Preparo de filmes-suporte para microscópio eletrônico

Working with low voltage microscope (R.C.A., EMC-2, of 30KV.) the authors verified that parlodion and Formvar films are quickly destroyed by intense heating under the electron beam. They have tried to employ oxide films, as Al2O3 and SiO, more resistant to heat. Al2O3 films are prepared by anodic oxidation of thin aluminium sheets, under 8 to 10 volts in a 3% ammonium citrate solution and subsequent aluminium dissolution in a O.25% HgCl2 solution. These films are very suitable when prepared with highly pure aluminium of extremely homogeneous surface. Best results were obtained with SiO films, evaporated in high vacuum over Parlodion films mounted on metallic grids. Employing 1 or 1.5 mg of SiOm highly homogeneous and resistant films are obtained, having little inferior transparence than the Parlodion ones. Pure SiO films (1.5 mg) are obtained by elimination of the Parlodion under slow heating until 250°C; they are greatly transparent but little resistant to water, thus beeing indicated in dry preparations. For particles which deposite in a chain-like form around thin fibers, the authors employ the mounting on Parlodion fibers, obtained by heating Parlodion films on microscope grids about 190°C.

Fotocromismo em filmes finos de óxidos de tungstênio de diferentes composições

Tungsten oxide thin films with three different compositions were deposited by reactive sputtering in an oxygen-argon plasma. In a system composed of a home made photochemical reactor coupled with an optic fiber spectrophotometer, the photochromic effect was studied in these oxide films as function of UV irradiation time, in ethanol, methanol and formaldehyde atmospheres. It was observed that the photochromic efficiency depends on the vapor chemical nature where the film is irradiated as well as the film composition. Kinetic analysis suggest that two kinds of optical absorption centers should respond by the photochromic effect in these films, one generated at film surface and other inside it, which one presenting a different time constant.

Catálise eletroquímica da redução do bromato em superfícies modificadas por filmes de molibdênio

In this paper some studies concerning the electroreduction of Mo(VI) in sulphuric acid solutions are described. We have shown that at suitable experimental conditions very stable molybdenum oxide films can be electrochemically deposited at glassy carbon electrodes, the reduction of bromate occurring at less negative potentials on the modified surface. Coulometric experiments have shown that bromide is not the only product of the catalytic bromate reduction by the molybdenum film and species like BrO2 may have part in this process. Based on chronoamperometric curves recorded at -0.60 V, analytical curves have been obtained for the reduction of bromate in the 0.1 - 0.8 mM range, a limit of detection of 20 µM for bromate being determined.

Filmes de óxidos anódicos de nióbio: efeito eletrocrômico e cinética da reação de eletro-intercalação

The aim of this work is to study the electrochromism and the reaction kinetics of lithium electrointercalation in anodic niobium oxide films. The oxide grown in an acid environment by application of an alternating potential shows interference colour (iridescence) and when reduced in lithium perclorate/PC solution, the intercalation of Li+ ions and electrons causes a reversible colour change (electrochromism), characterized here by electrochemical and optical measurements. A model where the reaction kinetics is dominated by diffusion of ionic pairs (Li+, e-) in the oxide film permitted the reproduction of current and absorbance temporal dependence, confirming the relationship between the electrochromic and electrochemical reactions. From the results obtained, a relation was established where the colour change is associated to the reduction of Nb+5 to Nb+4 ions with simultaneous cations injection.

Dióxido de titânio sol-gel: propriedades e comportamento eletrocrômico

Titanium dioxide was prepared by hydrolysis and polycondensation of titanium tetraisopropoxide. TiO2 films were obtained by spin coating of the precursor solution on ITO substractes (glass covered with indium doped tin oxide). Films were prepared using different temperatures and hydrochloric acid contents. The effect of the drying temperature of the films (100 or 400ºC) was also investigated. TiO2 films were characterized by cyclic voltammetry, chronoamperometry, ultraviolete-visible spectroscopy, scanning electron microscopy and X-ray diffractrometry.

Estudo de efeito dos sais precursores sobre as propriedades eletrocatalíticas de eletrodos de Ti-SnO2/Sb preparados por decomposição térmica

The physical and electrochemical properties of Ti-SnO2/Sb electrodes obtained by the thermal decomposition of solutions of the precursor salts SnCl2×2H2O/SbCl3 and SnSO4/Sb2(SO4)3 were investigated. The reversibility of the cyclic voltammetric response of the Fe(CN)6(4-)/Fe(CN)6(3-) redox couple was assessed using the obtained electrodes. Their catalytic activity for the oxygen-evolving reaction and maximum capacity for electronic transfer were also evaluated by potential and current linear scans in 0.5 mol L-1 H2SO4. Additionally, scanning electron microscopy analyses allowed the visualization of the morphology of the oxide films obtained. The best results were presented by the electrodes obtained from the chloride salt precursors.

Influência das condições de resfriamento sobre as propriedades superficiais e eletroquímicas de anodos dimensionalmente estáveis

Surface and electrochemical properties of the dimensionally stable anode Ti/(Ru0.3Ti0.7)O2 were studied as a function of the annealing temperature using different conditions in order to perform the cooling process of the oxide films (conventional thermal shock and the slow cooling processes). It was found that surface and electrochemical properties for the oxygen evolution reaction are both affected through the cooling process, being the electrode prepared at 400 ºC using the slow cooling process the less susceptible to wear. The Tafel slope obtained in the high overpotential domain was analysed in light of the apparent charge transfer coefficient.

Use of thin films obtained by plasma polymerization for grain protection and germination enhancement

In this work, preliminary results of the use of hydrophobic thin films obtained by plasma deposition to protect grains and seeds are presented: grains coated by the films did not present biological degradation when stored in a saturated water vapor environment, but had their germination accelerated in the presence of water. A model that explains the difference of behavior of the films when exposed to water in vapor form or in liquid form, based on the formation of microchannels within the film that lead to water uptake in seeds, is presented. The model was successfully tested using quartz crystal measurements, which showed that the microchannels within the films can favor the adsorption and permeation of water when the films are immersed in water.

Plasma polymerized acetaldehyde thin films for retention of volatile organic compounds

The aim of this work is the production and characterization of plasma polymerized acetaldehyde thin films. These films show highly polar species, are hydrophilic, organophilic and easily adsorb organic reactants with CO radicals but only allow permeation of reactants with OH radicals. The good step coverage of films deposited on aluminum trenches is useful for sensor development. Films deposited on hydrophobic substrates may result in a discontinued layer, which allows the use of preconcentration in sample pretreatment. Deposition on microchannels showed the possibility of chromatographic columns and/or retention system production to selectively detect or remove organic compounds from gas flows.

Preparation and electrochemical characterization of Pt nanoparticles dispersed on niobium oxide

Electrodes consisting of Pt nanoparticles dispersed on thin films of niobium oxide were prepared onto titanium substrates by a sol-gel method. The physical characterization of these electrodes was carried out by X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. The mean size of the Pt particles was found to be 10.7 nm. The general aspects of the electrochemical behavior were studied by cyclic voltammetry in 1 mol L-1 HClO4 aqueous solution. The response of these electrodes in relation to the oxidation of formaldehyde and methanol in acidic media was also studied.