Advanced Powder Technology V

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Authors: Leszek Adam Dobrzański, J. Mikuła, Klaudiusz Gołombek
Abstract: Within the project framework the structure and properties was investigated of the cemented carbides, cermets and oxide ceramics using the scanning electron microscope (SEM). The X-ray qualitative microanalysis and surface distribution analysis of elements in the investigated materials were made using the EDS X-ray energy dispersive radiation spectrometer. The roughness measurements of the developed materials were made in two orthogonal directions. The Ra parameter was assumed to be the value describing surface roughness. The microhardness tests using the Vickers method were made on the dynamic ultra microhardness tester. The measurements were made in the „load - unload” mode.
Authors: Wilton Silva Lopes, Crislene Rodrigues da Silva Morais, A.G. de Souza
Abstract: In this work the kinetics of the thermal decomposition of two ß-diketone lanthanide complexes of the general formula Ln(thd)3phen (where Ln = Nd+3 or Tm+3, thd = 2,2,6,6- tetramethyl-3,5-heptanodione and phen = 1,10-phenantroline) has been studied. The powders were characterized by several techniques. Thermal decomposition of the complexes was studied by non-isothermal thermogravimetry techniques. The kinetic model that best describes the process of the thermal decomposition of the complexes it was determined through the method proposed by Coats-Redfern. The average values the activation energy obtained were 136 and 114 kJ.mol-1 for the complexes Nd(thd)3phen and Tm(thd)3phen, respectively. The kinetic models that best described the thermal decomposition reaction the both complexes were R2. The model R2 indicating that the mechanism is controlled by phase-boundary reaction (cylindrical symmetry) and is defined by the function g(α) = 2[1-(1-a)1/2], indicating a mean reaction order. The values of activation energy suggests the following decreasing order of stability: Nd(thd)3phen > Tm(thd)3phen.
Authors: Wilton Silva Lopes, Crislene Rodrigues da Silva Morais, A.G. de Souza
Abstract: Recently, highly luminescent lanthanide complexes with mixed ligands such as and β-diketone and two herobiaryl ligands have been synthesized and suggested as promising light-conversion molecular devices as described by several authors. The synthesis, luminescence, quantum yields, spectroscopic characteristics, structure, among others properties of these complexes, including the possibility of production thin film films from these materials have been discussed, but little is known about their thermal decomposition kinetics. In this work we report the determination of kinetic parameters of thermal decomposition of the complexes Gd(thd)3phen and Er(thd)3phen (thd=2,2,6,6-tetramethyl-3,5- heptanodione; phen=1,10-phenantroline) using the method proposed by Ozawa (1965). The kinetic parameters obtained for activation energy were: 90 and 87 kJ.mol-1, the values of frequency factor were: 2.3x107 and 2.0x107 s-1 for Gd(thd)3phen and Er(thd)3phen, respectively. On the kinetic energy of the complexes, we notice the following order in thermal stability: Gd(thd)3phen < Er(thd)3phen.
Authors: R.A. Rocha, E.N.S. Muccillo
Abstract: High ionic conductivity ceramics have potential technological applications in chemical sensors, ceramic permeable membranes, oxygen pumps, and solid oxide fuel cells. Recently ionic conductivity values as high as those of doped zirconia solid solutions have been found in a lanthanum molybdate compound. The high ionic conductivity of this compound, La2Mo2O9, is obtained at temperatures above the structural phase transition temperature (~580 °C). In this work the La2Mo2O9 ceramic material was prepared by the polymeric precursor technique and sintered at several dwell temperatures and soaking times to study the effect of sintering conditions on phase transition. It was found that there is a strong dependence of phase transition on the sintering profile. At 950 °C the phase transition is suppressed for short soaking times, whereas it is observed to occur for longer times. Moreover, the relative magnitude of conductivity is also dependent on the sintering conditions. The main conclusion is that the phase transition in La2Mo2O9 is particle sizedependent.
Authors: Claudinei dos Santos, L.H.P. Teixeira, J.K.M.F. Daguano, Kurt Strecker, Carlos Nelson Elias
Abstract: In this work the influence of isothermal sintering time on the microstructural development of ZrO2-Al2O3 composite was studied. Powder mixture of ZrO2 containing 20 wt% Al2O3 was prepared by milling, compaction and sintering at 16000C, in air. The isothermal sintering time at 16000C was varied between 0 and 1440 min. The sintered samples were characterized in terms of phase composition and relative density. Their microstructures were characterized by grain size distributions and average grain size. These results were evaluated using the classic grain growth equation as a function of time, determining the grain growth exponent of these materials. Furthermore, the microstructural aspects were related to the mechanical properties (Vicker’s hardness and fracture toughness) of these composites.
