335 resultados para DENSIFICATION
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Ultra-fine powders of Na1-xLixNbO3 (x=0; 0.06; 0.09; 0.12) were synthesized by the Polymeric Precursors Method. Such powders had their orthorhombic structures determined by X-ray diffraction and their surface area determined by BET isotherms (less than 10 m(2) g(-1)). Densification was followed by dilatometric study. The powders, calcined at 700 degrees C for 5 h, were sintered at 1290 degrees C during 2 h under ambient atmosphere with no application of extra pressure. The samples with relative densities higher than 95% were analyzed by impedance spectroscopy at room temperature, under a signal amplitude of 1 V-rms. Dielectric constants of about 180 and dielectric loss factor of about 0.03 were measured showing small dependence with frequency. The electrical properties were similar to those obtained for samples sintered by hot pressing. (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.
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To obtain SnO2 films to be used for surface protection of fluoride glasses, a non-aqueous sol-gel route for the preparation was developed. An ethanolic SnO2 colloidal suspension was prepared by thermohydrolysis of SnCl4 solution at 70 degreesC. By using this procedure, redispersable powders with nanometer sized particles were obtained. Films were obtained by dip coating on glass and mica substrates. The structures of the ethanolic precursor suspension and films were compared to those of similar samples prepared by the classical aqueous sol-gel route. Comparative analyses performed by photon correlation spectroscopy demonstrated that the powders obtained by freeze-drying are fully redispersable either in aqueous or in alcoholic solutions at pH greater than or equal to 8. As prepared sols and redispersed colloidal suspensions have hydrodynamic radius distribution (2-14 nm) with an average size close to 7 nm. The variations in film structures with firing temperature were investigated by small-angle X-ray scattering and X-ray reflectometry. The experimental results show that the films have a two level porous structure composed of agglomerates of primary colloidal particles. The sintering of the primary particles leads to the densification of agglomerates and to the formation of inter-agglomerate spatially correlated pores. The volume fraction of intra-agglomerate pores is reduced from approximate to 50% to approximate to 30% by the precipitation of precursor salts partially hydrolyzed in ethanolic solution. (C) 2001 Elsevier B.V. B.V. All rights reserved.
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Small angle X-ray scattering measurements, bulk and skeleton density data and an in-situ study by dilatometric thermal analysis about the nanoporosity elimination above 800 degreesC in TEOS sonogels are presented. Apparently, two processes act during the nanoporosity elimination, which precedes the foaming phenomenon often observed in such systems. The first, with an activation energy of (3.9 +/- 0.4) x 10(2) kJ/mol and high frequency factor, is the controlling process of the most nanoporosity elimination at higher temperature. The value of this activation energy is compatible to that for viscous flux throughout densification process in typical silica-based materials. The second, with an activation energy of (49 +/- 5) kJ/mol and low frequency factor, seems to be the controlling process of the first and extremely slow nanoporosity elimination at low temperature.
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70SiO(2)-30HfO(2) planar waveguides, doped with Er(3+) concentrations ranging from 0.3 to 1 mol %, were prepared by sol-gel route, using dip-coating deposition on silica glass substrates. The waveguides show high densification degree, effective intermingling of the two components of the film, and uniform surface morphology. Propagation losses of about 1 dB/cm were measured at 632.8 nm. When pumped with 987 or 514.5 nm continuous-wave laser light, the waveguides show the (4)I(13/2)-->(4)I(15/2) emission band with a bandwidth of 48 nm. The spectral features are found independent both on erbium content and excitation wavelength. The (4)I(13/2) level decay curves presented a single-exponential profile, with a lifetime between 2.9 and 5.0 ms, depending on the erbium concentration. (C) 2002 American Institute of Physics.
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The structure of silica-polypropyleneglycol (PPG) nanocomposites with weak physical bonds between the organic (PPG) and inorganic (silica) phase, prepared by the sol-gel process, was investigated by small angle X-ray scattering (SAXS). These nanocomposite materials are transparent, flexible, have good chemical stability and exhibit high ionic conductivity when doped with lithium salt. Their structure was studied as a function of silica weight fraction x (0.06 less than or equal to x less than or equal to 0.29) and [O]/[Li] ratio (oxygens being of ether-type). The shape of the experimental SAXS curves agrees with that expected for scattering intensity produced by fractal aggregates sized between 30 and 90 Angstrom. This result suggests that the structure of the studied hybrids consists of silica fractal aggregates embedded in a matrix of PPG. The correlation length of the fractal aggregates decreases and the fractal dimension increases for increasing silica content. The variations in structural parameters for increasing Li+ doping indicate that lithium ions favor the growth of fractal silica aggregates without modifying their internal structure and promote the densification of the oligomeric PPG matrix.
