Electrodeposition and characterization of thin selenium films modified with lead ad-atoms

The deposition and characterization of Se films doped with Pb underpotentially deposited (UPD) ad-atoms was studied in this work. The employed experimental techniques were cyclic voltammetry, chronoamperometry, electrochemical impedance spectroscopy, UV-vis spectroscopy and atomic force microscopy. The initial deposition of Se film by chronoamperometry yielded a thin film composed of approximately 700 layers. The Pb UPD on Se was achieved by chronoamperometry in a potential value previously determined in voltammetric experiments. This deposition yielded a deposition charge of approximately 7.5% of the total one. The film resistance altered from 320 Omega cm(2) for Se to 65 Omega cm(2) for the Se/Pb one. Flat band potential values and number of acceptors and donors were also calculated for both films and the values obtained were + 0.95 and -0.51 V for Se and Se/Pb, respectively. The Se coating presented 1.2 x 10(17) cm(3) acceptors while the Se/Pb one presented 3.2 x 10(17) cm(3) donors. The band gap values for both films were 2.4 eV and 1.9 eV, correspondingly. (C) 2008 Elsevier B.V. All rights reserved.

Preparation and characterization of ordered intermetallic platinum phases for electrocatalytic applications

Ordered intermetallic phases of Pt with several transition metals have been prepared and their electrocatalytic properties studied. In light of these tests it is proposed that these catalysts could be used as electrodes in fuel cells, as they combine an excellent capacity to adsorb organic fuels at the Pt sites with low susceptibility to being poisoned by intermediates and reaction products at the transition-metal sites. An experimental procedure used to obtain the four intermetallic phases Pt-M (M = Mn, Pb, Sb and Sn) is described. The phases thus produced were characterized by X-ray diffraction, scanning electron microscopy with surface analysis by energy-dispersive X-ray spectrometry, scanning tunneling microscopy and X-ray photoelectron spectroscopy. The data thus obtained support the conclusion that the method described here is highly effective for the preparation of Pt-M phases featuring a range of structural and electronic modifications that will allow a useful relation to be established between their physicochemical properties and predicted electrocatalytic activity. (C) 2007 Elsevier Ltd. All rights reserved.

Electrodeposition and characterization of undoped and nitrogen-doped ZnSe films

Semiconducting films of (n-type) ZnSe and (p-type) nitrogen-doped ZnSe were electrodeposited by a linear-sweep voltammetric technique on to a substrate of fluorine-tin oxide (FM) glass ceramics. The films were characterized by scanning electron microscopy, energy-dispersive X-ray analysis and grazing-incidence X-ray diffraction. The results indicated that the material was deposited uniformly over the substrate, forming clusters when the Zn content of the bath was 0.1 mol L(-1) and a film when it was 0.2 or 0.3 mol L(-1). The effectiveness of doping the films with nitrogen by adding ammonium sulfate to the deposition solution was assessed by measuring the film-electrolyte interface capacitance (C) at various applied potentials (E(ap)) and plotting Mott-Schottky curves (C(-2) vs E(ap)), whose slope sign was used to identify p-type ZnSe. (C) 2009 Elsevier B.V. All rights reserved.

A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E(1/2)(ox)) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v = 20 mV s(-1)). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10(-4) to 4.0 x 10(-3) mol L(-1) for the determination of nitrite, with a detection limit of 2.1 x 10(-4) mol L(-1) and the amperometric sensitivity of 8.04 mA/mol L(-1). (C) 2010 Elsevier Ltd. All rights reserved.

Preparation and characterization of PVDF/CaCO3 composites

The contribution of new materials, involving composites and blends, has been reaching the most varied fields of science, as much of the scientific as technological point of view. This is due to the man's needs in applications, especially in medicine areas. Thus, this work shows the preparation and characterization of poly(vinylidene fluoride) (PVDF) and calcium carbonate (CaCO3) Composite films in order to analyse the incorporation of CaCO3 in PVDF for future application in bony restoration and bony filling. The films were prepared by casting method, where the PVDF pellet shape was dissolved in dimethylacetamide (DMA) and in a separate container CaCO3/DMA emulsion was also made. Soon afterwards they were mixed in several proportions 100/00, 95/05, 85/15, 70/30 in weight and left to dry in greenhouse. Homogeneous and flexible films were obtained and structurally characterized by attenuated total reflection infrared spectroscopy (FT-IR/ATR), thermal analyses (DSC, TGA), X-ray diffractometry, optical and scanning electron microscopies. The results showed that the material was a composite with good thermal stability until around 400 degrees C, the crystallinity of PVDF was non-polar alpha-phase and the obtained films were porous, being these filled with CaCO3. (c) 2006 Elsevier B.V. All rights reserved.

