Mulita com composição 1,4 Al2O3.SiO2 foi sintetizada a partir de α-alumina comercial (Alfa Cesar Company) e de sílica obtida da calcinação da casca de arroz. Essa sílica possui alta área superficial, alta pureza e pequeno diâmetro médio de partícula. Pós de sílica e de alumina foram misturados na proporção estequiométrica 3Al2O3-2SiO2 correspondente a 71,8 % em peso de Al2O3 e 26,2 % em peso de SiO2, homogeneizados em moinho de disco orbital de alumina antes e após a calcinação a 1100ºC, durante 4 h, ao ar. Em seguida, os pós foram prensados uniaxialmente sob uma pressão de 1200 MPa. Os corpos verdes foram sinterizados a 1650ºC, por 4 h, ao ar. As densidades dos corpos sinterizados foram determinadas pelo método hidrostático. As caracterizações química e estrutural foram realizadas por ICP, DRX e MAS RMN de 29Si, respectivamente, e a análise microestrutural por MEV. Os resultados obtidos mostram que é possível sintetizar cerâmica mulita de alta pureza, com pouca fase vítrea, a partir da α-alumina e sílica, obtida da casca de arroz purificada e calcinada.

Mullite, composed of 1,4Al2O3.SiO2 was synthesized using commercial α-alumina (Alpha Cesar Company) and silica obtained from the calcinations of rice husk. This silica exhibits a high specific surface area, high purity and small average particle diameter. Silica (26.2 wt.%) and α-alumina powders (71.8 wt. %) were mixed and homogenized using an alumina orbital disc mill before and after the calcinations at 1100ºC for 4 h in an air atmosphere. Then, the powders were pressed uniaxially at a pressure of 1200 MPa. The green compacts were sintered at 1650ºC, for 4 h, in air. The density of compacted sintering samples was determined using the hydrostatic method. The chemical and structural properties were observed using ICP (Inductively Coupled Plasma), XRD (X-ray diffraction) and 29Si MAS (Magic Angle Spinning) NMR (Nuclear Magnetic Resonance) and the microstructural characterization performed using SEM (Scanning Electron Micrography). The results show that it is possible to synthesize mullite ceramic of high-purity and with little glassy phase from the α-alumina and silica obtained from the rice husk that is purified and calcinated.

The high temperature oxidation behavior of two ferritic stainless steels type AISI 430A and AISI 430E is examined at low oxygen pressure and high temperatures. The AISI 430A steel is ferritic up to 860 °C. Above this temperature, this steel is bi-phased: presence of austenite and ferrite phases. The 430E steel is stabilized with Nb, and is ferritic at all temperatures. The oxidation experiments were performed in a thermobalance SETARAM TGDTA 92, in the range of 850-950 °C, in Ar/H2/H2O atmosphere, under oxygen partial pressures lower than 1.3 x 10-18 atm. The microstructure and the composition of the oxide scales were analysed by scanning electronic microscopy (SEM) and energy dispersive spectroscopy (EDS). Different oxidation behaviors in AISI 430A and AISI 430E stainless steels were observed. At 850 °C, the oxidation of the 430A steel is greater than that of the 430E steel, but above 900 °C the oxidation of the 430A steels is lower than that of the 430E steel. The oxidation rate of the 430A steel shows low dependence on temperature, while the oxidation of the 430E follows an Arrhenius law, with an activation energy corresponding to the chromia scale growth.

In order to clarify the influence of Bi-doping on oxygen diffusion in ZnO, the bulk and grain boundary oxygen diffusion coefficients were measured in Bi2O3-doped ZnO polycrystals by means of the gas-solid exchange method using the isotope 18O as the oxygen tracer. The experiments were performed on ZnO sintered samples containing 0.1, 0.3 and 0.5 mol% Bi2O3. The diffusion annealings were performed at 942, 1000 and 1092 °C, in an Ar+18O2 atmosphere under an oxygen partial pressure of 0.2 atm. After the diffusion annealings, the 18O diffusion profiles were established by secondary ion mass spectrometry (SIMS). The results show an increase in the oxygen diffusion in the Bi2O3-doped ZnO, when compared to the oxygen diffusion in the undoped ZnO polycrystal under the same experimental conditions, both in bulk and in grain-boundaries. Moreover, it was observed that the higher the Bi2O3 concentration, the higher the oxygen diffusion. These results suggest that the incorporation of Bi2O3 increases the interstitial oxygen concentration which agrees with an interstitial diffusion mechanism both in bulk and in grain-boundaries.

