SrBi2Ta2O9 ferroelectric thick films prepared by electrophoretic deposition using aqueous suspension

SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol.% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). It was investigated the influence of the different dispersants in the surface properties of the powder by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by a 4 mA constant current, for 10 min, using two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit were carried out until reaching the desired thickness. After thermal treatment at temperatures ranging from 700 to 1000 degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy for the microstructure observation. (C) 2003 Elsevier Ltd. All rights reserved.

Improvement of the Mo/TiO2-Al2O3 catalyst by the control of the sol-gel synthesis

Traditional hydrotreating catalysts are constituted by molybdenum deposited on Al2O3 promoted by nickel and phosphorous. Several studies have shown that TiO2-Al2O3 mixed oxides are excellent supports for the active phases. Results concerning the preparation, characterization and testing of molybdenum catalyst supported on titania-alumina are presented. The support was prepared by sol-gel route using titanium and aluminum isopropoxides, the titanium one chelated with acetylacetone (acac) to promote similar hydrolysis ratio for both the alcoxides. The effect of nominal molar ratio [Ti]/[Ti+Al] on the microstructural features of nanometric particles was analyzed by X-Ray Diffraction, N-2 Adsorption Isotherms and Transmission Electron Microscopy. The catalytic activity of Mo impregnated supports was evaluated using the thiophene hydrodesulfurization at different temperatures and atmospheric pressure. The pores size distribution curve moves from the micropores to the mesopores by increasing the Ti contents, allowing the fine tuning of average size from 2.5 to 6 nm. Maximal (367 m(2).g(-1)) and minimal (127 m(2).g(-1)) surface area were found for support containing [Ti]/[Ti+Al] ratio equal to 0.1 and 1, respectively. The good mesopore texture of alumina-titania support with [Ti]/[Ti+Al] molar ratio between 0.3 and 0.5 was found particularly valuable for the preparation of well dispersed MoS2 active phase, leading to HDS catalyst with somewhat higher activity than that prepared using a commercial alumina support.

On the stabilizing behavior of zirconia: A combined experimental and theoretical study

Reactive zirconia powder was synthesized by the complexation of zirconium metal from zirconium hydroxide using a solution of 8-hydroxiquinoline. The kinetics of zirconia crystallization was followed by X-ray diffraction, scanning electron microscopy and surface area measured by the nitrogen adsorption/desorption technique. The results indicated that zirconia with a surface area as high as 100 m(2)/g can be obtained by this method after calcination at 500degreesC. Zirconia presents three polymorphic phases (monoclinic, tetragonal and cubic), which are reversibly interconversible. The cluster model Zr4O8 and Z(r)4O(7)(+2) was used for a theoretical study of the stabilization process. The ab initio RHF method was employed with the Gaussian94 program and the total energies and the energy gap of the different phases were calculated and compared with the experimental energy gap. The theoretical results show good reproducibility of the energy gap for zirconia. (C) 2004 Kluwer Academic Publishers.

Sol-gel entrapped cobalt complex

This work describes optimized conditions for preparation of a cobalt complex entrapped in alumina amorphous materials in the form of powder. The hybrid materials, CoNHG, were obtained by a nonhydrolytic sol-gel route through condensation of aluminum chloride with diisopropylether in the presence of cobalt chloride. The materials were calcined at various temperatures. The presence of cobalt entrapped in the alumina matrix is confirmed by ultraviolet visible spectroscopy. The materials have been characterized by X-ray diffraction (XRD), surface area analysis, thermogravimetric analysis (TGA), differential thermal analyses (DTA) and transmission electron microscopy (TEM). The prepared alumina matrix materials are amorphous, even after heat treatment up to 750 degreesC. The XRD, TGA/DTA and TEM data support the increase of sample crystallization with increasing temperature. The specific surface area, pore size and pore diameter changed as a function of the heat treatment temperature employed. Different heat treatment temperatures result in materials with different compositions and structures, and influence their catalytic activity. The entrapped cobalt materials calcined at 750 degreesC efficiently catalyzed the epoxidation of (Z)-cyclooctene using iodozylbenzene as the oxygen donor. (C) 2003 Elsevier B.V. All rights reserved.

