Sinterização de filmes finos de LiNbO3 em forno microondas: estudo da influência da direção do fluxo de calor

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

Síntese e processamento de cerâmicas em forno de microondas doméstico

O uso de microondas no processamento e obtenção de materiais tem adquirido nos últimos anos crescente interesse por parte de diversas áreas do conhecimento como a química e a engenharia de materiais. Neste sentido, aparatos especialmente projetados têm começado a ser descritos na literatura como reatores e câmaras de processamento a microondas visando aplicação na pesquisa e na indústria. em particular o uso de fornos de microondas domésticos em atividades científicas tem se mostrado de interesse dado uma série de novas aplicações, simplicidade e baixo custo. O presente trabalho reporta um dispositivo desenvolvido a partir de um forno de microondas doméstico, capaz de efetuar sínteses e processamentos de sólidos mesmo quando os materiais envolvidos não possuem susceptibilidade as microondas. O novo dispositivo tem sido utilizado com sucesso na síntese de óxidos metálicos e, em especial na sinterização e ordenamento de redes cristalinas de filmes finos.

Influência do uso do forno de microondas ou convencional na síntese de ZrO2

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

BACTERIAL LEACHING OF URANIUM ORE FROM FIGUEIRA-PR, BRAZIL, AT LABORATORY AND PILOT-SCALE

A bacterial leaching program was carried out in order to evaluate the potential of applying this process to leach uranium from the ore of Figueira-PR, Brazil. The experiments were carried out in shake flasks, column percolation (laboratory and semipilot scale) and in heap leaching. In shake flasks and in column percolation experiments at laboratory scale, bacterial activity on the ore was confirmed: approximately 60% of uranium was leached, against around 30% in sterilized controls. Column percolation experiments at semipilot scale and heap leaching (850 tons of ore) showed uranium extractions of approximately 50%. In both experiments, a complementary sulfuric acid attack, after the bacterial leaching phase, was necessary to reach this level of uranium extraction.

Improvement of the ferroelectric properties of ABO(3) (A= Pb, Ca, Ba; B=Ti, Zr) films

High-quality ABO(3)/LaNiO3 (A = Ph, Ca, Ba; B = Ti, Zr) hetero structures have been grown on LaAlO3 (1 0 0) substrate by the chemical solution deposition method and crystallized by a microwave oven technique. The structural, morphological and electric properties were characterized by means of X-ray diffraction (XRD), atomic force microscope (AFM), and dielectric and ferroelectric measurements. XRD patterns revealed single-phase polycrystalline and oriented thin films whose feature depends on the composition of the films. The AFM surface morphologies showed a smooth and crack-free surface with the average grain size ranging from 116 to 300 nm for both LaNiO3 electrode and the ferroelectric films. Dielectric measurements on these samples revealed dielectric constants as high as 1800 at frequency of 100 KHz. Such results showed that the combination of the chemical solution method with the microwave process provides a promising technique to grow high-quality thin films with good dielectric and ferroelectric properties. (c) 2005 Elsevier Ltd. All rights reserved.

Barium strontium titanate nanocrystalline thin films prepared by soft chemical method

Barium strontium titanate (Ba0.65Sr0.35TiO3) nanocrystalline thin films, which were produced by the soft chemical method, were crystallized at low temperature using a domestic microwave oven. A SiC susceptor were used to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are crack-free, well-adhered, and fully crystallized. The microstructure displayed a polycrystalline nature with nanograin size. The metal-BST-metal structure of the thin films treated at 700 degrees C show food electric properties. The ferroelectric nature of the BST35 thin film was indicated by buttertly- shaped C-V curves. The capacitance-frequency curves reveal that the dielectric constant may reach a value up to 800 at 100kHz. The dissipation factor was 0.01 at 100kHz. The charge storage density as function of applied voltage graph showed that the charge storage densities are suitable for use in trench type 64 Mb ( 1-5 mu C/cm(2) and 265 Mb (2-11 mu C/cm(2)) DRAMs. (C) 2007 Elsevier Ltd. All rights reserved.

Nucleation and growth of mullite whiskers from lanthanum-doped aluminosilicate melts

Nucleation and growth of mullite whiskers in the La2O3-Al2O3-SiO2 system were investigated in the 1500degrees-1700degreesC temperature range. A differential thermal analysis (DTA) showed that the mullitization temperature decreases from 1350degreesC to 1240degreesC as a result of lanthania doping. In the temperature range of 1250-1500degreesC, most of the mullite grains have an Al2O3/SiO2 = 1.5 composition throughout the ceramic body; however, from 1400degreesC upward, the number of anisotropic grains with the Al2O3/SiO2 = 1.3 composition begins to increase. The concentration of alumina in the composition of the grain-boundary phase decreases as firing temperatures increase. At temperatures > 1500degreesC, alumina grains and whiskers grow on the internal and external surfaces of the ceramic body with the characteristic Al2O3/SiO2 = 1.3 composition. Removal of the mullite whisker layer by acid attack revealed an alumina-rich, rosace-like patterned microstructure correlated with the process of whisker nucleation and growth. In the early stages, whisker growth rates were found to be near 60 mum/h. Experimental evidence pointed to nucleation inside the thin glass layer on the external surface.

Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado

ANALYSIS OF CLAYS BY INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY AFTER CLOSED-VESSEL MICROWAVE-ASSISTED ACID DECOMPOSITION. In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.

