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  1. Characterization of the thermal expansion in the rare earth di-titanates is important for their use in high-temperature structural and dielectric applications. Powder samples of the rare earth di-titanates R 2 Ti 2 O 7 (or R 2 O 3 ·2TiO 2 ), where R = La, Pr, Nd, Sm, Gd, Dy, Er, Yb, Y, which crystallize in either the monoclinic or cubic phases, were synthesized for the first time by the solution-based steric entrapment method. The three-dimensional thermal expansions of these polycrystalline powder samples were measured by in situ synchrotron powder diffraction from 25°C to 1600°C in air, nearly 600°C higher than other in situ thermal expansion studies. The high temperatures in synchrotron experiments were achieved with a quadrupole lamp furnace. Neutron powder diffraction measured the monoclinic phases from 25°C to 1150°C. The La 2 Ti 2 O 7 member of the rare earth di-titanates undergoes a monoclinic to orthorhombic displacive transition on heating, as shown by synchrotron diffraction in air at 885°C (864°C–904°C) and neutron diffraction at 874°C (841°C–894°C).
  2. 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.
  3. The previously unknown experimental HfO2–Ta2O5‐temperature phase diagram has been elucidated up to 3000°C using a quadrupole lamp furnace and conical nozzle levitator system equipped with a CO2 laser, in conjunction with synchrotron X‐ray diffraction. These in‐situ techniques allowed the determination of the following: (a) liquidus, solidus, and invariant transformation temperatures as a function of composition from thermal arrest experiments, (b) determination of equilibrium phases through testing of reversibility via in‐situ X‐ray diffraction, and (c) molar volume measurements as a function of temperature for equilibrium phases. From these, an experimental HfO2–Ta2O5‐temperature phase diagram has been constructed which is consistent with the Gibbs Phase Rule.