Plasma nitriding of sintered AISI 316L at several temperatures

Samples of sintered AISI 316L stainless steel were plasma nitrided in a mixture of H-2-20% N-2, for 3 or 4 h. The treatment temperature was selected in 400-550 degreesC interval, in steps of 50 degreesC. X-ray diffraction (glancing angle geometry-GAXRD), conversion electron Mossbauer spectroscopy (CEMS), optical microscopy and Vickers microhardness were used as analytical techniques. For T greater than or equal to 500 degreesC and t = 4 h, a 40-mum layer is formed. The GAXRD results showed a transformation of the austenite gamma phase to the martensite in the sinterization process and showed as well, that the gamma' (Fe4N) phase is the predominant nitride besides small amounts of epsilon-Fe2N, gamma(N) CrN, Cr2O3 and the fcc nitrogen supersatured solid phase gamma(N). The CrN phase seems to decrease with temperature while the gamma(N) phase fraction is almost less than or equal to10%, independently on the temperature. The CEMS results indicated that while the gamma(N) fraction decreases with temperature of plasma nitriding, the gamma' fraction increases proportionally. (C) 2003 Elsevier B.V. All rights reserved.

Crytallization and high-resolution X-ray diffraction data collection of an Asp49 PLA(2) from Bothrops jararacussu venom both in the presence and absence of Ca2+ ions

Snake venom PLA(2)s have been extensively studied due to their role in mediating and disrupting physiological processes such as coagulation, platelet aggregation and myotoxicity. The Ca2+ ion bound to the putative calcium-binding loop is essential for hydrolytic activity. We report the crystallization in the presence and absence of Ca2+ and X-ray diffraction data collection at 1.60 Angstrom (with Ca2+) and 1.36 Angstrom (without Ca2+) of an Asp49 PLA(2) from Bothrops jararacussu venom. The crystals belong to orthorhombic space group C222(1). Initial refinement and electron density analysis indicate significant conformational. changes upon Ca2+ binding. (C) 2004 Elsevier B.V. All fights reserved.

Monodispersed spindle-type goethite nanoparticles from Fe-III solutions

A new synthetic route for producing monodispersed and single crystal acicular goethite particles with small particle size and a high axial ratio adequate for use as a high density magnetic recording media precursor is reported. It essentially consists of the hydrolysis of alkaline Fe-III suspensions in the presence of carbonate by a three-step procedure, the formation of ferrihydrite primary particles, the ferrihydrite dissolution and nucleation of goethite, and the growth of the goethite nuclei. Changing the temperature of heating during ageing achieved a separation of the two last stages. X-Ray diffraction, transmission electron microscopy, infrared spectroscopy and surface area data have been used to determine the mechanism responsible for the formation of goethite particles with controlled size and shape. The best conditions to prepare monodispersed goethite particles have been established. The results show that uniform goethite particles of (a) 60 nm length with an axial ratio of 6 and (b) 230 nm length with a high axial ratio of 10, can be obtained by using an [OH]/[Fe] molar ratio of 0.35 in the initial suspensions with carbonate or sodium hydroxide, respectively. The [OH]/[Fe] molar ratio determines the particle size and elongation by controlling the hydrolysis reaction rate, while the carbonate ions promote a constant [OH] in the solution, keeping the pH around 10 during the entire synthesis process. This procedure, associated with the appropriate temperature control, leads, under certain conditions, to highly homogeneous goethite particles with sizes smaller than those obtained using sodium hydroxide with the same [OH]/[Fe] ratio.

Preparation of SrBi2Ta2O9 ferroelectric thick films by electrophoretic deposition using aqueous suspensions

SrBi2Ta2O9 ferroelectric thick films were prepared by electrophoretic deposition (EPD). For that, ceramic powders were prepared by chemical method in order to obtain compounds with chemical homogeneity. The polymeric precursor method was used for the synthesis of the SrBi2Ta2O9 powder. The crystallographic structure of the powder was examined by X-ray diffraction, and the surface area was determined by single point BET adsorption. The 0.03 vol% suspension was formed by dispersing the powder in water using two different polymers as dispersants: an ester polyphosphate (C213) and an ammonium polyacrilate (Darvan 821-A). The influence of the different dispersants on the powder surface properties were investigated by zeta potential measurements. The films were deposited on platinum-coated alumina and Pt/Ti/SiO2/Si substrates by electrophoretic deposition using a 4 mA constant current, for 10 min, with two parallel electrodes placed at a separation distance of 3 min in the suspension. Several cycles of deposition-drying of the deposit was carried out until the desired thickness was obtained. After thermal treatment at temperatures ranging from 700 to 1000degreesC, the films were characterized by X-ray diffraction and scanning electron microscopy.

