High pressure neutron diffraction studies using the Paris-Edinburgh cell

Abstract

Neutron diffraction was until recently confined to pressures below ～ 3 GPa. This restricted range has limited the high-pressure structural information that is available for a wide range of phenomena for which neutron diffraction is the technique of choice. But now the recently-developed Paris-Edinburgh cell can achieve pressures up to ～ 30 GPa with a sample volume large enough to allow accurate structural studies with neutrons. After a period of development of the neutron scattering techniques needed to obtain the best possible results using the cell, a variety of successful structural studies have been performed. These illustrate the value of neutron diffraction in important areas such as locating hydrogen and other low-Z atoms in structures, the measurement of accurate structural pressure dependence and the examination of the changes in atomic thermal motion with pressure.     

Combined X-ray absorption and X-ray diffraction under high pressure

ABSTRACT

X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are two complementary structural techniques. Their combination improves the understanding of the effect of pressure on materials as illustrated by examples taken from studies on different types of materials (semiconductors, molecular solid, ferroelectric perovskite and gas mixture). The introduction of nanopolycrystalline diamonds anvils has extended XAS to high-energy edges with the possibility to use energy-scanning XAS beamlines where XRD can be performed in addition to XAS experiments.     

X-ray diffraction analysis for quasi-crystals under pressure

Abstract

X-ray diffration analysis under high pressure was performed on the icosahedral phase (I-phase) of an Al₈₀Mn₂₀ alloy and Al₆Li₃Cu alloy. The I-phase of an Al-Mn alloy was stable and there was no indication of phase transformations. In an Al-Li-Cu alloy, the I-phase underwent irreversible transformation successively to the amorphous state and the long-range ordered state. This is the first observation of the pressure-induced amorphization.     

X-ray diffraction study of potassium metal under high pressure

Abstract

The equation of state of potassium metal at ～25°C was measured to 6.1 GPa using energy-dispersive synchrotron radiation diffraction and a Drickamer-type cell. Previous piston-cylinder, shock wave and x-ray measurements disagree and this study is intended to help resolve these disagreements. Our P-V data fit closely to a Murnaghan equation of state and least-squares refinement gives B_o = 3.35 GPa and B_o′ = 3.28 in good agreement with recent theoretical calculations based on accurate experimental results.     

X-ray diffraction studies on oxide-superconductors under pressure by a new X-ray detection system

Abstract

A new high pressure x-ray diffraction system has been developed, which consists of a diamond anvil cell, an imaging plate as a detector and an 18 kW rotating anode type generator. By this system we found an anisotropic compression and anomalies in linear compressibility for the Bi-oxide superconductors.     

Angular dispersive diffraction using a diamond-anvil pressure cell and synchrotron X-ray source

Abstract

Wavelength dispersive diffraction studies have been performed using a diamond-anvil pressure cell and bending magnet synchrotron produced radiation. A double-crystal monochromator was used to select 15 and 17 keV photons and a 80 μm diameter collimator was used to restrict the beam entering the pressure cavity. Parallelism between the incident beam and the collimator axis was assisted by computer control of the collimator. The image of the transmitted beam was observed using a Hamamatsu x-ray Vidicon and TV monitor, for this alignment. The diffracted beam was recorded on x-ray film using a double film cassette and exposure times ranged from 6 to 8 hours. Neither the exposure time nor the line width of the diffraction lines was significantly altered by replacement of the incident beam collimator with a slit system.     

X-ray diffraction investigation of the hexagonal-fcc structural transition in yttrium trihydride under hydrostatic pressure

Pressure induced structural transition of yttrium hydride has been investigated using synchrotron radiation X-ray diffraction measurement up to 24 GPa at room temperature. A reversible hexagonal-fcc transition with a wide intermediate region from 11 to 20 GPa is confirmed, which is consistent with previously reported X-ray results. The diffraction patterns measured for the intermediate state are not interpreted in terms of a hexagonal-fcc coexisting state or as rare-earth structures with various metal-layer stacking sequences. The equation of state determined for the hexagonal-YH₃ provides a bulk modulus B₀ of 71.9 GPa, which is nearly half of the previously reported value, but is within the range of values reported for other rare-earth metal trihydrides with hexagonal structures.     

Debye temperature of gold under high pressure determined by X-ray powder diffraction method

In order to verify pressure scales of gold, the atomic-volume dependence of Debye temperature under high pressure up to 14 GPa was measured based on Debye–Waller factor by an X-ray diffraction method. High-pressure and high-temperature X-ray powder diffraction patterns were collected by an energy-dispersive method using synchrotron radiation. The X-ray Debye temperature under high pressure was calculated from the integrated intensity ratio between the diffraction patterns collected at two different temperatures. The atomic-volume dependence of the Debye temperature obtained in the present study was consistent with that predicted by a first-principles calculation, in which Debye temperature and Grüneisen parameter of the volume at ambient condition were ${\Theta }_{D0}=180K$ and ${\gamma }_0=3.16$, respectively.     

High-energy X-ray diffraction of a hydrous silicate liquid under conditions of high pressure and temperature in a modified hydrothermal diamond anvil cell

In situ high-energy X-ray diffraction measurements were made for the first time on a water-saturated silicate melt at high pressure and temperature. A modified hydrothermal diamond anvil cell (HDAC), designed to minimize the path length of the X-ray beam within a diamond anvil and to increase the solid angle of the diffracted beam, was used to reduce high background contributions and extend X-ray diffraction data collection in Q space. Quantitative differential pair distribution function (PDF) analysis of X-ray diffraction data show that the first measurable (Si–O) peak is 0.095 Å greater in length in the hydrous melt than in the starting glass. Contributions from the H₂O O–O correlations, as well as from the second nearest neighbor O–O correlations within the silicate melt, are evident within the second peak of the differential PDF. The procedure described opens new opportunities to directly investigate volatile-rich melts at high pressure and temperature.     

