Revisiting spin state crossover in (MgFe)O by means of high resolution X-ray diffraction from a single crystal

(MgFe)O is a solid solution with ferrous iron undergoing the high to low spin state (HS-LS) crossover under high pressure. The exact state of the material in the region of the crossover is still a mystery, as domains with different spin states may coexist over a wide pressure range without changing the crystal structure neither from the symmetry nor from the atomic positions point of view. At the conditions of the crossover, (MgFe)O is a special type of microscopic disorder system. We explore the influences of (a) stress-strain relations in a diamond anvil cell, (b) time relaxation processes, and (c) the crossover itself on the characteristic features of a single crystal (111) Bragg spot before, during and after the transformation. Using high resolution X-ray diffraction as a novel method for studies of unconventional processes at the conditions of suppressed diffusion, we detect and discuss subtle changes of the (111) Bragg spot projections which we measure and analyze as a function of pressure. We report changes of the spot shape which can be correlated with the HS-LS relative abundance. In addition, we report the formation of structural defects as an intrinsic material response. These static defects are accumulated during transformation of the material from HS to LS.Comment: 28 pages, 11 Figure

Isostructural phase transition in Tb2Ti2O7 under pressure and temperature: Insights from synchrotron X-ray diffraction

Tb2Ti2O7, a pyrochlore system, has garnered significant interest due to its intriguing structural and physical properties and their dependence on external physical parameters. In this study, utilizing high-brilliance synchrotron X-ray diffraction, we conducted a comprehensive investigation of structural evolution of Tb2Ti2O7 under external pressure and temperature. We have conclusively confirmed the occurrence of an isostructural phase transition beyond the pressure of 10 GPa. The transition exhibits a distinct signature in the variation of lattice parameters under pressure and leads to changes in mechanical properties. The underlying physics driving this transition can be understood in terms of localized rearrangement of atoms while retaining the overall cubic symmetry of the crystal. Notably, the observed transition remains almost independent of temperature. Our findings provide insights into the distinctive behaviour of the isostructural phase transition in Tb2Ti2O7

Compression experiments to 126 GPa and 2500 K and thermal equation of state of Fe3S: Implications for sulphur in the Earth’s core

Pressure-volume-temperature (P-V-T) experiments on tetragonal Fe3S were conducted to 126 GPa and 2500 K in laser-heated diamond anvil cells (DAC) with in-situ X-ray diffraction (XRD). Seventy nine high-T data as well as four 300-K data were collected, based on which new thermal equations of state (EoS) for Fe3S were established. The room-T data together with existing data were fitted to the third order Birch-Murnaghan EoS, which yielded, GPa and with fixed at 377.0 Å3. A constant term in the thermal pressure equation, Pth = , fitted the high-T data well to the highest temperature, which implies that the contributions from the anharmonic and electronic terms should be minor in the thermal pressure term. The high-T data were also fitted to the Mie-Grüneisen-Debye model; with and q fixed at 417 K and 1 respectively. Calculations from the EoS show that crystalline Fe3S at 4000-5500 K is denser than the Earth's outer core and less dense than the inner core. Assuming a density reduction due to melting, liquid Fe3S would meet the outer core density profile, which however suggests that no less than 16 wt%S is needed to reconcile the observed outer core density deficit. The S-rich B2 phase, which was suggested to be a potential liquidus phase of an Fe3S-outer core above 250 GPa, namely the main constituent of its solid inner core, would likely be less dense than the Earth's inner core. As such, while the outer core density requires as much sulphur as 16 wt%, the resulting liquidus phase cannot meet the density of the inner core. Any sulphur-rich composition should therefore be rejected for the Earth's core

Automated pipeline processing X‐ray diffraction data from dynamic compression experiments on the Extreme Conditions Beamline of PETRA III

Presented and discussed here is the implementation of a software solution that provides prompt X‐ray diffraction data analysis during fast dynamic compression experiments conducted within the dynamic diamond anvil cell technique. It includes efficient data collection, streaming of data and metadata to a high‐performance cluster (HPC), fast azimuthal data integration on the cluster, and tools for controlling the data processing steps and visualizing the data using the DIOPTAS software package. This data processing pipeline is invaluable for a great number of studies. The potential of the pipeline is illustrated with two examples of data collected on ammonia–water mixtures and multiphase mineral assemblies under high pressure. The pipeline is designed to be generic in nature and could be readily adapted to provide rapid feedback for many other X‐ray diffraction techniques, e.g. large‐volume press studies, in situ stress/strain studies, phase transformation studies, chemical reactions studied with high‐resolution diffraction etc