Modelagem dos processos químicos em plasmas de misturas gasosas usadas na corrosão de silício. Parte 1: CF4 / O2

The plasma etching of semiconductor surfaces with fluorine-containing compounds has technological interest. Presently, considerable effort is being devoted to understand the chemistry involved. In this work, a numerical modeling analysis of the gas-phase decomposition of CF4/O2 mixtures, in the presence of silicon, was performed. The relative importance of individual processes was determined as well as the effect of the parameters' uncertainties. The results were compared with experimental data. The main etching agent in the system is the fluorine atom. The concentration of the main species, SiF4, CO, CO2 and COF2 depend on the composition of the mixture.

Vidros recobertos com camadas delgadas transparentes de SnO2

SnO2 thin layers, prepared from aqueous colloidal suspensions by the sol-gel process, have been dip-coated on commercial borosilicate glasses. The effect of the conditions of deposition on the optical and structural characteristics of the thin layers was analysed by UV-Vis spectroscopy, x-ray reflectometry and electron scanning microscopy. Layers prepared with withdrawal speed in between 0.1 and 10cm/min show thickness smaller than 90nm, roughness of the order of 2nm and transmittance higher than 80%, resulting in good optical quality samples. The roughness increases from 2 to 11nm as the withdrawal speed increases from 10 to 80cm/min, what seems to be associated to the enlargement of the layers thickness (> 90nm). The measurements of mass loss, done after etching with fluoridric acid show that the coated samples are more corrosion resistant than the uncoated borosilicate glass.

Rotas de síntese e a homogeneidade dos precursores de mulita e cordierita

Multicomponent ceramics are mainly synthesized by conventional solid-state reaction route and sol-gel routes. In the sol-gel route, colloidal or polymeric gel are envolved. In this work, some principles of the chemistry of theses routes are discused and it is ilustrated a variety of strategies for obtaining a homogeneous multicomponent precursors.

Utilização de eletrodos potenciométricos de amálgama em estudos de complexação de substâncias húmicas

Potentiometric amalgam electrodes of lead, cadmium, and zinc are proposed to study the complexation properties of commercial and river sediment humic acids. The copper complexation properties of both humic acids were studied in parallel using the solid membrane copper ion-selective electrode (Cu-ISE). The complexing capacity and the averaged conditional stability constants were determined at pH 6.00 ± 0.05 in medium of 2x10-2 mol L-1 sodium nitrate, using the Scatchard method. The lead and cadmium amalgam electrodes presented a Nernstian behavior from 1x10-5 to 1x10-3 moles L-1 of total metal concentration, permitting to perform the complexation studies using humic acid concentrations around of 20 to 30 mg L-1, that avoids colloidal aggregation. The zinc amalgam electrode showed a subnernstian linear response in the same range of metal concentrations. The Scatchard graphs for both humic acids suggested two classes of binding sites for lead and copper and one class of binding site for zinc and cadmium.

Aplicação da espectroscopia de ressonância magnética nuclear para estudos de difusão molecular em líquidos: a técnica DOSY

Diffusion coefficients provide uniquely detailed and easily interpreted information on molecular organization and phase structure. They are quite sensitive to structural changes, and to binding and association phenomena, in particular for liquid colloidal or macromolecular systems. This paper describes the principles of diffusion measurements in liquids by pulsed magnetic field gradient spin-echo (PFG-SE) NMR spectroscopy. The important PFG-SE technique known as DOSY is presented and discussed. This is a noninvasive technique that can provide individual multicomponent translational diffusion coefficients with good precision in a few minutes, without the need for radioactive isotopic labelling.

Caracterização e estabilidade físico-química de sistemas poliméricos nanoparticulados para administração de fármacos

Polymeric nanoparticle systems such as nanocapsules and nanospheres present potential applications for the administration of therapeutic molecules. The physico-chemical characteristics of nanoparticle suspensions are important pre-requisites of the success of any dosage form development. The purpose of this review is to present the state of the art regarding the physico-chemical characterization of these drug carriers, in terms of the particle size distribution, the morphology, the polymer molecular weight, the surface charge, the drug content and the in vitro drug release profiles. Part of the review is devoted to the description of the techniques to improve the stability of colloidal systems.

Construção de uma fonte de corrente e de uma sonda para medida de condutividade pelo método da sonda de quatro pontas

This paper describes the construction of an eletrical current source and of a probe to be used in the measurement of eletrical conductivity through a four-point probe method. These pieces of equipments can be obtained at the low price of US$ 50.00 and are adequate for eletrical conductivity measurements in the semiconductor range, that is from 10-1 to 10-6 S cm-1.

Decomposição térmica de complexos de Zn e Cd com isomaleonitriladitiolato (imnt)

Thermal decomposition of [Bu4N]2[Zn(imnt)2] and [M(NH3)2(imnt)] complexes with M = Zn and Cd, and imnt = (bis 1,1-dicyanoethylene-2,2 dithiolate) in inert atmosphere was investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Pyrolysis studies at different temperatures, 300, 400, 500, and 600 ºC, in N2 atmosphere were performed and the products were characterized by X-ray diffraction (XRD), infrared and Raman spectroscopy, and scanning electron microscopy (SEM). The products were identified as sulfide sub-micron particles, along with amorphous carbon. Particle sizes estimated by SEM were ca. 50 nm for the cationic complexes and 500 nm for the neutral complexes.