Nanocrystalline Ga1-xMnxN films grown by reactive sputtering

The growth of nanocrystalline Ga1-zMnxN (0.00 <= x <= 0.18) films grown by reactive RF-magnetron sputtering is focused here for the first time. The films were grown in a N-2 atmosphere by co-sputtering technique using a Ga target covered with small pieces of Mn onto c-GaAs (10 0), c-Si (10 0) and amorphous SiO2 substrates maintained at 500 K. Scanning electron microscopy and X-ray diffraction (XRD) experiments did not show any evidence for Mn segregation within the studied composition range. EDX measurements show that the Mn concentration is increased monotonically with the fraction of the target area covered by Mn. The XRD characterization show that the films are nanocrystalline, the crystallites having mean grain sizes in the 15-19 nm range and wurtzite structure with preferential growth orientation along the c-axis direction. The lattice parameters of alpha-GaN (a and c) increase practically linearly with the increase of Mn incorporation. The changes in the structural properties of our films due to the Mn incorporation are similar to those that occur in ferromagnetic GaMnN single-crystal films. (c) 2006 Elsevier B.V. All rights reserved.

Photoinduced effect in Ga-Ge-S based thin films

Glassy films of Ga10Ge25S65 with 4 mu m thickness were deposited on quartz substrates by electron beam evaporation. Photoexpansion (PE) (photoinduced increase in volume) and photobleaching (PB) (blue shift of the bandgap) effects have been examined. The exposed areas have been analyzed using perfilometer and an expansion of 1.7 mu m (Delta V/V approximate to 30%) is observed for composition Ga10Ge25S65 exposed during 180 min and 3 mW/cm(2) power density. The optical absorption edge measured for the film Ge25Ga10S65 above and below the bandgap show that the blue shift of the gap by below bandgap photon illumination is considerable higher (Delta E-g = 440 meV) than Delta E-g induced by above bandgap illumination (Delta E-g = 190 meV). The distribution of the refraction index profile showed a negative change of the refraction index in the irradiated samples (Delta n = -0.6). The morphology was examined using a scanning electron microscopy (SEM). The chemical compositions measured using an energy dispersive analyzer (EDX) indicate an increase of the oxygen atoms into the irradiated area. Using a Lloyd's mirror setup for continuous wave holography it was possible to record holographic gratings using the photoinduced effects that occur in them. Diffraction efficiency up to 25% was achieved for the recorded gratings and atomic force microscopy images are presented. (c) 2005 Elsevier B.V. All rights reserved.

Crystallization at room temperature from amorphous to trigonal selenium as a byproduct of the synthesis of water dispersible zinc selenide

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

Leishmania chagasi infection in cats with dermatologic lesions from an endemic area of visceral leishmaniosis in Brazil

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

Crystallization of nordstrandite in ethylene glycol water solutions: electron microscopic studies

The present work shows the growth of nordstrandile microcrystals observed by transmission and scanning electron microscopy. Nordstrandite was synthesised from non-crystalline aluminium hydroxide reacted in 20% ethylene glycol/water solution, at room temperature. This material was characterized by TEM, SEM, SAED, XRD and EDS/TEM, during six month and revealed the formation and growth of nordstrandite. Fibrillar pseudoboehmite is the only aluminium hydroxide which could be identified during the first two weeks. The nuclei grow, from complete dissolution/recrystallization of pseudoboehmite fibrils, into platy rectangular microscrystals of nordstrandite. Some tabular microcrystals recrystallise, forming after six months only the mufti-point nordstrandite stars. This electron-optical study suggest that the star shape results from the overlapping of rectangular plates, and pseudoboehmite fibrils act as the precursor of nordstrandite crystallisation in ethylene glycol/water solution.

Leishmania chagasi infection in cats with dermatologic lesions from an endemic area of visceral leishmaniosis in Brazil

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

Calcium polyphosphate coacervates: effects of thermal treatment

The addition of calcium chloride eletrolyte to sodium polyphosphate solutions lead to Calcium polyphosphate coacervates. The effects of a thermal treatment were investigated with the objective to increase the relative stability of the obtained material. Thermogravimetry analysis indicates that coacervates became less hydrophilic and more thermally stable after the thermal treatment. Crystallization was identified through differential scanning calorimetry and X-ray diffraction. Morphological changes were observed after the thermal treatment by scanning electron microscopy. N-2 adsorption-desorption isotherms suggest that both materials, thermally treated or not, display type IV isotherms, low superficial area and mesoporous structure. Stability experiments in solutions at different pH values show that the thermally treated calcium polyphosphate is relatively more stable than the non-treated coacervate.