Dielectric and impedance properties of Nd3/2Bi3/2Fe5O12 ceramics

The polycrystalline sample of Nd3/2Bi3/2Fe5O12 was prepared by a high- temperature solid-state reaction technique. Preliminary X-ray structural analysis exhibits the formation of a single-phase tetragonal structure at room temperature. Microstructural analysis by scanning electron microscopy shows that the sintered sample has well defined grains. These grains are distributed uniformly throughout the surface of the sample. Detailed studies of dielectric response at various frequencies and temperatures exhibit a dielectric anomaly at 400 A degrees C. The electrical properties (impedance, modulus and conductivity) of the material were studied using a complex impedance spectroscopy technique. These studies reveal a significant contribution of grain and grain boundary effects in the material. The frequency dependent plots of modulus and the impedance loss show that the conductivity relaxation is of non-Debye type. Studies of electrical conductivity with temperature demonstrate that the compound exhibits Arrhenius-type of electrical conductivity. Study of ac conductivity with frequency suggests that the material obeys Jonscher's universal power law.

Structural and dielectric properties of relaxor Sr0.5Ba0.5Bi2Nb2O9 ceramic

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermally stimulated crystallization glass system of (20-x)LiO2-80TeO(2)-xWO(3)

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e caracterização de pós Ba(x)Sr(1-x)Co0,8Fe0,2O3- através do método de coprecipitação via oxalato

Ceramic powders based on oxides of perovskite-type structure is of fundamental interest nowadays, since they have important ionic-electronic conductivity in the use of materials with technological applications such as gas sensors, oxygen permeation membranes, catalysts and electrolytes for solid oxide fuel cells (SOFC). The main objective of the project is to develop nanostructured ceramic compounds quaternary-based oxide Barium (Br), Strontium (Sr), Cobalt (Co) and Iron (Fe). In this project were synthesized compounds BaxSr(1-x)Co0, 8Fe0,2O3- (x = 0.2, 0.5 and 0.8) through the oxalate co-precipitation method. The synthesized powders were characterized by thermogravimetric analysis and differential thermal analysis (TGADTA), X-ray diffraction (XRD) with the Rietveld refinement using the software MAUD and scanning electron microscopy (SEM). The results showed that the synthesis technique used was suitable for production of nanostructured ceramic solid solutions. The powders obtained had a crystalline phase with perovskite-type structure. The TGA-DTA results showed that the homogeneous phase of interest was obtained temperature above 1034°C. It was also observed that the heating rate of the calcination process did not affect the elimination of impurities present in the ceramic powder. The variation in the addition of barium dopant promoted changes in the average crystallite size in the nanometer range, the composition being BSCF(5582) obtained the lowest value (179.0nm). The results obtained by oxalate co-precipitation method were compared with those synthesis methods in solid state and EDTA-citrate method

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d

Espectros fractais em sistemas nanoestruturados e cristais fotônicos

The study of the elementary excitations such as photons, phonons, plasmons, polaritons, polarons, excitons and magnons, in crystalline solids and nanostructures systems are nowdays important active field for research works in solid state physics as well as in statistical physics. With this aim in mind, this work has two distinct parts. In the first one, we investigate the propagation of excitons polaritons in nanostructured periodic and quasiperiodic multilayers, from the description of the behavior for bulk and surface modes in their individual constituents. Through analytical, as well as computational numerical calculation, we obtain the spectra for both surface and bulk exciton-polaritons modes in the superstructures. Besides, we investigate also how the quasiperiodicity modifies the band structure related to the periodic case, stressing their amazing self-similar behavior leaving to their fractal/multifractal aspects. Afterwards, we present our results related to the so-called photonic crystals, the eletromagnetic analogue of the electronic crystalline structure. We consider periodic and quasiperiodic structures, in which one of their component presents a negative refractive index. This unusual optic characteristic is obtained when the electric permissivity and the magnetic permeability µ are both negatives for the same range of angular frequency ω of the incident wave. The given curves show how the transmission of the photon waves is modified, with a striking self-similar profile. Moreover, we analyze the modification of the usual Planck´s thermal spectrum when we use a quasiperiodic fotonic superlattice as a filter.

