We present a portable CO laser heating system for in situ x-ray absorption spectroscopy (XAS) studies at 16-BM-D (High Pressure Collaborative Access Team, Advanced Photon Source, Argonne National Laboratory). Back scattering optical measurements are made possible by the implementation of a Ge beamsplitter. Optical pyrometry is conducted in the near-infrared, and our temperature measurements are free of chromatic aberration due to the implementation of the peak-scaling method [A.
View Article and Find Full Text PDFThe ultrafast synthesis of ε-FeN in a diamond-anvil cell (DAC) from Fe and N under pressure was observed using serial exposures of an X-ray free electron laser (XFEL). When the sample at 5 GPa was irradiated by a pulse train separated by 443 ns, the estimated sample temperature at the delay time was above 1400 K, confirmed by transformation of α- to γ-iron. Ultimately, the Fe and N reacted uniformly throughout the beam path to form FeN, as deduced from its established equation of state (EOS).
View Article and Find Full Text PDFIn this report, we present results of high-pressure experiments probing the melt line of zirconium (Zr) up to 37 GPa. This investigation has determined that temperature versus laser power curves provide an accurate method to determine melt temperatures. When this information is combined with the onset of diffuse scattering, which is associated with the melt process, we demonstrate the ability to accurately determine the melt boundary.
View Article and Find Full Text PDFZirconium (Zr) has properties conducive to nuclear applications and exhibits complex behavior at high pressure with respect to the effects of impurities, deviatoric stress, kinetics, and grain growth which makes it scientifically interesting. Here, we present experimental results on the 300 K equation of state of ultra-high purity Zr obtained using the diamond-anvil cell coupled with synchrotron-based x-ray diffraction and electrical resistance measurements. Based on quasi-hydrostatic room-temperature compression in helium to pressure P = 69.
View Article and Find Full Text PDFMany rutile-type materials are characterized by a softness in shear with pressure which is coupled to a Raman-active librational motion. Combining direct studies of anion positions in SnO with measurements of its electronic properties, we find a correlation between O sublattice disorder between 5 and 10 GPa and an anomalous decrease up to 4 orders of magnitude in electrical resistance. Hypotheses into the atomistic nature of the phenomenon are evaluated via ab initio calculations guided by extended X-ray absorption fine structure spectroscopy analysis, and the most likely mechanism is found to be the displacement of single anions resulting from the pressure-induced softening of the librational mode.
View Article and Find Full Text PDFThe viscosity of Earth's lower mantle is poorly constrained due to the lack of knowledge on some fundamental variables that affect the deformation behaviour of its main mineral phases. This study focuses on bridgmanite, the main lower mantle constituent, and assesses its rheology by developing an approach based on mineral physics. Following and revising the recent advances in this field, pure climb creep controlled by diffusion is identified as the key mechanism driving deformation in bridgmanite.
View Article and Find Full Text PDFThe pioneering of x-ray diffraction with in situ laser heating in the diamond-anvil cell has revolutionized the field of high-pressure mineral physics, expanding the ability to determine high-pressure, high-temperature phase boundaries and equations of state. Accurate determination of high-pressure, high-temperature phases and densities in the diamond-anvil cell rely upon collinearity of the x-ray beam with the center of the laser-heated spot. We present the development of microfabricated samples that, by nature of their design, will have the sample of interest in the hottest portion of the sample.
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