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The dynamic diamond anvil cell (dDAC) is a recently developed experimental platform that has shown promise for studying the behavior of materials at strain rates ranging from intermediate to quasi-static and shock compression regimes. Combining dDAC with time-resolved x-ray diffraction (XRD) in the radial geometry (i.e., with incident x-rays perpendicular to the axis of compression) enables the study of material properties such as strength, texture evolution, and deformation mechanisms. This work describes a radial XRD dDAC setup at beamline P02.2 (Extreme Conditions Beamline) at DESY's PETRA III synchrotron. Time-resolved radial XRD data are collected for titanium, zirconium, and zircon samples, demonstrating the ability to study the strength and texture of materials at compression rates above 300 GPa/s. In addition, the simultaneous optical imaging of the DAC sample chamber is demonstrated. The ability to conduct simultaneous radial XRD and optical imaging provides the opportunity to characterize plastic strain and deviatoric strain rates in the DAC at intermediate rates, exploring the strength and deformation mechanisms of materials in this regime. [ABSTRACT FROM AUTHOR]

We have performed in situ synchrotron X-ray diffraction experiments on TaC0.99 compressed in a diamond anvil cell along 3 isothermal paths to maximum pressure (P)-temperature (T) conditions of 38.8 GPa at 1073 K. By combining measurements performed in axial diffraction geometry at 296 K and in radial geometry at 673 K and 1073 K, we place constraints on the pressure-volume-temperature (P-V-T) equation of state of TaC in a wide range of conditions. A fit of the Birch-Murnaghan equation to the measurements performed in axial geometry at ambient temperature yields a value of the isothermal bulk modulus at ambient conditions K T 0 = 305 ± 5 (1 σ) GPa and its pressure derivative (∂ K T / ∂ P) T 0 = 6.1 ± 0.5. The fit of the Birch-Murnaghan-Debye model to our complete P-V-T dataset allows us to constrain the Grüneisen parameter at ambient pressure γ 0 = V (∂ P / ∂ E) V 0 to the value of 1.2 ± 0.1. [ABSTRACT FROM AUTHOR]

The high‐precision X‐ray diffraction setup for work with diamond anvil cells (DACs) in interaction chamber 2 (IC2) of the High Energy Density instrument of the European X‐ray Free‐Electron Laser is described. This includes beamline optics, sample positioning and detector systems located in the multipurpose vacuum chamber. Concepts for pump–probe X‐ray diffraction experiments in the DAC are described and their implementation demonstrated during the First User Community Assisted Commissioning experiment. X‐ray heating and diffraction of Bi under pressure, obtained using 20 fs X‐ray pulses at 17.8 keV and 2.2 MHz repetition, is illustrated through splitting of diffraction peaks, and interpreted employing finite element modeling of the sample chamber in the DAC. [ABSTRACT FROM AUTHOR]

A resistively-heated dynamic diamond anvil cell (RHdDAC) setup is presented. The setup enables the dynamic compression of samples at high temperatures by employing a piezoelectric actuator for pressure control and internal heaters for high temperature. The RHdDAC facilitates the precise control of compression rates and was tested in compression experiments at temperatures up to 1400 K and pressures of ∼130 GPa. The mechanical stability of metallic glass gaskets composed of a FeSiB alloy was examined under simultaneous high-pressure/high-temperature conditions. High-temperature dynamic compression experiments on H2O ice and (Mg, Fe)O ferropericlase were performed in combination with time-resolved x-ray diffraction measurements to characterize crystal structures and compression behaviors. The employment of high brilliance synchrotron radiation combined with two fast GaAs LAMBDA detectors available at the Extreme Conditions Beamline (P02.2) at PETRA III (DESY) facilitates the collection of data with excellent pressure resolution. The pressure–temperature conditions achievable with the RHdDAC combined with its ability to cover a wide range of compression rates and perform tailored compression paths offers perspectives for a variety of future experiments under extreme conditions. [ABSTRACT FROM AUTHOR]

