Lead-cadmium oxyfluoride glasses and glass-ceramics

Glasses and glass-ceramics have been obtained in oxyfluoride systems involving lead and cadmium fluorides and one of the well-known glass former oxides SiO2, B2O3 and TeO2. Vitreous domains were established and a wide range of compositions including high heavy metal contents lead to stable glasses. Amorphous structures have been studied by short-range order spectroscopy techniques (Raman scattering and x-ray absorption) and molecular basic structures have been identified. Besides the usual oxides, the role of glass former could also be proposed for cadmium ions. Special attention has been paid for crystallization process. Cubic lead fluoride, cubic lead tellurite, tetragonal tellurium oxide and a solid solution of the type Pb1-xCdxF2 are obtained as crystallization products depending on the composition and temperature of heat treatments. Pb1-xCdxF2 solid solutions are well known superionic materials and obtaining this solid solution as a crystal phase could be very interesting for applications concerning ionic electrical conduction properties. The addition of rare earth ions led to the control of the crystallization process. In the presence of the nucleating ion only the cubic form beta-PbF2 was identified. Rare earth ions are present in the crystal phase and crystal-like spectroscopic properties were observed suggesting interesting applications for these perfectly transparent glass ceramics in photonics.

Molecular dynamics simulation on devitrification: Isothermal devitrification and thermodynamics of PbF2 glasses

The vitrification and devitrification features of lead fluoride are investigated by means of molecular dynamic simulations. The influence of heating rate on the devitrification temperature as well as the dependence of the glass properties on its thermal history, i.e., the cooling rate employed, is identified. As expected, different glasses are obtained when the cooling rates differ. Diffusion coefficient analysis during heating of glass and crystal, indicates that the presence of defects on the glassy matrix favors the transition processes from the ionic to a superionic state, with high mobility of fluorine atoms, responsible for the high anionic conduction of lead fluoride. Nonisothermal and isothermal devitrification processes are simulated in glasses obtained at different cooling rates and structural organizations occurring during the heat treatments are clearly observed. When a fast cooling rate is employed during the glass formation, the devitrification of a single crystal (limited by the cell dimensions) is observed, while the glass obtained with slower cooling rate, allowing relaxations and organization of various regions on the glass bulk during the cooling process, devitrifies in more than one crystalline plane. (C) 2004 American Institute of Physics.

THE INFLUENCE OF THE ELECTROCHEMICAL TREATMENT ON CU-AL-AG ALLOYS IN DEAERATED 0.5M NAOH

The effect of consecutive cyclic polarization in de-aerated 0.5 M NaOH solutions on the surface microstructure of mechanically polished Cu-Al-Ag alloys of different compositions and heat treatments has been studied using optical microscopy, SEM and EDS. The current peaks of the cyclic polarization curves do not depend on the alloy composition in the composition range studied. The repetitive potential scans between H2 and O2 evolution in alkaline media lead to preferential dissolution of aluminium, the roughness and phase composition of the surface of the alloys changing significantly. The quasistationary I-E curves of the different Cu-Al-Ag alloys studied consist in the superposition of the quasistationary I-E curves of high-purity Cu and Ag, the EDS microanalysis showing that aluminium is not present on the surface of the alloy in these conditions.

Aging behaviour of 25Cr-17Mn high nitrogen duplex stainless steel

The precipitation behaviour of a nickel free stainless steel containing 25% chromium, 17% manganese and 0.54% nitrogen, with duplex ferritic-austenitic microstructure, was studied using several complementary techniques of microstructural analysis after aging heat treatments between 600 and 1 000 degrees C for periods of lime between 15 and 6 000 min. During aging heat treatments, ferrite was decomposed into sigma phase and austenite by a eutectoid reaction, like in the Fe-Cr-Ni duplex stainless steel. Chromium nitride precipitation occurred in austenite, which had a high nitrogen supersaturation. Some peculiar aspects were observed in this austenite during its phase transformations. Chromium nitride precipitation occurred discontinuously in a lamellar morphology, such as pearlite in carbon steels. This kind of precipitation is not an ordinary observation in duplex stainless steels and the high levels of nitrogen in austenite can induce this type of precipitation, which has not been previously reported in duplex stainless steels. After chromium nitride precipitation in austenite, it was also observed sigma phase formation near the cells or colonies of discontinuously precipitated chromium nitride. Sigma phase formation was made possible by the depletion of nitrogen in those regions. Time-temperature-transformation (precipitation) diagrams were determined.