Very large dielectric constant of highly oriented Pb1-xBaxTiO3 thin films prepared by chemical deposition

Highly (100) oriented Pb0.8Ba0.2TiO3/LaNiO3 structures were grown on LaAlO3(100) substrates by using a wet, soft chemical method and crystallized by the microwave oven technique. The Au/PBT/LaNiO3/LaAlO3 capacitor shows a hysteresis loop with remnant polarization, P-r, of 15 muC/cm(2), and coercive field, E-c, of 47 kV/cm at an applied voltage of 3 V, along with a dielectric constant over 1800. Atomic force microscopy showed that Pb0.8Ba0.2TiO3 is composed of large grains about 300 nm. The experimental results demonstrated that the microwave preparation is rapid, clean, and energy efficient. Therefore, we demonstrated that the combination of the soft chemical method with the microwave process is a promising technique to grow highly oriented thin films with excellent dielectric and ferroelectric properties, which can be used in various integrated device applications. (C) 2004 American Institute of Physics.

Synthesis, structural refinement and optical behavior of CaTiO3 powders: A comparative study of processing in different furnaces

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural and properties of nanocrystalline WO3/TiO2-based humidity sensors elements prepared by high energy activation

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

Bacterial leaching of uranium ore from Figueira-PR, Brazil, at laboratory and pilot scale

A bacterial leaching program was carried out in order to evaluate the potential of applying this process to leach uranium from the ore of Figueira-PR, Brazil. The experiments were carried out in shake flasks, column percolation (laboratory and semipilot scale) and in heap leaching. In shake flasks and in column percolation experiments at laboratory scale, bacterial activity on the ore was confirmed: approximately 60% of uranium was leached, against around 30% in sterilized controls. Column percolation experiments at semipilot scale and heap leaching (850 tons of ore) showed uranium extractions of approximately 50%. In both experiments, a complementary sulfuric acid attack, after the bacterial leaching phase, was necessary to reach this level of uranium extraction.

Effect of post-polymerization heat treatments on the cytotoxicity of two denture base acrylic resins

Introduction: Most denture base acrylic resins have polymethylmethacrylate in their composition. Several authors have discussed the polymerization process involved in converting monomer into polymer because adequate polymerization is a crucial factor in optimizing the physical properties and biocompatibility of denture base acrylic resins. To ensure the safety of these materials, in vitro cytotoxicity assays have been developed as preliminary screening tests to evaluate material biocompatibility. 3H-thymidine incorporation test, which measures the number of cells synthesizing DNA, is one of the biological assays suggested for cytotoxicity testing. Aim: The purpose of this study was to investigate, using 3H-thymidine incorporation test, the effect of microwave and water-bath post-polymerization heat treatments on the cytotoxicity of two denture base acrylic resins. Materials and Methods: Nine disc-shaped specimens (10 x 1 mm) of each denture base resin (Lucitone 550 and QC 20) were prepared according to the manufacturers' recommendations and stored in distilled water at 37°C for 48 h. The specimens were assigned to 3 groups: 1) post-polymerization in a microwave oven for 3 min at 500 W; 2) post-polymerization in water-bath at 55°C for 60 min; and 3) without post-polymerization. For preparation of eluates, 3 discs were placed into a sterile glass vial with 9 mL of Eagle's medium and incubated at 37°C for 24 h. The cytotoxic effect of the eluates was evaluated by 3H-thymidine incorporation. Results: The results showed that the components leached from the resins were cytotoxic to L929 cells, except for the specimens heat treated in water bath (p<0.05). Compared to the group with no heat treatment, water-bath decreased the cytotoxicity of the denture base acrylic resins. Conclusion: The in vitro cytotoxicity of the tested denture base materials was not influenced by microwave post-polymerization heat treatment.

Simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation process by GFAAS

A method has been developed for the simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation by GFAAS. The integrated platform of transversely heated graphite atomizer was treated with tungsten to form a coating of tungsten carbide. Six samples of commercial solid antibiotics were analyzed by injecting 20 μL of digested samples into the pretreated graphite platform with co-injection of 5 μL of 1000 mg L-1 Pd as chemical modifier. Samples were mineralized in a closed-vessel microwave-assisted acid-digestion system using nitric acid plus hydrogen peroxide. The pyrolysis and atomization temperatures of the heating program of the atomizer were selected as 600°C and 2200°C, respectively. The calculated characteristic mass for Cd and Pb was 1.6 pg and 42 pg, respectively. Limits of detection (LOD) based on integrated absorbance were 0.02 μg L -1 Cd and 0.7 μg L-1 Pb and the relative standard deviations (n = 10) for Cd and Pb were 5.7% and 8.0%, respectively. The recoveries of Cd and Pb added to the digested samples varied from 91% to 125% (Cd) and 80% to 112% (Pb).

Microondas doméstico na síntese de derivados ftalimídicos

Microwaves have been used in organic synthesis, since 1986, and have proved advantageous in several respects: the possibility of higher yields, greater selectivity and less thermal decomposition. Phthalimide and its derivatives constitute an important class of compounds for use in synthetic organic chemistry; in medicinal chemistry, it is considered an important biophore, acting as a pharmacophoric structural subunit for the synthesis of a number of compounds with different pharmacological uses, such as against sickle-cell disease. The purpose of the work reported here was to develop an alternative method for the synthesis of phthalimide derivatives by exploiting the condensation of phthalic anhydride with amino groups under microwave radiation. The results showed that phthalimide derivatives were obtained in shorter reaction times (5-10 min) and higher yields (60-89%) than by with conventional heating (reflux), demonstrating the potential use of microwaves in the synthesis of this class of molecules.