Synthesis and structural characterization of Eu(III)-doped Zn7Sb2O12

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

Fractal characterization of brittle fracture in ceramics under mode I stress loading

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

Mechanical, physical, and chemical characterization of Ti-35Nb-5Zr and Ti-35Nb-10Zr casting alloys

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

Characterization and in vitro evaluation of bacterial cellulose membranes functionalized with osteogenic growth peptide for bone tissue engineering

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

Synthesis, characterization, structural refinement and optical absorption behavior of PbWO(4) powders

The present paper describes the synthesis, characterization, structural refinement and optical absorption behavior of lead tungstate (PbWO(4)) powders obtained by the complex polymerization method heat treated at different temperatures for 2h in air atmosphere. PbWO(4) powders were characterized by X-ray diffraction (XRD), Rietveld refinement, Fourier transform Raman (FT-Raman) spectroscopy and ultraviolet visible (UV-vis) absorption spectroscopy measurements. XRD, Rietveld refinement and FT-Raman revealed that PbWO(4) powders are free of secondary phases and crystallizes in a tetragonal structure. The UV-vis absorption spectroscopy measurements suggest the presence of intermediary energy levels into the band gap of structurally disordered powders. (C) 2008 Elsevier B.V. All rights reserved.

Electrical characterization of in situ polymerized polyaniline thin films

The alternating conductivity, sigma*(f) = sigma'(f) + i sigma ''(f), of in situ polymerized polyaniline thin films doped with hydrochloric acid, deposited on top of an interdigitated gold line array previously deposited on glass substrates, were measured in the frequency (f) range between 0.1 Hz to 10 MHz and in the temperature range from 100 to 430 K. The results for sigma'(f) are typical of a disordered solid material: for frequencies lower than a certain hopping frequency gamma(hop), log[sigma'(f)] is frequency-independent rising almost linearly for in logf > gamma(hop). A master curve was thus obtained by plotting the real component of the conductivity using normalized scales sigma'(f)/sigma(dc) and f/gamma(hop) which is indicative of a single process operating in the whole frequency range. An expression encompassing the conduction through a disordered structure taken from previous random free energy barrier model for hopping carriers, as well a dielectric function to represent the capacitive behavior of the PAni was employed to fit the experimental results. The dielectric constant and activation energy for hopping carriers were obtained as function of the polymer doping level. (c) 2007 Elsevier B.V. All rights reserved.

Electrochemical impedance spectroscopy characterization of passive film formed on implant Ti-6Al-7Nb alloy in Hank's solution

The influence of potential on electrochemical behavior of Ti-6Al-7Nb alloy under simulate physiological conditions was investigated by electrochemical impedance spectroscopy (EIS). The experimental results were compared with those obtained by potentiodynamic polarization curves. All measurements were carried out in Hank's aerated solution at 25degreesC, at pH 7.8 and at different potentials (corrosion potential, 0 mV(SCE), 1000 mV(SCE), and 2000 mV(SCE)). The EIS spectra exhibited a two-step or a two-time constant system, suggesting the formation of a two-layer oxide film on the metal surface. The high corrosion resistance, displayed by this alloy in electrochemical polarization tests, is due to the dense inner layer, while its osseointegration ability can be ascribed to the presence of the outer porous layer. (C) 2004 Kluwer Academic Publishers.

Development of Ti-Mo alloys for biomedical applications: Microstructure and electrochemical characterization

Ti-Mo alloys from 4 to 20 Mo wt.% were arc-melted. Their compositions and surfaces were analyzed by EDX, XRF and SEM. The Mo mapping shows a homogeneous distribution for all alloys. The XRD analysis showed that the crystal structure of the alloys is sensitive to the Mo concentration; a mixture of the hexagonal alpha' and orthorhombic alpha '' phases was observed for the Ti-4Mo alloy, and the alpha '' phase is observed almost exclusively when the concentration of Mo added to the Ti reaches 6%. A significant retention of the beta phase is observed for the alloy containing 10% Mo, while at higher Mo concentrations (15% and 20%), retention of phase beta is only verified. Preliminary electrochemical studies have indicated a valve-metal behavior and good corrosion resistance in aerated Ringer solution for all alloys. (c) 2006 Published by Elsevier B.V.

Characterization of an all sol-gel electrochromic device WO3/Ormolyte/CeO2-TiO2

Electrochemical lithium intercalation in thin films of CeO2-TiO2 and WO3, prepared by the sol-gel technique was investigated with cyclic voltammetry and spectroelectrochemical techniques in propylene carbonate solutions. A solid state system having the configuration WO3/Ormolyte/CeO2-TiO2 has been assembled. The solid electrolyte, an organically modified electrolyte (ormolyte), was prepared with different [O]/[Li] ratios. The transmittance variation of this system during a potentiostatic step from -0.7 V to 0.8 V was about 35% at 550 nm.

An image processing method for morphology characterization and pitting corrosion evaluation

A digital image processing and analysis method has been developed to classify shape and evaluate size and morphology parameters of corrosion pits. This method seems to be effective to analyze surfaces with low or high degree of pitting formation. Theoretical geometry data have been compared against experimental data obtained for titanium and aluminum alloys subjected to different corrosion tests. (C) 2002 Elsevier B.V. B.V. All rights reserved.