We present an improved setup for the experimental study of deformation of solids at simultaneous high pressures and temperatures by radial x-ray diffraction. This technique employs a graphite resistive heated Mao–Bell type diamond anvil cell for radial x-ray diffraction in combination with a water-cooled vacuum chamber. The new chamber has been developed by the sample environment group at PETRA III and implemented at the Extreme Conditions Beamline P02.2 at PETRA III, DESY (Hamburg, Germany). We discuss applications of the new setup to study deformation of a variety of materials, including ferropericlase, calcium perovskite, bridgmanite, and tantalum carbide, at high-pressure/temperature. [ABSTRACT FROM AUTHOR]

We performed high-pressure synchrotron x-ray diffraction experiments on nanocrystalline (nc-) MgO compressed both under quasi-hydrostatic and non-hydrostatic conditions in a diamond-anvil cell. Data obtained under hydrostatic conditions show that nc-MgO (average crystallite size of 20 nm) is 8-9% more compressible than 'bulk' MgO. Analysis of our results collected under non-hydrostatic conditions yields a bulk modulus that is about 27% larger than the one derived from the quasi-hydrostatic compression experiments. Thus, the apparent bulk modulus strongly depends on the experimental stress conditions. [ABSTRACT FROM AUTHOR]

Fast compression experiments performed using dynamic diamond anvil cells (dDACs) employing piezoactuators offer the opportunity to study compression-rate dependent phenomena. In this paper, we describe an experimental setup which allows us to perform time-resolved x-ray diffraction during the fast compression of materials using improved dDACs. The combination of the high flux available using a 25.6 keV x-ray beam focused with a linear array of compound refractive lenses and the two fast GaAs LAMBDA detectors available at the Extreme Conditions Beamline (P02.2) at PETRA III enables the collection of x-ray diffraction patterns at an effective repetition rate of up to 4 kHz. Compression rates of up to 160 TPa/s have been achieved during the compression of gold in a 2.5 ms fast compression using improved dDAC configurations with more powerful piezoactuators. The application of this setup to low-Z compounds at lower compression rates is described, and the high temporal resolution of the setup is demonstrated. The possibility of applying finely tuned pressure profiles opens opportunities for future research, such as using oscillations of the piezoactuator to mimic propagation of seismic waves in the Earth. [ABSTRACT FROM AUTHOR]

High pressure angle-dispersive X-ray diffraction investigations have been carried out on α-cristobalite form of Al0.5Ga0.5PO4. Our investigations show that the structural stability of this phase under high pressure depends on the nature of pressure conditions in the diamond anvil cell. Under hydrostatic pressure conditions using neon as a pressure transmitting medium, ambient orthorhombic C2221 phase transforms to orthorhombic Cmcm phase at 4.9 GPa. The high pressure Cmcm phase remains stable up to the highest pressure in the experiment, i.e. 19 GPa. The values of bulk modulus for C2221 and Cmcm phases are 19(2) and 126(4) GPa, respectively. In contrast to this, under non-hydrostatic pressure conditions, transformation of ambient C2221 phase to Cmcm phase has not observed up to 17.4 GPa. Instead, a new monoclinic phase P21 is observed which contains layers of six coordinated Al/Ga ions separated by less dense five coordinated Al/Ga ions. [ABSTRACT FROM AUTHOR]

The crystal structure and vibration spectra of sodium niobate NaNbO3have been studied by means of neutron diffraction, X-ray diffraction and Raman spectroscopy at high pressures. An isostructural phase transformation from the initial antiferroelectric phase to an intermediate antiferroelectric phase HP-I have been observed under 2 GPa. This transformation is caused by complex reorientations of NbO6octahedra. Subsequent structural phase transition from the phase HP-I to an orthorhombic phase HP-III have been detected at pressures above 10 GPa. This transition leads to suppression of an antiferroelectric state of NaNbO3. The observed phase transitions are accompanied by anomalies in lattice parameters compression. [ABSTRACT FROM PUBLISHER]