Study of electrical, chemical and structural characteristics of superconductor thin film obtained by polymeric precursors method

Superconductor films of the BSCCO system have been grown by dip coating technique with good success. The chemical method allows us to grow high temperature superconductor thin films to get better control of stoichiometry, large areas and is cheaper than other methods. There is a great technological interest in growth oriented superconductor films due anisotropic characteristics of superconductor materials of high critical temperature, specifically the cuprates, as we know that the orientation may increase the electrical transport properties. Based on this, the polymeric precursor method has been used to obtain thin films of the BSCCO system. In this work we have applied that method together with the deposition technique known as dip coating to obtain Bi-based superconductor thin films, specifically, Bi1.6Pb0.4Sr2.0C2.0Cu3.0Ox+8, also known as 2223 phase with a critical temperature around 110 K. The films with multilayers have been grown on crystalline substrates of LaAlO3 and orientated (100) after being heat treated around 790 degrees C - 820 degrees C in lapse time of 1 hour in a controlled atmosphere. XRD measurements have shown the presence of a crystalline phase 2212 with a critical temperature around 85 K with (001) orientation, as well as a small fraction of 2223 phase. SEM has shown a low uniformity and some cracks that maybe related to the applied heat treatment. WDS has also been used to study the films composition. Different heat treatments have been used with the aim to increase the percentage of 2223 phase. Measurements of resistivity confirmed the presence of at least two crystalline phases, 2212 and 2223, with T-c around 85 K and 110 K, respectively.

Luminescence and ESR properties of Brazilian feldspars

The IRSL and TL responses of three different feldspar crystals have been analysed. TL measurements were taken in the ultraviolet UV (290-370 nm) and the visible VIS (340-610 nm) regions of the spectrum. For the UV region and for a natural sample, peaks were observed at 283, 287 and 310 degrees C for grey, white and pink crystals, respectively. For samples irradiated after prior preheating, it was noted that TL peaks occurred at about 200 degrees C for all the samples; irradiation with high doses above 500 Gy induced the formation of one additional peak at 170 degrees C. The VIS region results were similar to those for the UV. ESR experiments have been developed to verify the influence of radiation and heat treatments on the centres and preliminary results showed great variation in the intensities of [TiO(4)](-), Al-O(-)-Al and Fe(3+) centres. (c) 2006 Elsevier Ltd. All rights reserved.

Effect of heated solutions on decay control and residues of imazalil in lemons

Freshly harvested lemons [(Citrus limon (L.) Burm)] were dipped 3 min in water with and without imazalil (IMZ) at 50, 100, and 200 ppm at 50 degrees C and at 1000 ppm IMZ at 20 degrees C. Following treatments fruit were kept at 9 degrees C and 90%-95% relative humidity (RH) for 13 weeks and an additional week at 21 degrees C and ca. 75% RH, to simulate a marketing period (SMP). No decay control was observed with fruit dipped in water at 50 degrees C. In contrast, IMZ treatments provided 90%-96% control of Penicillium rots during cold storage and SMP. Fungi other than Penicillium spp. were also found in all samples as differences among treatments were negligible. IMZ treatment caused some external damage to the fruit (peel browning), and the percentage of damaged fruit was related to the amount of active ingredient (AI) present in it. Dipping in 200 or 1000 ppm IMZ promoted off-flavor development after 10 weeks of storage, and fruit were judged to be unacceptable for consumption after 13 weeks of cold storage. After 1000 ppm IMZ dipping at 20 degrees C, residue concentration in fruit was 8.20 ppm; this value doubled that found in a previous investigation on lemons treated with comparable IMZ levels. Residue concentrations in fruit after treatment at 50 degrees C was strictly related to the amount of fungicide employed. After 13 weeks Al residues in fruit decreased to average ca. 35% of the initial values. During the 1 week SMP, residue levels decreased by a further ca. 25%. It was concluded that it is possible to achieve significant control of decay in lemons during longterm storage by dipping fruit in 50 ppm IMZ mixtures at 50 degrees C. Such treatment should be advised to remarkably reduce potential pollution in the environment due to packinghouse wastewater disposal.