NMR and conductivity study of the protonic conductor HPb2Nb3O10 center dot nH(2)O

Electrical conductivity and H-1 Nuclear Magnetic Resonance (NMR) techniques were used to investigate the ion-exchanged layered lead-niobate perovskite HPb2Nb3O10. nH(2)O, over the temperature range 90-350 K. Compounds were synthesized by the sol-gel method and calcinated at 650 degreesC. Analysis of the NMR data gives activation energies for the proton motion in the range 0.14-0.40 eV, which are dependent on the water content. The frequency and temperature dependencies of the proton spin-lattice relaxation times show that the character of the motion of the: water molecules is essentially two-dimensional, reflecting the layered structure of the material. The H-1 line-narrowing transition and the single spin-lattice relaxation rate maximum, observed in the hydrated compounds, are consistent with a Grotthuss-like mechanism for the proton diffusion. (C) 2000 Elsevier B.V. B.V. All rights reserved.

Evaluation of solid and submerged fermentations for the production of cyclodextrin glycosyltransferase by Paenibacillus campinasensis H69-3 and characterization of crude enzyme

Cyclodextrin glycosyltransferase (CGTase) is an enzyme that produces cyclodextrins from starch by an intramolecular transglycosylation reaction. Cyclodextrins have been shown to have a number of applications in the food, cosmetic, pharmaceutical, and chemical industries. In the current study, the production of CGTase by Paenibacillus campinasensis strain H69-3 was examined in submerged and solid-state fermentations. P. campinasensis strain H69-3 was isolated from the soil, which grows at 45 C, and is a Gram-variable bacterium. Different substrate sources such as wheat bran, soybean bran, soybean extract, cassava solid residue, cassava starch, corn starch, and other combinations were used in the enzyme production. CGTase activity was highest in submerged fermentations with the greatest production observed at 48-72 h. The physical and chemical properties of CGTase were determined from the crude enzyme produced from submerged fermentations. The optimum temperature was found to be 70-75 degrees C, and the activity was stable at 55 degrees C for 1 h. The enzyme displayed two optimum pH values, 5.5 and 9.0 and was found to be stable between a pH of 4.5 and 11.0.

Hydrothermal syntheses of ETS-10 like vanadosilicates using chiral organic molecules. Part I

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Micromorphology and spectroscopic characteristics of organic matter in waterlogged podzols of the upper Amazon basin

In waterlogged environments of the upper Amazon basin, organic matter is a major driver in the podzolisation of clay-depleted laterites, especially through its ability to weather clay minerals and chelate metals. Its structure in eight organic-rich samples collected at the margin and in the centre of the podzolic area of a soil sequence was investigated. The samples illustrate the main steps in the development of waterlogged podzols and belong either to eluviated topsoil A horizons or to illuviated subsoil Bhs, Bh and 2BCs horizons. Organic matter micromorphology was described, and the overall molecular structure of their clay size fractions was assessed using Fourier transform infrared (FTIR) spectroscopy and cross polarization/magic angle spinning (CP/MAS) C-13 nuclear magnetic resonance (NMR). Organic features of the horizons strongly vary both vertically and laterally in the sequence. Topsoil A horizons are dominated by organic residues juxtaposed to clean sands with a major aliphatic contribution. In the subsoil, numerous coatings, characteristic of illuviation processes, are observed in the following horizons: (i) At the margin and bottom parts of the podzolic area, dark brown organic compounds of low aromacity with abundant oxygen-containing groups accumulate in Bhs and 2BCs horizons. Their spectroscopic features agree with the observation of cracked coatings in 2BCs and the presence of organometallic complexes, whose abundance decreases towards low lying positions. (ii) By contrast, black organic compounds of high aromacity with few chelating functions accumulate as coatings and infills in the overlying sandy Bh horizon of well-expressed waterlogged podzols. (c) 2008 Elsevier B.V. All rights reserved.