Metallic osmium (Os) is one of the most exceptional elemental materials, having, at ambient pressure, the highest known density and one of the highest cohesive energies and melting temperatures. It is also very incompressible, but its high-pressure behaviour is not well understood because it has been studied so far only at pressures below 75 gigapascals. Here we report powder X-ray diffraction measurements on Os at multi-megabar pressures using both conventional and double-stage diamond anvil cells, with accurate pressure determination ensured by first obtaining self-consistent equations of state of gold, platinum, and tungsten in static experiments up to 500 gigapascals. These measurements allow us to show that Os retains its hexagonal close-packed structure upon compression to over 770 gigapascals. But although its molar volume monotonically decreases with pressure, the unit cell parameter ratio of Os exhibits anomalies at approximately 150 gigapascals and 440 gigapascals. Dynamical mean-field theory calculations suggest that the former anomaly is a signature of the topological change of the Fermi surface for valence electrons. However, the anomaly at 440 gigapascals might be related to an electronic transition associated with pressure-induced interactions between core electrons. The ability to affect the core electrons under static high-pressure experimental conditions, even for incompressible metals such as Os, opens up opportunities to search for new states of matter under extreme compression. [ABSTRACT FROM AUTHOR]

A detailed description is presented of the Extreme Conditions Beamline P02.2 for micro X-ray diffraction studies of matter at simultaneous high pressure and high/low temperatures at PETRA III, in Hamburg, Germany. This includes performance of the X-ray optics and instrumental resolution as well as an overview of the different sample environments available for high-pressure studies in the diamond anvil cell. Particularly emphasized are the high-brilliance and high-energy X-ray diffraction capabilities of the beamline in conjunction with the use of fast area detectors to conduct time-resolved compression studies in the millisecond time regime. Finally, the current capability of the Extreme Conditions Science Infrastructure to support high-pressure research at the Extreme Conditions Beamline and other PETRA III beamlines is described. [ABSTRACT FROM AUTHOR]

The behavior of a natural topaz, AlSiO(OHF), has been investigated by means of in situ single-crystal synchrotron X-ray diffraction up to 45 GPa. No phase transition or change in the compressional regime has been observed within the pressure-range investigated. The compressional behavior was described with a third-order Birch-Murnaghan equation of state (III-BM-EoS). The III-BM-EoS parameters, simultaneously refined using the data weighted by the uncertainties in P and V, are as follows: K = 158(4) GPa and K ′ = 3.3(3). The confidence ellipse at 68.3 % (Δχ = 2.30, 1σ) was calculated starting from the variance-covariance matrix of K and K′ obtained from the III-BM-EoS least-square procedure. The ellipse is elongated with a negative slope, indicating a negative correlation of the parameters K and K ′, with K = 158 ± 6 GPa and K ′ = 3.3 ± 4. A linearized III-BM-EoS was used to obtain the axial-EoS parameters (at room- P), yielding: K( a) = 146(5) GPa [ β = 1/(3 K( a)) = 0.00228(6) GPa] and K′( a) = 4.6(3) for the a-axis; K( b) = 220(4) GPa [ β = 0.00152(4) GPa] and K′( b) = 2.6(3) for the b-axis; K( c) = 132(4) GPa [ β = 0.00252(7) GPa] and K′( c) = 3.3(3) for the c-axis. The elastic anisotropy of topaz at room- P can be expressed as: K( a): K( b): K( c) = 1.10:1.67:1.00 ( β: β: β = 1.50:1.00:1.66). A series of structure refinements have been performed based on the intensity data collected at high pressure, showing that the P-induced structure evolution at the atomic scale is mainly represented by polyhedral compression along with inter-polyhedral tilting. A comparative analysis of the elastic behavior and P/ T-stability of topaz polymorphs and 'phase egg' (i.e., AlSiOOH) is carried out. [ABSTRACT FROM AUTHOR]