Sol-gel Eu3+/Tm3+ doped transparent glass-ceramic waveguides

Eu3+ and Tm3+ doped lanthanum fluoride and lanthanum oxyfluoride are obtained from Eu3+, Tm3+ containing lanthanum fluoracetate solutions. The nature of the crystal phase obtained could be controlled by the temperature of heat treatment. Spectral characteristics of Eu3+ doped crystal phases were sufficiently different to allow utilization of Eu3+ as structural probes. Tm3+ emission at the technologically important spectral region of 1450nm could be observed for the fluoride and oxyfluoride crystal phases. The large bandwidth obtained (around 120nm) suggests potential applications in optical amplification. SiO2-LaF3-LaOF composite materials were also prepared. It is observed that for heat treatments above 800degreesC, fluorine loss, probably in the form of SiF4 hinder the observation of Tm3+ emission. Eu3+ spectroscopic characteristics clearly show the evolution of a fluoride like environment to an amorphous oxide one as the temperature of heat treatment increased. Thin films obtained by dip-coating on V-SiO2 substrates and treated at 300degreesC, 500degreesC and 800degreesC display guided modes in the visible and infrared regions. Optical characteristics (refractive index and films thickness) were obtained at 543.5, 632.8 and 1550nm. Attenuation as low as 1.8dB/cm was measured at 632.8nm. (C) 2004 Published by Elsevier B.V.

Structural and spectroscopic study of oxyfluoride glasses and glass-ceramics using europium ion as a structural probe

Transparent oxyfluoride glasses and beta-PbF(2) nanocrystals containing glass-ceramics were prepared with varying Eu(3+) content (0.3, 0.4, 0.5 and 0.6%). The effect of Eu(3+) content on the preparation of glass-ceramics was investigated. From differential scanning calorimetry, the T(x)-T(g)(T(x)-temperature of the onset of crystallization; T(g)-glass transition temperature) parameter for glasses has shown slight variation, and an exothermic peak near T(g) called the ceramization temperature (T(c)) has been observed. Heat treatments were performed at this temperature to obtain transparent glass-ceramics containing beta-PbF(2) nanocrystals, identified by x-ray diffraction. Heat treatments for different periods of time were performed and were observed to be very important in the control of the crystal size and of the crystallization rate. Based upon the absorption spectra, the scattering level due to the presence of beta-PbF(2) nanocrystals in the glass-ceramics was observed to be similar to that for the mother glasses. Detailed analysis of emission spectra and decay time measurements led to the identification of Eu(3+) ions as the beta-PbF(2) crystalline phase. Excitation spectra at 70 K show the interaction of Eu(3+) ions with the fluorogermanate network.

Optimization of the mechanical properties of low-carbon steels by formation of a multiphase microstructure

In this work five methods of heat treatments are investigated in order to obtained convenient volume fractions of ferrite, bainite, martensite and retained austenite, starting with a low carbon steel and seeking the distinction of the phases, through optical microscopy. Specific chemical etching is improved. The results in tensile and fatigue tests were accomplished and the results were related with the microstructural parameters. The results show that the mechanical properties are closely related with the phases, grains size and the phases morphology. Copyright © 2001 Society of Automotive Engineers, Inc.

Otimização das propriedades mecânicas por meio de modificações microestruturais em aços de baixo carbono

This paper discusses the formation of microstructures with different volume fractions, as an outcome of a specific heat treatment, with the following phases: ferrite, martensite, bainite and retained austenite. For the microstructure characterization it is developed a chemical etching that allows to distinguish the phases by optical microscopy. The evaluation of the mechanical properties is done based on the results of tensile and fatigue tests. The experimental results show that appropriate heat treatments can contribute to a significant improvement in the mechanical properties of the steel. In this process it is essential to control the fraction volume, morphology of the phases, and grain size.