SrZrO3 powders obtained by chemical method: Synthesis, characterization and optical absorption behaviour

Strontium zirconate (SrZrO3) powders have been synthesized by the polymeric precursor method after heat treatment at different temperatures for 2 h in oxygen atmosphere. The decomposition of precursor powder was followed by thermogravimetric analysis, X-ray diffraction (XRD) and Fourier transform Raman (FT-Raman). The UV-vis absorption spectroscopy measurements suggested the presence of intermediary energy levels in the band gap of structurally disordered powders. XRD, Rietveld refinement and FT-Raman revealed that the powders are free of secondary phases and crystallizes in the orthorhombic structure. (C) 2007 Elsevier Masson SAS. All rights reserved.

Dielectric properties of Ca(Zr0.05Ti0.95)O-3 thin films prepared by chemical solution deposition

Ca(Zr0.05Ti0.95)O-3 (CZT) thin films were grown on Pt(1 1 1)/Ti/SiO2/Si(1 0 0) substrates by the soft chemical method. The films were deposited from spin-coating technique and annealed at 928 K for 4 h under oxygen atmosphere. CZT films present orthorhombic structure with a crack free and granular microstructure. Atomic force microscopy and field-emission scanning electron microscopy showed that CZT present grains with about 47 nm and thickness about 450 nm. Dielectric constant and dielectric loss of the films was approximately 210 at 100 kHz and 0.032 at 1 MHz. The Au/CZT/Pt capacitor shows a hysteresis loop with remnant polarization of 2.5 mu C/cm(2), and coercive field of 18 kV/cm, at an applied voltage of 6 V. The leakage current density was about 4.6 x 10(-8) A/cm(2) at 3 V. Dielectric constant-voltage curve is located at zero bias field suggesting the absence of internal electric fields. (c) 2006 Elsevier B.V. All rights reserved.

Synthesis and characterization of CaBi4Ti4O15 thin films annealed by microwave and conventional furnaces

CaBi4Ti4O15 thin films were deposited by the polymeric precursor method and crystallized in a domestic microwave oven and conventional furnace. The films obtained for microwave energy are well-adhered, homogeneous and with good specularity, when treated at 700 degrees C for 10 min. The microstructure and the structure of the films can be tuned by adjusting the crystallization conditions. When microwave oven is employed, the films presented bigger grains with mean grain size around 80 nm. For comparison, films were also prepared by the conventional furnace at 700 degrees C for 2 h. (C) 2007 Elsevier Masson SAS. All rights reserved.

Barium strontium titanate powders prepared by spray pyrolysis

Ultasonic spray pyrolysis (SP) has been investigated for the production of the barium strontium titanate (BST) powders from the polymeric precursors. The processing parameters, such as flux of aerosol and temperature profile inside the furnace, were optimized to obtain single phase BST. The powders were characterized by the methods of X-ray diffraction analysis, SEM, EDS and TEM. The obtained powders were submicronic, consisting of spherical, polycrystalline particles, with internal nanocrystalline structure. Crystallite size of 10 nut, calculated using Rietveld refinement, is in a good agreement with results of HRTEM. (c) 2005 Elsevier B.V. All rights reserved.

Ferroelectric and dielectric properties of Ba0.5Sr0.5(Ti0.80Sn0.20)O-3 thin films grown by the soft chemical method

Polycrystalline Ba0.5Sr0.5(Ti0.80Sn0.20)O-3 (BST:Sn) thin films with a perovskite structure were prepared by the soft chemical method on a platinum-coated silicon substrate from spin-coating technique. The resulting thin films showed a dense structure with uniform grain size distribution. The dielectric constant of the films estimated from C-V curve is around 1134 and can be ascribed to a reduction in the oxygen vacancy concentration. The ferroelectric nature of the film indicated by butterfly-shaped C-V curves and confirmed by the hysteresis curve, showed remnant polarization of 14 mu C/cm(2) and coercive field of 74 kV/cm at frequency of 1 MHz. At the same frequency, the leakage current density at 1.0 V is equal to 1.5 x 10(-7) A/cm(2). This work clearly reveals the highly promising potential of BST:Sn for application in memory devices. (c) 2006 Elsevier B.V. All rights reserved.