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Materials Research, Volume: 9, Número: 4, Publicado: 2006
  • Materials Research: Ibero-american Journal of Materials

  • Simulation of the solidification of pure nickel via the phase-field method Regular Articles

    Ferreira, Alexandre Furtado; Silva, Alexandre José da; Castro, José Adilson de

    Resumo em Inglês:

    The Phase-Field method was applied to simulate the solidification of pure nickel dendrites and the results compared with those predicted by the solidification theory and with experimental data reported in the literature. The model's behavior was tested with respect to some initial and boundary conditions. For an initial condition without supercooling, the smooth interface of the solid phase nucleated at the edges of the domain grew uniformly into the liquid region, without branching. In an initially supercooled melt, the interface became unstable under 260 K supercooling, generating ramifications into the liquid region. The phase-field results for dendrite tip velocity were close to experimental results reported in the literature for supercooling above 50 K, but they failed to describe correctly the nonlinear behavior predicted by the collision-limited growth theory and confirmed by experimental data for low supercooling levels.
  • NewIn-situ synthesis method of magnesium matrix composites reinforced with TiC particulates Regular Articles

    Xiuqing, Zhang; Lihua, Liao; Naiheng, Ma; Haowei, Wang

    Resumo em Inglês:

    Magnesium matrix composites reinforced with TiC particulates was prepared using a new in-situ synthesis method of remelting and dilution technique. And measurements were performed on the composites. The results of x ray diffraction (XRD) analysis confirmed that TiC particulates were synthesized during the sintering process, and they retained in magnesium matrix composites after the remelting and dilution processing. From the microstructure characterization and electron probe microanalysis (EPMA), we could see that fine TiC particulates distributed uniformly in the matrix material.
  • Characteristics of the double-torsion test to determine the R-curve of ceramic materials Regular Articles

    Albuquerque, Maria da Consolação Fonseca de; Rodrigues, José de Anchieta

    Resumo em Inglês:

    Double-torsion tests were carried out on a commercial ceramic floor tile to verify whether this test is suitable for determining the R-curve of ceramics. The instantaneous crack length was obtained by means of compliance calibration, and it was found that the experimental compliance underestimates the real crack length. The load vs. displacement curves were also found to drop after maximum loading, causing the stress intensity factor to decline. The R-curves were calculated by two methods: linear elastic fracture mechanics and the energetic method. It was obtained that the average values of crack resistance, R, and the double of the work of fracture, 2 <FONT FACE=Symbol>× g</FONT>wof, did not depend on notch length, a0, which is a highly relevant finding, indicating that these parameters were less dependent on the test specimen's geometry. The proposal was to use small notches, which produce long stable crack propagation paths that in turn are particularly important in the case of coarse microstructures.
  • Evaluation via multivariate techniques of scale factor variability in the rietveld method applied to quantitative phase analysis with X ray powder diffraction Regular Articles

    Oliveira, Terezinha Ferreira de; Avillez, Roberto Ribeiro de; Epprecht, Eugenio Kahn; Queiroz, Joaquim Carlos Barbosa

    Resumo em Inglês:

    The present work uses multivariate statistical analysis as a form of establishing the main sources of error in the Quantitative Phase Analysis (QPA) using the Rietveld method. The quantitative determination of crystalline phases using x ray powder diffraction is a complex measurement process whose results are influenced by several factors. Ternary mixtures of Al2O3, MgO and NiO were prepared under controlled conditions and the diffractions were obtained using the Bragg-Brentano geometric arrangement. It was possible to establish four sources of critical variations: the experimental absorption and the scale factor of NiO, which is the phase with the greatest linear absorption coefficient of the ternary mixture; the instrumental characteristics represented by mechanical errors of the goniometer and sample displacement; the other two phases (Al2O3 and MgO); and the temperature and relative humidity of the air in the laboratory. The error sources excessively impair the QPA with the Rietveld method. Therefore it becomes necessary to control them during the measurement procedure.
  • Effect of rare earth oxide additions on oxidation behavior of AISI 304L stainless steel Regular Articles

