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The effect of small changes in the specimen-to-detector distance on the unit-cell parameters is examined for synchrotron powder diffraction in Debye–Scherrer (transmission) geometry with a flat area detector. An analytical correction equation is proposed to fix the shift in 2θ values due to specimen capillary displacement. This equation does not require the use of an internal reference material, is applied during the Rietveld refinement step, and is analogous to the specimen-displacement correction equations for Bragg–Brentano and curved-detector Debye–Scherrer geometry experiments, but has a different functional form. The 2θ correction equation is compared with another specimen-displacement correction based on the use of an internal reference material in which new integration and calibration parameters of area-detector images are determined. Example data sets showing the effect of a 3.3 mm specimen displacement on the unit-cell parameters for 25°C CeO 2 , including both types of displacement correction, are described. These experiments were performed at powder X-ray diffraction beamlines at the National Synchrotron Light Source II at Brookhaven National Laboratory and the Advanced Photon Source at Argonne National Laboratory. 

Geopolymers (GPs) are emerging, low‐density ceramic materials that are simple to manufacture, with high elastic modulus and strength, albeit with low toughness. Fiber reinforcements have been used to achieve varied ductile behaviors, but little is known about the GP addition to polymeric frame structures. Thus, drawing inspiration from the nanostructure of bones, this paper investigated an interpenetrating, co‐continuous composite consisting of a GP as the stiff but brittle phase, and a 3D‐printed polymer (PA12 White) as the soft and deformable phase. The composite mechanical properties and failure modes were studied experimentally using uniaxial compression and four‐point bending tests. The co‐continuous network constrained brittle cracking within the GP and reduced strain localization in the polymer. The results showed that the composite had higher strength (56.11 ± 2.12 MPa) and elastic modulus (6.08 ± 1.37 GPa) than the 3D‐printed polymer and had higher toughness (5.98 ± 0.24 MJ/mm³) than the GP for the specific geometries examined. The shape effect study demonstrated that cubic structures had higher elastic modulus and strength but at the expense of lower toughness when compared to rectangular prism structures. The study of scale effects indicated that increasing the number of periodic unit cells while maintaining consistent bulk dimensions led to augmented strength and toughness, albeit without statistically significant alterations in elastic modulus. Thus, this paper presents an experimental realization of a novel, bio‐inspired, interpenetrating, GP–polymer composite design, offering improved strength and toughness. It also provides valuable insights into the shape and size effects on the mechanical properties of this new composite.

 

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). 

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. 

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 CO₂laser, 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.