Authors: Kurt Strecker, Claudinei dos Santos, M.J. Bondioli, Michael J. Hoffmann
Abstract: In this work, SiC ceramics were prepared by liquid phase sintering using 10 wt.% of AlN and Y2O3 mixtures in the proportion of 4:1 and 2:3 as additives Sintering was done in a graphite resistance heated furnace at 2080oC under 0.2 MPa N2 atmosphere for 1h. Part of the samples was further heat-treated at 2000oC for 4h to allow grain growth. The microstructures of the sintered samples were analyzed using polished and plasma etched surfaces. Furthermore, relative densities, weight loss during sintering and SiC-polytype distributions are reported.
Authors: Monica Castoldi Borlini Gadioli, J.L.C.C. Mendonça, R.A. Conte, Daltro Garcia Pinatti, Carlos Maurício Fontes Vieira, Sérgio Neves Monteiro
Abstract: The influence of the particle size of an ash from sugarcane bagasse on the properties of incorporated red ceramics was investigated. Mixtures of kaolinitic clay from the municipal area of Campos of Goytacazes-RJ were prepared with additions of 0, 5 and 10% in weight of ashes from sugarcane bagasse. Ashes with different particle sizes lower than 149 μm (100 mesh), 75 μm (200 mesh) and 44 μm (325 mesh), were used in each incorporated composition. Specimens were 20 MPa uniaxially press-molded and sintered at 900 and 1050°C. The firing technological properties evaluated were diametrical shrinkage, water absorption and mechanical strength by diametrical compression. The results showed that the ash incorporation caused significant changes in the ceramic properties.
Authors: P.M. Andrade, Carlos Maurício Fontes Vieira, Sérgio Neves Monteiro, F. Vernilli Jr.
Abstract: The present paper has for objective to evaluate the effect of fine steel sludge waste incorporation on the properties and microstructure of a kaolinitic clayey body used to the fabrication of bricks and roofing tiles. Compositions were prepared with additions of waste of 0, 5 and 10 wt.% in a kaolinitic clay from the county of Campos dos Goytacazes, State of Rio de Janeiro, Brazil. To determine the technological properties such as bulk density, linear shrinkage, water absorption and flexural strength, specimens were prepared by uniaxial pressure at 20 MPa and then fired in a laboratory furnace at 700°C, 900°C and 1100°C. The microstructure of the fired specimen was evaluated by SEM. The results showed that the incorporation up to 10 wt. % of fine steel sludge does not change the ceramic properties, specially, at low temperatures. Hence, the recycling of steel sludge into red ceramic fabrication can be considered as an environmentally correct solution for the final disposal of this type of waste.
Authors: Juliana Maria de Albuquerque Gimenez, Carlos Roberto Grandini, M.S. Góes, A.R. Jurelo, R. Dobrzanski
Abstract: The discovery of the spatial uniform coexistence of superconductivity and ferromagnetism in rutheno-cuprates, RuSr2GdCu2O8 (Ru-1212), has spurred an extraordinary development in the study of the competition between magnetism and superconductivity. However, several points of their preparation process and characterization that determine their superconductive behavior are still obscure. The improvement of sample preparation conditions involves some thermal treatments in inert atmosphere. The first treatment results in the immediate formation of Sr2GdRuO6. Using the CuO composition as a precursor, we produced Ru-1212. To turn it metallic and superconductor, besides the previous treatment, a final sinterization is carried out in oxygen flow for several days. Three Ru-1212 samples were produced by varying the last sinterization time (two, four, and six days under oxygen flow). Through measurements of x-ray diffraction, scanning electron microscopy, differential thermal analysis, magnetic susceptibility and mechanical spectroscopy, it was studied the influence of the treatments under oxygen atmosphere on the structural and superconducting properties of the material.
Authors: Rubens Maribondo Nascimento, Juliana Maria de Albuquerque Gimenez, Carlos Roberto Grandini, Alfredo Gonçalves da Cunha
Abstract: The composite SmBa2Cu3O7-δ (Sm-123), obtained by the substitution of the ion Y for Sm in the very well known and studied YBa2Cu3O7-δ (Y-123), is potentially attractive for better understanding superconductivity mechanisms and for its applications as electronic devices. Sm-123 samples show higher critical temperatures than Y-123 ones do and a larger solubility of Sm in Ba-Cu-O solvent, which makes their growth process faster. When oxygen is present interstitially, it strongly affects the physical properties of the material. The dynamics of oxygen can be investigated by anelastic spectroscopy measurements, a powerful technique for the precise determination of the oscillation frequency and the internal friction when atomic jumps are possible. Anelastic spectroscopy allows determining the elasticity modulus (related to the oscillation frequency) and the elastic energy loss (related to the internal friction) as a function of the temperature. The sample was also investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), and electric resistivity. The results obtained show a thermally activated relaxation structure composed by at least 3 relaxation processes. These processes may be attributed to the jumps of oxygen atoms present of the Cu-O plane in the orthorhombic phase.

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