    Pillis, Marina Fuser; Araújo, Edval Gonçalves de; Ramanathan, Lalgudi Venkataraman

    Resumo em Inglês:

    AISI 304L stainless steel powder compacts containing 2 vol% high purity rare earth oxides were prepared by mixing the different powders in a vibratory mill followed by pressing. The compacts thus obtained were sintered in a vacuum furnace and isothermal oxidation measurements were carried out in a muffle furnace, in air, up to 200 hours at 900 °C. The oxidized surfaces were examined in a scanning electron microscope and micro regions of the reaction products were studied using energy dispersive analysis. The addition of rare earth oxides decreased the oxidation rate of the stainless steel. Further evidence of predominant oxygen ion diffusion controlling the overall oxidation process in rare earth containing chromium oxide forming alloys has been observed.
  • Production of selective membranes using plasma deposited nanochanneled thin films Regular Articles

    Carvalho, Rodrigo Amorim Motta; Carvalho, Alexsander Tressino de; Silva, Maria Lúcia Pereira da; Demarquette, Nicole Raymond

    Resumo em Inglês:

    The hydrolization of thin films obtained by tetraethoxysilane plasma polymerization results in the formation of a nanochanneled silicone like structure that could be useful for the production of selective membranes. Therefore, the aim of this work is to test the permeation properties of hydrolyzed thin films. The films were tested for: 1) permeation of polar organic compounds and/or water in gaseous phase and 2) permeation of salt in liquid phase. The efficiency of permeation was tested using a quartz crystal microbalance (QCM) technique in gas phase and conductimetric analysis (CA) in liquid phase. The substrates used were: silicon for characterization of the deposited films, piezoelectric quartz crystals for tests of selective membranes and cellophane paper for tests of permeation. QCM analysis showed that the nanochannels allow the adsorption and/or permeation of polar organic compounds, such as acetone and 2-propanol, and water. CA showed that the films allow salt permeation after an inhibition time needed for hydrolysis of the organic radicals within the film. Due to their characteristics, the films can be used for grains protection against microorganism proliferation during storage without preventing germination.
  • Electrochemical behavior of Ti and Ti6Al4V in aqueous solutions of citric acid containing halides Regular Articles

    Schmidt, Anelise Marlene; Azambuja, Denise Schermann

    Resumo em Inglês:

    This paper reports on an investigation of the electrochemical behavior of Ti grade 2 and Ti6Al4V alloy in aqueous citric acid solutions with pH 2.0 containing halide ions. Voltammetric studies of Ti and the alloy in citric acid, with and without chloride ions, indicate that the Ti and Ti alloy presented a passive behavior in the test solutions used. Pitting was observed at 3.0 and 2.5 V/SCE for Ti and Ti6Al4V, respectively, when bromide ions were added to the solution. In solutions containing fluoride ions, dissolution of the film occurred at potentials close to - 1.0 V/SCE in both electrodes. The iodide ions oxidized on the passive oxide film at potentials close to 1.0 V/SCE. EIS results of the materials in citric acid solutions containing chloride ions revealed that the film's resistance increased as the applied potential rose from 0 to 1.0 V. In bromide-containing solutions, breakdown of the film was confirmed at potentials above 2.0 V/SCE in both electrodes. These results suggest film reformation for Ti and the alloy in solutions containing fluoride at potentials within the passive region.
  • High temperature oxidation behavior of AISI 304 and AISI 430 stainless steels Regular Articles

    Carvalho, Carlos Eduardo Reis de; Costa, Geraldo Magela da; Cota, André Barros; Rossi, Edson Hugo

    Resumo em Inglês:

    The oxidation behavior of AISI 304 and AISI 430 stainless steels was investigated from 1100 °C up to 1200 °C. Mössbauer spectroscopy and x ray diffraction were used to access the phase composition of the formed scales. The main crystalline phases found in the oxidized materials at temperatures above 1100 °C were hematite and magnetite for AISI 430 steel, and hematite and a spinel-like phase for AISI 304 steel. Hematite was found to be the dominant oxide at lower temperatures, whereas magnetite preferentially forms at higher temperatures. The activation energy for oxidation is smaller for AISI 430 steel in relation to AISI 304 steel in the range of studied temperatures, and therefore the AISI 430 steel is less resistant towards oxidation at high temperatures.
  • Development and characterization of 5% mol Zn bioceramic in granular form Regular Articles

    Lima, Ingrid Russoni de; Costa, Andrea Machado; Bastos, Ivan Napoleão; Granjeiro, José Mauro; Soares, Gloria de Almeida

    Resumo em Inglês:

    Hydroxyapatite (HA) is capable of accepting substitute ions within its lattice, including zinc ions. Zinc is a trace element that activates the osteogenesis of osteoblastic cells and therefore plays an important role in the activity of alkaline phosphatase enzyme. The purpose of this work was to produce and characterize 5% mol Zn bioceramic in granular form (Zn-granules) for clinical applications and compare it with granules made from HA by using the same production route. Granules with addition of porogen agents were produced from powders of HA and zinc-containing HA by uniaxial pressing and heat treatment. The granules were subsequently ground and sieved. The results indicated that zinc contributed to the reduction of sample crystallinity and formed a biphasic structure after calcination at 1200 °C. Additionally, zinc release from granular material may have clinical applications as bone graft.
  • Initial rheological description of high performance concretes Regular Articles

    Castro, Alessandra Lorenzetti de; Liborio, Jefferson Benedicto Libardi

    Resumo em Inglês:

    Concrete is defined as a composite material and, in rheological terms, it can be understood as a concentrated suspension of solid particles (aggregates) in a viscous liquid (cement paste). On a macroscopic scale, concrete flows as a liquid. It is known that the rheological behavior of the concrete is close to that of a Bingham fluid and two rheological parameters regarding its description are needed: yield stress and plastic viscosity. The aim of this paper is to present the initial rheological description of high performance concretes using the modified slump test. According to the results, an increase of yield stress was observed over time, while a slight variation in plastic viscosity was noticed. The incorporation of silica fume showed changes in the rheological properties of fresh concrete. The behavior of these materials also varied with the mixing procedure employed in their production. The addition of superplasticizer meant that there was a large reduction in the mixture's yield stress, while plastic viscosity remained practically constant.
  • Computer simulation of the mechanism for the synthesis of carbonado diamond Regular Articles

    Rangel, João José de Assis; Rosenthal, Ruben; Bobrovnitchii, Guerold Sergueevitch; Monteiro, Sergio Neves

    Resumo em Inglês:

    The synthesis mechanism associated with the formation of carbonado type polycrystalline diamond has been analyzed. This analysis was performed by computer simulation of the field of temperature developed at the moment of graphite transformation into polycrystalline diamond. It was found that during the synthesis of this carbonado diamond, a strong non-steady thermal condition occurs, leading to changes in the thermodynamic equilibrium. As a consequence, a region comprising non-transformed graphite and carbonado with different characteristics is established. An experimental comparison was carried out between the carbonado hardness profile and the field of temperatures. The results show that the higher the temperature attained at local points inside the high-pressure chamber, the higher the hardness of the diamond. The simulation and experimental results indicated that concurrent mechanisms are acting during the carbonado synthesis.
  • In Vitro studies of bioactive glass/polyhydroxybutyrate composites Regular Articles

    Paiva, André Oliveira; Duarte, Maria Gabriela; Fernandes, Maria Helena Vaz; Gil, Maria Helena; Costa, Necésio Gomes

    Resumo em Inglês:

    Bioactive materials can help bone reparation and regeneration by offering support to bone growth. In vitro studies of bioactive glass/polyhydroxybutyrate composites were carried out to evaluate the influence of the composition on the bioactivity through the presence of calcium phosphate (Ca-P) on the layer formed when the substrates were immerse in simulated body fluid (SBF). The in vitro tests were carried out by soaking the composites bioactive glass/polyhydroxybutyrate 30/70 and 40/60 in SBF. The surface of the composites was analyzed by Scanning Electron Microscopy (SEM) with Energy Dispersive Spectroscopy (EDS) and also via x ray Diffraction (XRD). The solutions were analyzed by Inductively Couple Plasma (ICP). SEM images show a formation of a Ca-P rich layer on surface of composites. XRD results characterized the layer as calcium hydrogen phosphate. Ca/P ratios found via EDS results show a value close to 1.67. According to ICP results, the Ca e P ions are from SBF.
  • The effect of hydrogen peroxide on the electrochemical behaviour of Ti-13Nb-13Zr alloy in Hanks' solution Regular Articles

    Assis, Sérgio Luiz de; Costa, Isolda

    Resumo em Inglês:

    Titanium alloys are largely used for biomedical applications mainly due to their high corrosion resistance resulting from the protective oxide film formed on their surface. The literature, however, has pointed out discrepancies between in vitro tests and in vivo tests. These discrepancies have been ascribed to hydrogen peroxide (H2O2) generated by inflammatory reactions. In this investigation the electrochemical behaviour of a Ti-13Nb-13Zr alloy, which was developed as material for implants, has been evaluated in Hanks' solution, with and without H2O2. The evolution of the electrochemical behavior was monitored by electrochemical impedance spectroscopy (EIS) and the results were fitted to an equivalent circuit that simulates an oxide film as a duplex layer structure composed of an inner barrier layer and an outer porous layer. In the solution without H2O2, the oxide film was very stable during the whole test period. On the other hand, in the solution with H2O2, the EIS results varied significantly, indicating a progressive decrease in the barrier layer resistance until 35 days which was followed by the restoration of the barrier layer protective characteristics against corrosion, either due to its growth or to its self-healing after partial consumption of the oxidant agent. The oxide film formed on the Ti alloy samples after 125 days of immersion in Hanks' solution, either with or without H2O2 was analyzed by XPS. The XPS results revealed the presence of TiO and TiO2 on the samples immersed in the two electrolytes, however, Ti2O3 was only found on the samples exposed to the H2O2 containing solution.
  • Determination of the oxygen and nitrogen interstitial diffusion coeficient in niobium by mechanical spectroscopy Regular Articles

    Florêncio, Odila; Silva Jr., Paulo Sergio da; Stefanini, Thais França; Grandini, Carlos Roberto

    Resumo em Inglês:

    Mechanical spectroscopy measurements have been extensively used in the last decades to obtain information about many aspects of the behavior of solutes in metallic materials. Metals of body-centered cubic lattice that contain heavy interstitial elements (oxygen, nitrogen and carbon) in solid solution, present anelastic relaxation peaks when submitted to cyclic tensions, due to process know stress-induced ordering. Internal friction and frequency as a function of temperature were performed between 300 K and 650 K in a polycrystalline sample of Nb, for three distinct conditions, using a torsion pendulum inverted Kê-type operating in a frequency oscillation between 1Hz and 10 Hz range, with a heating rate of 1 K/min and pressure lower than 2 x 10-5 mbar. The experimental spectra obtained for each condition of the sample, were decomposed by the successive subtraction method in elementary Debye peaks. The following metal-interstitial interactions were identified: Nb-O and Nb-N for all conditions of the sample. From the anelastic relaxation parameters obtained (relaxation strength, peak temperature, activation energy and relaxation time) and lattice parameter (obtained from x ray diffraction), the determination of the oxygen and nitrogen interstitial diffusion coefficient in Nb was possible, for each condition of the sample.
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