The high-pressure behavior of LiLaNbO ( x = 1/6, 1/3, 1/2, 2/3) perovskites where Li cations were substituted for the existing vacancies was studied using synchrotron X-ray diffraction. It was shown that all these materials undergo irreversible pressure-induced amorphization around 14.5 GPa regardless of the Li concentration. The Li-inserted materials were found to exhibit a standard pressure response (bulk modulus pressure derivative B′ ~4) when in the crystalline phase, whereas LaNbO shows a linear volume contraction versus pressure, i.e., B′ ~(−1). These results suggest that the structural collapse is not a consequence of cation disorder resulting from the Nb atoms (B-site) migrating to the A-site vacancies. The observed pressure response can be understood by increased occupancy of the A-sites opposing the tilting of the NbO octahedra. The pressure evolution of the Nb oxidation state is discussed. [ABSTRACT FROM AUTHOR]

Abstract: Using a newly developed experimental protocol based on externally heated diamond anvil cells, in situ stress and textures studies are performed on polycrystalline body-centered cubic-(α-), face-centered cubic-(γ-) and hexagonal close-packed-(ε-)Fe during plastic deformation up to 36GPa and 1000K. At 7GPa and 973K, α-Fe displays a texture attributed to dominant slip on . Upon pressure increase up to 24GPa at constant temperature, differential stress is shown to increase to 0.6±0.1GPa while Fe is transforming into γ-Fe and ε-Fe. Textures observed in γ-Fe are fully induced by phase transformation, with little effect of plastic deformation. Textures observed in ε-Fe are the result of phase transformation from γ-Fe combined with plastic deformation, with dominant basal slip. The differential stress measured in ε-Fe is consistent with a shear strength of ∼1.9GPa at 17GPa and 300K, with a temperature dependence of −0.003GPaK−1 and a pressure dependence of 0.074. [Copyright &y& Elsevier]

Data on partitioning behavior of elements between different phases at in situ conditions are crucial for the understanding of element mobility especially for geochemical studies. Here, we present results of in situ partitioning of trace elements (Zr, Pd, and Ru) between silicate and iron melts, up to 50 GPa and 4200 K, using a modified laser heated diamond anvil cell (DAC). This new experimental set up allows simultaneous collection of x-ray fluorescence (XRF) and x-ray diffraction (XRD) data as a function of time using the high pressure beamline ID27 (ESRF, France). The technique enables the simultaneous detection of sample melting based to the appearance of diffuse scattering in the XRD pattern, characteristic of the structure factor of liquids, and measurements of elemental partitioning of the sample using XRF, before, during and after laser heating in the DAC. We were able to detect elements concentrations as low as a few ppm level (2-5 ppm) on standard solutions. In situ measurements are complimented by mapping of the chemical partitions of the trace elements after laser heating on the quenched samples to constrain the partitioning data. Our first results indicate a strong partitioning of Pd and Ru into the metallic phase, while Zr remains clearly incompatible with iron. This novel approach extends the pressure and temperature range of partitioning experiments derived from quenched samples from the large volume presses and could bring new insight to the early history of Earth. [ABSTRACT FROM AUTHOR]

The structural and magnetic properties of Cr 2 O 3 have been studied by means of X-ray and neutron powder diffraction at high pressures up to 35 GPa. The lattice compression of the rhombohedral crystal structure of R 3 ¯ c symmetry is slightly anisotropic with anomaly in the pressure behavior of the c/a parameters ratio at P ≈ 20 GPa of presumably magnetic nature. The oxygen octahedra around chromium ions become more symmetric with close values of shared and unshared bonds under high pressure. The antiferromagnetic structure of Cr 2 O 3 remains stable in the studied pressure range up to 35 GPa. The pressure coefficient of the Néel temperature, (1/ T N )( dT N /dP ) = + 0.0091 GPa −1 , is significantly less in comparison with perovskite-like compounds containing Cr 3+ and Mn 4+ ions of similar electronic configuration. [ABSTRACT FROM AUTHOR]

