of the system decrease when x drops from 1 to 0, a behavior explained by the increase of the junction heterogeneity within the system's microstructure. accompanied by ail excess of precipitates at the triple point in the grain boundary region due to modified MnO sintering. The presence of these precipitates causes the leakage current to increase in response to the creation of ail ineffective barrier. The effect produced by heat-treating these systems in oxygen- and nitrogen-rich atmospheres suggests that, according to mechanisms previously discussed in the literature, Cr2O3 is more susceptible to oxygen, so that increasing the amount of oxygen in the grain boundary region may improve the system's nonohmic properties. (c) 2005 Elsevier Ltd. All rights reserved.

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Zirconia-ceria powders with 12 mol % of CeO2 doped with 0.3 mol% of iron, copper, manganese and nickel oxides were synthesized by the conventional mixed oxide method. These systems were investigated with regard to the sinterability and electrical properties. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. Small amount of dopant such as iron reduces sintering temperature by over 150degreesC and more than 98% of tetragonal phase was retained at room temperature in samples sintered at 1450degreesC against 1600degreesC to stabilize the tetragonal phase on pure ZrO2-CeO2 system. The electrical conductivity was measured using impedance spectroscopy and the results were reported. The activation energy values calculated from the Arrhenius's plots in the temperature range of 350-700degreesC for intragrain conductivities are 1.04 eV.

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Pure and W-doped PZT ceramics (PZT and PZTW) were prepared by a hybrid process consisting in the association of polymeric precursor and partial oxalate methods. The phase formation was investigated by simultaneous thermal analysis (TG/DSC) and X-ray diffraction (XRD). The effect of W doping PZT and their electrical properties was evaluated. Substitution of W by Ti leads to an increase of Curie temperature and broadening of dielectric constant. A typical hysteresis loop was observed at room temperature and the remnant polarization was increased with the content of W. (c) 2007 Elsevier B.V. All rights reserved.

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Theoretical data using ab initio perturbed ion calculation were compared with ferroelectric and piezoelectric experimental data of strontium doped PZT. Various concentrations of SrO in PZT at constant temperature and sintering time were carried out. Experimental results, such as the remanent polarization, P-R of 6.9-8.9 muC/Cm-2, the coercive field, E-C of 6.6-7.8 kVcm, and the planar coupling factor, Kp of 0.45-0.53, were compared with the energy of Zr4+ and Ti4+ ion dislocation and the lattice interaction energy which show that strontium increment in PZT alter the energies and increase the values of piezoelectric and ferroelectric variables. Calculations of lattice energy of the rhombohedral phase show that a phase non-stability is coincident with increasing experimental values of the P-R, E-C and Kp. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

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PZT ceramics were obtained from the mechanochemically synthesized powders. Milling and sintering conditions were optimized based on results of density measurements, as well as on microstructural and electrical characterization. As a result, highly dense and homogeneous ceramics were obtained. Excellent microstructural properties resulted in good electrical properties. Samples showed values of dielectric constants reaching 12800 at the Curie temperature, as well as low dielectric loss under the optimal processing conditions. High values of remanent polarization, reaching 60 muC cm(-2), indicate high internal polarizability. (C) 2003 Kluwer Academic Publishers.