Determinação turbidimétrica de dipirona em fluxo utilizando um reator contendo cloreto de prata imobilizado em resina poliéster

A simple flow injection procedure was developed for determining dipyrone (1-phenyl-2,3-dimethyl-4-methylaminomethano-5-pyrazolone sodium, metamizol, analgin) in pharmaceutical formulations. The determination is based on the reduction of Ag+ ions to Ag0 by dipyrone. A colloidal suspension of Ag0 produced was transported by carrier solution (0.01 mol L-1 NaOH) and turbidimetrically detected at 425 nm. The analytical curve for dipyrone was linear in the range from 5.0 x 10-4 to 2.5 x 10-3 mol L-1 with a correlation coefficient of 0.9990. The detection limit was 1.3 x 10-4 mol L-1 (3sigmaB/slope). The relative standard deviation for ten successive measurements was 1.8% and an analytical frequency of 45 h-1 was obtained. The recovery values from three samples ranged from 96.0 to 102%.

Preparação e caracterização de substratos SERS ativos: um estudo da adsorção do cristal violeta sobre nanopartículas de prata

The structural characterization of molecules used in the sterilization of blood for transfusions, such as crystal violet (CV), is relevant for understanding the action of these prophylactic drugs. The characterization is feasible by surface enhanced resonance Raman spectroscopy (SERRS) of CV in solution or on surfaces. The limit of detection of CV by SERRS, in the presence of colloidal particles, using 514.5 nm as excitation radiation, was found to be around 1 ppb. The characterization of CV was also made by SERS, by using different active-particles-containing substrates, proving the versatility of this technique for the study of such structures. The results suggest that the controlled production of highly efficient SERS-active substrates may allow qualitative and quantitative analysis, with high sensitivity, with potential applications in medical and environmental fields.

O pKa de indicadores ácido-base e os efeitos coloidais

An experiment is proposed that can be included in undergraduate courses of chemistry. The subject is the acidity of organic compounds, which are employed as pH indicators, particularly in acid-base titrations. The indicators used are methyl orange, bromophenol blue and bromocresol green in aqueous medium. The influence of colloidal systems on the equilibrium is evaluated by the pKa. The colloids employed are surfactants like sodium dodecyl sulfate, cetyl-trimethylammonium bromide and a polymeric non-ionic F127 (pluronics). The effect of stabilization promoted by the system on the acidic or basic structureof the indicator establishes the action mechanism of the colloid on the pKa values.

Espectroscopia de impedância eletroquímica aplicada ao estudo das reações heterogêneas em ânodos dimensionalmente estáveis

This paper discusses different aspects related to the application of electrochemical impedance spectroscopy (EIS) in the study of heterogeneous electrochemical reactions occurring on Dimensionally Stable anodes (DSA®). The most relevant aspects of the semiconductor/electrolyte interface, the application of the EIS classical equivalent circuit approach and the ac porous model in DSA are presented. The paper shows that DSA type electrodes can be consistently investigated by using the ac porous model and an analysis is presented showing the advantage of applying this kind of approach to study heterogeneous reactions on DSA electrodes. Furthermore, some preliminary results on Ti/Ru0,3Ti(0,7-x)Sn x O2 based electrodes are presented to exemplify the use of the ac porous model analysis.

Obtenção de filmes espessos de seleneto de cobre sobre carbono vítreo, ouro, titânio e cobre

Copper selenide (berzelianite) films were prepared on the title substrates using the chemical bath deposition technique (CBD). Film composition was determined by energy dispersion of x-rays. The kinetics of film growth is parabolic and film adherence limits the film thickness. On titanium, copper selenide forms islands that do not completely cover the surface, unless the substrate is prepared with a tin oxide layer; film composition also depends on the titanium oxide layer. On vitreous carbon, CBD and mechanical immobilization techniques lead to films with similar resistances for the electron transfer across the film/substrate interface. On gold, composition studies revealed that film composition is always the same if the pH is in the range from 8 to 12, in contrast to films prepared by an ion-ion combination route. On copper, a new procedure for obtaining copper selenide films as thick as 5 µm has been developed.

Electrical and magnetic properties of new compounds of the conductor anion [Ni(dmit)2]- and nitronyl nitroxide magnetic radicals

Three compounds have been synthesized with formulae [3-MeRad][Ni(dmit)2] (1), [4-MeRad][Ni(dmit)2] (2) and [4-PrRad][Ni(dmit)2] (3) where [Ni(dmit)2]- is an anionic pi-radical (dmit = 1,3-dithiol-2-thione-4,5-dithiolate) and [3-MeRad]+ is 3-N-methylpyridinium alpha-nitronyl nitroxide, [4-MeRad]+ is 4-N-methylpyridinium alpha-nitronyl nitroxide and [4-PrRad]+ is 4-N-propylpyridinium alpha-nitronyl nitroxide. The temperature-dependent magnetic susceptibility of 1 revealed that an antiferromagnetic interaction operates between the 3-MeRad+ radical cations with exchange coupling constants of J1 = - 1.72 cm-1 and antiferromagnetism assigned to the spin ladder chains of the Ni(dmit)2 radical anions. Compound 1 exhibits semiconducting behavior and 3 presents capacitor behavior in the temperature range studied (4 - 300 K).

Características ópticas e morfológicas de nanoestruturas de ouro

The present study describes a new procedure to obtain gold nanoparticles, directly in the pores of polycarbonate membranes commonly used in ultrafiltration. The dimensions of the particles may be controlled through the reduction time of the ions in the channels of the harbor matrix. The dissolution of the metallized polymer enables an investigation of the optical and morphologic properties of these elements.