The crystal, magnetic structure and vibrational spectra of multiferroic GaFeO 3 have been studied by means of neutron, X-ray powder diffraction and Raman spectroscopy at pressures up to 6.2 and 42 GPa, respectively. A presence of Fe/Ga antisite disorder leads to a formation of the ferrimagnetic ground state with the Néel temperature T N = 292 K at ambient pressure. Upon compression, the magnetic ground state symmetry remains the same and the Néel temperature increases with a pressure coefficient (1/T N )(dT N /dP) = 0.011(1) GPa −1 . Application of high pressure above 21 GPa leads to a gradual structural phase transition from the polar orthorhombic Pc 2 1 n phase to nonpolar orthorhombic Pbnm phase. It is accompanied by anomalies in the pressure behaviour of several Raman modes. Pressure dependencies of lattice parameters and Raman modes frequencies in the observed structural phases were obtained. [ABSTRACT FROM AUTHOR]

The melting of bismuth in response to shock compression has been studied using in situ femtosecond x-ray diffraction at an x-ray free electron laser. Both solid-solid and solid-liquid phase transitions are documented using changes in discrete diffraction peaks and the emergence of broad, liquid scattering upon release from shock pressures up to 14 GPa. The transformation from the solid state to the liquid is found to occur in less than 3 ns, very much faster than previously believed. These results are the first quantitative measurements of a liquid material obtained on shock release using x-ray diffraction, and provide an upper limit for the time scale of melting of bismuth under shock loading. [ABSTRACT FROM AUTHOR]

Between 19 and 54 GPa, potassium has a complex composite incommensurate host-guest structure which undergoes two intraphase transitions over this pressure range. The temperature dependence of these host-guest phases is further complicated by the onset of an order-disorder transition in their guest chains. Here, we report single-crystal, quasi-single-crystal, and powder synchrotron x-ray diffraction measurements of this order-disorder phenomenon in incommensurate potassium to 47 GPa and 750 K. The so-called chain melting transition is clearly visible over a 22 GPa pressure range, and there are significant changes in the slope of the phase boundary which divides the ordered and disordered phases, one of which results from the intraphase transitions in the guest structure. [ABSTRACT FROM AUTHOR]

We report on an x-ray diffraction (XRD) study of helical poly[9,9-bis(2-ethylhexyl)fluorene] (PF2/6) under high quasihydrostatic pressure and show an effect of pressure on the torsion angle (dihedral angle) between adjunct repeat units and on the hexagonal unit cell. A model for helical backbone conformation is constructed. The theoretical position for the most prominent 001 x-ray reflection is calculated as a function of torsion angle. The XRD of high molecular weight PF2/6 (Ma = 30 kg/mol) is measured through a diamond anvil cell upon pressure increase from 1 to 10 GPa. The theoretically considered 001 reflection is experimentally identified, and its shift with the increasing pressure is found to be consistent with the decreasing torsion angle between 2 and 6 GPa. This indicates partial backbone planarization towards a more open helical structure. The h00 peak is identified, and its shift together with the broadening of 00l implies impairment of the ambient hexagonal order, which begins at or below 2 GPa. Previously collected high-pressure photoluminescence data are reanalyzed and are found to be qualitatively consistent with the XRD data. This paper provides an example of how the helical 7r-conjugated backbone structure can be controlled by applying high quasihydrostatic pressure without modifications in its chemical structure. Moreover, it paves the way for wider use of high-pressure x-ray scattering in the research of Π-conjugated polymers. [ABSTRACT FROM AUTHOR]

The structural, magnetic, and vibrational properties of RbFe(MoO4)2 have been studied by means of x-ray and neutron powder diffraction, magnetic susceptibility measurements, and Raman spectroscopy at pressures up to 10 GPa. The gradual structural phase transition from the initial trigonal P3m1 phase to the monoclinic C2/c phase via the intermediate P3 phase was observed at P ∼ GPa. The triangular antiferromagnetic order with a propagation vector q = (1/3, 1/3, qz) in the suppressed trigonal phase remains incommensurate, and the qz value increases from 0.45 to 0.48 in the pressure range 0-2 GPa at T = 2 K. The pressure coefficient of the Néel temperature is equal to (1/TN)dTN/dP = 0.09 GPa-1. No evidence of the formation of the long-range magnetic order in the monoclinic phase was found. The pressure dependencies of the vibrational modes for the trigonal and monoclinic phases were obtained. [ABSTRACT FROM AUTHOR]