The structure of mullite obtained by thermal decomposition of topaz at 1340 °C and after additional thermal treatment at 1600 °C was characterized by 29Si and 27Al MAS NMR spectroscopy and x ray diffraction. No amorphous phase was detected by these techniques. The 29Si MAS NMR spectra of the mullite samples showed four resonance peaks at -81, -86, -90 and -94 ppm. The peak at -81 ppm corresponded to silicon near oxygen vacancies in the mullite structure. The peak at 86 ppm was related to a sillimanite-type site and was the major contribution, ranging from 42 to 50%. The two other peaks, at -90.0 ppm and -94 ppm, were interpreted as resulting from rearrangements of the sillimanite-type site by the replacement of AlO4 by SiO4 tetrahedra16. The 27Al MAS NMR data of the two samples exhibited three different peaks, two of which were attributed to tetrahedral sites at 40 -45 and 63 -67 ppm, while the third was assigned to an octahedral site at about -6 ppm. The ratio of tetrahedral to octahedral aluminum sites was found to depend on the temperature applied during the preparation of the mullite and was higher at 1600 °C.

Algumas formas de aproveitamento econômico do topázio incolor e, às vezes, do topázio imperial requerem o uso de tratamento térmico à alta temperatura. Nesse trabalho, revemos o comportamento térmico do topázio à alta temperatura. São mostrados os efeitos da temperatura sobre a composição química, estrutura e propriedades ópticas, assim como as condições nas quais o topázio transforma-se em outro material denominado de mulita.

A few ways of economical utilization of colorless topaz, and sometimes of the Imperial topaz, may require the heat treatment of this mineral at high temperature. This work deals with the thermal behaviour of the topaz at high temperature. The effects of the temperature on chemical composition, structure and optical properties are shown, as well as the conditions in which the topaz-to-mullite transformation takes place.

Oxygen diffusion coefficients in pure and doped ZnO polycrystals were determined by means of the gas-solid isotope exchange method using the isotope 18O as oxygen tracer. The diffusion experiments were performed from 900 to 1000 °C, under an oxygen pressure of 10(5) Pa. After the diffusion annealings, the 18O diffusion profiles were determined by secondary ion mass spectrometry. The results of the experiments show that oxygen diffusion in Li-doped ZnO is similar to the oxygen diffusion in pure ZnO, while in Al-doped ZnO the oxygen diffusion is enhanced in relation to that observed in pure ZnO, in the same experimental conditions. Based on these results is proposed an interstitial mechanism for oxygen diffusion in ZnO. Moreover, it was found that oxygen grain-boundary diffusion is ca. 3 to 4 orders of magnitude greater than oxygen volume diffusion in pure and doped ZnO, which means that the grain-boundary is a fast path for oxygen diffusion in ZnO.

This work deals with a comparison of high temperature oxidation behaviour in AISI 304 austenitic and AISI 439 ferritic stainless steels. The oxidation experiments were performed between 850 and 950 °C, in oxygen and Ar (100 vpm H2). In most cases, it was formed a Cr2O3 protective scale, whose growth kinetics follows a parabolic law. The exception was for the the AISI 304 steel, at 950 °C, in oxygen atmosphere, which forms an iron oxide external layer. The oxidation resistance of the AISI 439 does not depend on the atmosphere. The AISI 304 has the same oxidation resistance in both atmospheres, at 850 °C, but at higher temperatures, its oxidation rate strongly increases in oxygen atmosphere. Concerning the performance of these steels under oxidation, our results show that the AISI 439 steel has higher oxidation resistance in oxidizing atmosphere, above 850 °C, while, in low pO2 atmosphere, the AISI 304 steel has higher oxidation resistance than the AISI 439, in all the temperature range investigated.

Zinc self-diffusion coefficients were measured in polycrystalline ZnO of high density (>99% of the theoretical density) and of high purity (> 99.999%). The diffusion experiments were performed from 1006 to 1377 °C, in oxygen atmosphere, for times between 16 and 574 h. The diffusion profiles were established by means of Residual Activity Method using the 65Zn radioactive isotope as zinc tracer. In our experimental conditions, the zinc volume diffusion coefficients can be described by the following Arrhenius relationship: D(cm²/s) = 1.57×10-3 exp[(-2.66 ± 0.26) eV/kT]. In the same experimental conditions, the grain-boundary diffusion coefficients are approximately 4 orders of magnitude greater than the volume diffusion coefficients, and can be described by the Arrhenius relation: D'delta (cm³/s) = 1.59×10-6 exp[(-2.44 ± 0.45) eV/kT], where D' is the grain-boundary diffusion coefficient and delta is the grain boundary width.