Structural characterization of mullites synthesized by thermal decomposition of topaz

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

Effect of alloy grain size on the high-temperature oxidation behavior of the austenitic steel TP 347

Generally, oxide scales formed on high Cr steels are multi-layered and the kinetics are strongly influenced by the alloy grain boundaries. In the present study, the oxidation behaviour of an austenite steel TP347 with different grain sizes was studied to identify the role of grain-boundaries in the oxidation process. Heat treatment in an inert gas atmosphere at 1050 °C was applied to modify the grain size of the steel TP347. The mass gain during subsequent oxidation was measured using a microbalance with a resolution of 10-5 g. The scale morphology was examined using SEM in combination with energy-dispersive X-ray spectroscopy (EDS). Oxidation of TP347 with a grain size of 4 µm at 750 °C in air follows a parabolic rate law. For a larger grain size (65 µm), complex kinetics is observed with a fast initial oxidation followed by several different parabolic oxidation stages. SEM examinations indicated that the scale formed on specimens with smaller grain size was predominantly Cr2O3, with some FeCr2O4 at localized sites. For specimens with larger grain size the main oxide is iron oxide. It can be concluded that protective Cr2O3 formation is promoted by a high density of fast grain-boundary diffusion paths which is the case for fine-grained materials