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  1. Abstract

    A single‐crystal specimen of rutile (titania) was flashed repetitively, while increasing the electric field after each cycle. As expected, the flash onset temperature continued to drop modestly at higher fields. However, when the field was increased from 400 to 450 V cm–1, the flashed onset fell dramatically down to room temperature. We have investigated the electrical and optical properties of this room temperature flashed specimen (called SZ). The specimen was electronically conducting. Optical absorption spectroscopy revealed a narrow band of new energy levels that were generated just below the conduction band. The gap between the conduction band and this flash‐induced energy level agreed with the peak in the electroluminescence spectrum. Optical second harmonic generation (SHG) is reported. The flash‐on condition significantly lowered the SHG, which rebounded when the flash was turned off. This result suggests that the structure becomes more centrosymmetric in the state of flash, which may represent a disordered state of defects. The possibility of studying flash behavior at room temperature, without a furnace (as in SZ type specimens), opens a considerable simplification for in‐situ characterization of flash behavior. For example, a possible relationship between memristor physics and the flash phenomenon can be studied.

     
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  2. Abstract

    The oxidation behavior of SiC fibers coated with (a) undoped polysilazane and (b) precursors containing a mixture of polysilazane and hafnium butoxide in equal weight fractions, is reported. The coatings were prepared by repetitive cycles of nanolayer depositions, as reported in recent publications. The oxidation experiments were carried out at 1400°C in ambient air (Boulder, CO) for up to 100 hours. The extent of degradation of SiC was measured by the recession in the diameter of the fibers as a function of time. The fibers with undoped polymer precursor recessed significantly, whereas the fibers coated with HfSiCNO remained essentially unchanged. These results are in agreement with earlier work from our laboratory where the resilience of hafnon and zircon, as well as hafnia and zirconia, against high‐temperature corrosion in streaming humid environments had been highlighted.

     
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  3. In situ X-ray diffraction measurements at the Advanced Photon Source show that alpha-Al2O3 and MgAl2O4 react nearly instantaneously and completely, and nearly completely to form single-phase high-alumina spinel during voltage-to-current type of flash sintering experiments. The initial sample was constituted from powders of alpha-Al2O3, MgAl2O4 spinel, and cubic 8 mol% Y2O3-stabilized ZrO2 (8YSZ) mixed in equal volume fractions, the spinel to alumina molar ratio being 1:1.5. Specimen temperature was measured by thermal expansion of the platinum standard. These measurements correlated well with a black-body radiation model, using appropriate values for the emissivity of the constituents. Temperatures of 1600-1736 degrees C were reached during the flash, which promoted the formation of alumina-rich spinel. In a second set of experiments, the flash was induced in a current-rate method where the current flowing through the specimen is controlled and increased at a constant rate. In these experiments, we observed the formation of two different compositions of spinel, MgO center dot 3Al(2)O(3) and MgO center dot 1.5Al(2)O(3), which evolved into a single composition of MgO center dot 2.5Al(2)O(3) as the current continued to increase. In summary, flash sintering is an expedient way to create single-phase, alumina-rich spinel. 
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  4. Abstract

    The addition of small quantities of aluminum oxide (Al2O3) to 8 mol% yttria‐stabilized zirconia (8YSZ) benefits conventional sintering by acting as a sintering aid and altering grain growth behavior. However, it is uncertain if these benefits observed during conventional sintering extend to flash sintering. In this work, nanoscale films of Al2O3are deposited on 8YSZ powders by particle atomic layer deposition (ALD). The ALD‐coated powders were flash sintered using voltage‐to‐current control and current rate experiments. The sintering behavior, microstructural evolution, and ionic conductivities were characterized. The addition of Al2O3films changed the conductivity of the starting powder, effectively moving the flash onset temperature. The grain size of the samples flashed with current rate experiments was ~65% smaller than that of conventionally sintered samples. Measurement of grain size and estimates of sample density as a function of temperature during flash sintering showed that small quantities of Al2O3can enhance grain growth and sintering of 8YSZ. This suggests that Al2O3dissolves into the 8YSZ grain boundaries during flash sintering to form complexions that enhance the diffusion of species controlling these processes.

     
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