Metal-insulator transition in Nd1-xEuxNiO 3 compounds

Polycrystalline Nd1-xEuxNiO3 (0≤x≤0.5) compounds were synthesized in order to investigate the character of the metal-insulator (MI) phase transition in this series. Samples were prepared through the sol-gel route and subjected to heat treatments at ∼1000 °C under oxygen pressures as high as 80bar. X-ray diffraction (XRD) and neutron powder diffraction (NPD), electrical resistivity ρ(T), and magnetization M(T) measurements were performed on these compounds. The NPD and XRD results indicated that the samples crystallize in an orthorhombic distorted perovskite structure, space group Pbnm. The analysis of the structural parameters revealed a sudden and small expansion of ∼0.2% of the unit cell volume when electronic localization occurs. This expansion was attributed to a small increase of ∼0.003 of the average Ni-O distance and a simultaneous decrease of ∼-0.5° of the Ni-O-Ni superexchange angle. The ρ(T) measurements revealed a MI transition occurring at temperatures ranging from TMI∼193 to 336K for samples with x ≤ 0 and 0.50, respectively. These measurements also show a large thermal hysteresis in NdNiO3 during heating and cooling processes, suggesting a first-order character of the phase transition at TMI. The width of this thermal hysteresis was found to decrease appreciably for the sample Nd 0.7Eu0.3NiO3. The results indicate that cation disorder associated with increasing substitution of Nd by Eu is responsible for changing the first-order character of the transition in NdNiO3. © 2006 IOP Publishing Ltd.

Heating rate and temperature effects on the BaTiO3 formation by thermal decomposition of (Ba,Ti) organic precursors during the Pechini process

Different thermal treatments for the synthesis of BaTiO3 powder obtained through the Pechini method were studied. The synthesis of BaTiO3 starts at 150 °C by the thermal dehydration of organic precursors. The usual inevitable formation of barium carbonate during the thermal decomposition of the precursor could be retarded at lower calcination temperatures and optimized heating rates. The organic precursors were treated at temperatures between 200 and 400 °C. Then, the samples were calcined at 700 and 800 °C for 4 and 2 h, respectively. The resulting ceramic powders were characterized by gravimetric and differential thermal analyses, X-ray powder diffraction and infrared spectroscopy. It was found that depending on the heating rate and final temperature of the thermal treatment, high amounts of BaCO3 and TiO2 could be present due to the high concentration of organics in the final calcination step. © 2007 Elsevier B.V. All rights reserved.

Efeito da temperatura e tempo de austenitização nas transformações de fase da liga 13Cr2Ni0,1C

New classes of martensitic stainless steels, with low carbon levels, have been developed aiming to meet the needs of the petroleum industry segment. However, their use has been restricted due to the fact it is a recent development and many of its properties are still under investigation. This work determines the values of initial and final temperatures for the austenitic transformation and the initial and final temperatures of martensitic formation for alloy 13Cr2Ni0,1C, by means of dilatometric tests under continuous cooling. Based on these results the optimized conditions for quench and temper heat treatments were obtained. The microstructural characterization of the alloys under coarse fusion condition was carried out by optical microscopy and the presence of delta-ferrite in the martensitic matrix was observed.

Microstructural effects on fatigue crack growth behavior of a microalloyed steel

Thermal transformations on microalloyed steels can produce multiphase microstructures with different amounts of ferrite, martensite, bainite and retained austenite. These different phases, with distinct morphologies, are determinant of the mechanical behavior of the steel and can, for instance, affect the crack path or promote crack shielding, thus resulting in changes on its propagation rate under cyclic loading. The aim of the present work is to evaluate the effects of microstructure on the tensile strength and fatigue crack growth (FCG) behaviour of a 0.08%C-1,5%Mn (wt. pct.) microalloyed steel, recently developed by a Brazilian steel maker under the designation of RD480. This steel is being considered as a promising alternative to replace low carbon steel in wheel components for the automotive industry. Various microstructural conditions were obtained by means of heat treatments followed by water quench, in which the material samples were kept at the temperatures of 800, 950 and 1200 °C. In order to describe the FCG behavior, two models were tested: the conventional Paris equation and a new exponential equation developed for materials showing non-linear FCG behavior. The results allowed correlating the tensile properties and crack growth resistance to the microstructural features. It is also shown that the Region II FCG curves of the dual and multiphase microstructural conditions present crack growth transitions that are better modeled by dividing them in two parts. The fracture surfaces of the fatigued samples were observed via scanning electron microscopy in order to reveal the fracture mechanisms presented by the various material conditions. © 2010 Published by Elsevier Ltd.