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Ta2O5 doped SnO2 varistor systems containing 0.5 mol% ZnO and 0.5 mol% Coo were prepared by mixed oxide method. Considering that ZnO and Coo oxides are densification additives only the SnO(2)center dot ZnO center dot CoO ceramics cannot exhibit electrical nonlinearity. A small amount of Ta2O5 improves the nonlinear properties of the samples greatly. The height and width of the defect barriers were calculated. It was found that samples doped with 0.05 mol% Ta2O5 exhibit the highest density (98.5%), the lowest electric breakdown field (E-b = 1100 V/cm) and the highest coefficient of nonlinearity (alpha = 11.5). The effect of Ta2O5 dopant could be explained by the substitution of Ta5+ by Sn4+. A grain-boundary defect barrier model for the SnO(2)center dot ZnO center dot CoO center dot Ta2O5 varistor system was also introduced. (c) 2004 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
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SnO2:m mol% CoO (0.5 less than or equal to m less than or equal to 6.0) ceramic specimens were studied by impedance spectroscopy in the 5 Hz-13 MHz frequency range during heating cold-pressed specimens from room temperature to 1250 degrees C. The electrical resistivity during sintering decreases from 4 to 6 orders of magnitude in the 400-1500 K temperature range depending on the amount of CoO. An increase in electrical resistivity in the 570-670 K range is related to the release of adsorbed water. The results for the 970-1500 K show that the higher the amount of the CoO addition, the lower is the temperature at which SnO2:CoO reaches a minimum electrical resistivity. This suggests that oxygen point defects created by dissolution of cobalt ions in the SnO2 lattice are controlling the densification rate of these ceramics.
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In the studied region, 35% of the soil collapses are related to leakage from sewage ducts. The paper describes the soils from this part of Brazil and a series of laboratory tests undertaken using water and domestic sewage fluid as the wetting agents. It is considered that the presence of soaps and detergents as recorded by the sodium concentration facilitates the densification of the soils and hence has a major effect on the surface settlement/collapse.
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The X-ray reflectivity technique was applied in the study of tin oxide films deposited by sol-gel dip-coating on borosilicate glasses. The influence of the withdrawal speed and temperature of thermal treatment on the film structure was analyzed. We have compared the thermal evolution of the density and the shrinkage of the films with these properties measured for the monolithic xerogel by helium picnometry and thermomechanical analysis. In agreement with the Landau-Levich model, the layer thickness increases by increasing the withdrawal speed. Nevertheless, it decreases with the increase of the thermal treatment temperature, due to the densification process. The values of apparent density are smaller than the skeletal density, which shows that the films are porous. The comparison between the film and the monolith indicates that shrinkage during firing is anisotropic, occurring essentially perpendicular to the coating surface.
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We compare the effect of organic (Tiron (R)) and inorganic (Mn(11)) additives on the low temperature (< 600 degrees C) densification of the sol-gel dip-coated SnO2 films. The structural and compositional properties of the samples were investigated by X-ray reflectometry (XRR), X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS). The results suggest that the replacement of hydroxyl groups at the particle surface by Tiron (R) reduces the level of agglomeration of the sol, increasing the particles packing and the apparent density of the coatings. Undoped and Mn-doped films drawn from a Tiron (R) containing suspension show after firing at 500 degrees C a porosity reduction of 12 and 8.6%, respectively. The porosity decrease is less pronounced (4.3%) for the film without additives. Both XAS and XPS data show the presence of trivalent manganese. The formation of a non-homogeneous solid solution characterised by the presence of Mn(111) replacing tin atom near to the crystallite surface was evidenced by XAS. Additionally, XPS results reveal the presence of metallic Sn at the surface of films containing Tirono. (c) 2005 Elsevier Ltd. All rights reserved.
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This work illustrates the advancement of research on TiO2-based electroceramics. In this work will be presented that the addition of different dopants, as well as thermal treatments at oxidizing and inert atmosphere, influences of the densification, the mean grain size and the electrical properties of the TiO2-based varistor ceramics. Dopants like Ta2O5, Nb2O5, and Cr2O3 have an especial role in the barrier formation at the grain boundary in the TiO2 varistors, increasing the nonlinear coefficient and decreasing the breakdown electric field. The influence of Cr'(Ti) is to increase the O' and O'(2) adsorption at the grain boundary interface and to promote a decrease in the conductivity by donating electrons to O-2 adsorbed at the grain boundary. In this paper, TiO2 and (Sn,Ti)O-2-based studies of polycrystalline ceramics, which show a non-linear I-V electrical response typical of low voltage varistor systems are also presented. All these systems are potentially promising for varistor applications. (C) 2004 Kluwer Academic Publishers.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Titanium alloy parts are ideally suited for advanced aerospace systems and surgical implants because of their unique combination of high specific strength at both room temperature and moderately elevated temperature, in addition to excellent corrosion resistance. In this work, results of the Ti-35Nb alloy sintering are presented. This alloy, due to its lower modulus of elasticity and high biocompatibility, is a promising candidate for surgical and aerospace applications. Samples were produced by mixing of initial metallic hydride powders followed by uniaxial and cold isostatic pressing with subsequent densification by isochronal sintering between 700 and 1500 degrees C, in vacuum. Sintering behavior was studied by means of microscopy and density. Sintered samples were characterized for phase composition, microstructure and microbardness by X-ray diffraction, scanning electron microscopy and Vickers indentation, respectively. Samples sintered at high temperatures display a fine plate-like a structure and intergranular P. A few remaining pores are still found, and density above 97% for specimens sintered at 1500 degrees C is reached. (c) 2007 Elsevier B.V. All rights reserved.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)