High pressure X-ray diffraction study of potassium azide

Crystal structure and compressibility of potassium azide was investigated by in-situ synchrotron powder X-ray diffraction in a diamond anvil cell at room temperature up to 37.7 GPa. In the body-centered tetragonal (bct) phase, an anisotropic compressibility was observed with greater compressibility in the direction perpendicular to the plane containing N₃⁻ ions than directions within that plane. The bulk modulus of the bct phase was determined to be 18.6(7) GPa. A pressure-induced phase transition may occur at 15.5 GPa.     

X-ray resonance transition radiation under three-wave diffraction

It is shown that radiation losses from X-ray resonance transition parametric radiation under three-wave diffraction are doubled compared with the two-wave case. The frequency intervals prohibited for radiation over the entire cone (except for two symmetric points on the cone) are found. This results in a decrease in the spectral density maximum and in the asymmetry of the spectral distribution. The frequency width of the maximum is in good agreement with the latest experimental data. State University of Forest, Moscow, Russia. Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Radiofizika, Vol. 40, No. 3, pp. 345–350, March, 1997.     

In situ characterization of liquid network structures at high pressure and temperature using X-ray absorption spectroscopy coupled with the Paris-Edinburgh press

ABSTRACT

We review recent progress in studying structural properties of liquids using X-ray absorption spectroscopy coupled with the Paris-Edinburgh press at third-generation synchrotron facilities. This experimental method allows for detecting subtle changes in atomic arrangements of melts over a wide pressure–temperature range. It has been also employed to monitor variations of the local coordination environment of diluted species contained in glasses, liquids and crystalline phases as a function of the pressure and temperature. Such information is of great importance for gaining deeper insights into the physico-chemical properties of liquids at extreme condition, including the understanding of such phenomena as liquid–liquid phase transitions, viscosity drops and various transport properties of geological melts. Here, we describe the experimental approach and discuss its potential in structural characterization on selected scientific highlights. Finally, the current ongoing instrumental developments and future scientific opportunities are discussed.     

X-ray diffraction evaluation of stress in high pressure deformation experiments

This paper explores the applicability of x-ray diffraction measurements of stress to high pressure deformation experiments. We model measurements of elastic lattice strains in various geometries for both axial and rotational deformation apparatus. We then show that, for most cases, stresses can be inverted from the diffraction data. A comparison between the results of our models and actual experimental data also indicates that plastic deformation can have an influence that is not addressed properly in the elastic models of lattice strains and should therefore be treated with caution.     

Synchrotron X-ray diffraction study of phenacite at high pressure

We report the results of a natural phenacite from 0 to 30.9 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at the National Synchrotron Light Source, Brookhaven National Laboratory. Over this pressure range, no phase change or disproportionation has been observed. The isothermal equation of state was determined. The values of V₀, K₀, and K₀′ refined with a third-order Birch-Murnaghan equation of state are V₀=1116.1±1.2 ų, K₀=223±9 GPa, and K₀′=5.5±0.8. Furthermore, we confirm that the linear compressibilities (β) along a and c directions of phenacite are elastically isotropic (β_a=1.50×10^-3 and β_c=1.34×10^-3 GPa^-1). Consequently, it can be concluded that the compressibility of phenacite under high pressures has been accurately constrained.     

High pressure X-ray diffraction study of CaMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation,the in-situ high-pressure structure of CaMnO3 has been investigated.In the pressure up to 36.5 GPa,no pressure-induced phase transition is observed.The pressure dependence on the lattice parameters of CaMnO3 is reported,and the relationship of the axial compression coefficients is βa 〉 βc 〉 βb.The isothermal bulk modulus K298=224（25） GPa is also obtained by fitting the pressure-volume data using the Murnaghan equation of state.     

High pressure X-ray diffraction study of SrMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation, the in-situ high-pressure structure of SrMnO₃ has been investigated. At pressure up to 28.6 GPa, no pressure-induced phase transition is observed. The lattice parameters as a function of pressure is reported, and the relationship of the axial compression coefficients is β_a>β_c. The isothermal bulk modulus K₂₉₈=266(4) GPa is also obtained by fitting the pressure-volume data using the Murnaghan equation of state.     

High pressure X-ray diffraction study of SrMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation, the in-situ high-pressure structure of SrMnO3 has been investigated. At pressure up to 28.6 GPa, no pressure-induced phase transition is observed. The lattice parameters as a function of pressure is reported, and the relationship of the axial compression coefficients is β<,a>> β<,c>. The isothermal bulk modulus K<,298>=266(4) GPa is also obtained by fitting the pressure- volume data using the Murnaghan equation of state.     

High pressure X-ray diffraction study of CaMnO3 perovskite

Using a diamond anvil cell device and synchrotron radiation,the in-situ high-pressure structure of CaMnO3 has been investigated.In the pressure up to 36.5 GPa,no pressure-induced phase transition is observed.The pressure dependence on the lattice parameters of CaMnO3 is reported,and the relationship of the axial compression coefficients is βa >βc > βb.The isothermal bulk modulus K298=224(25)GPa is also obtained by fitting the pressure-volume data using the Murnaghan equation of state.     

High pressure X-ray diffraction study on BaWO4-II

BaWO₄-II has been synthesized at 5 GPa and 610°C. Its high pressure behavior was studied by in situ synchrotron X-ray diffraction measurements at room temperature up to 17 GPa. BaWO₄-II retains its monoclinic structure. Bulk and axial moduli determined by fitting a third-order Birch–Murnaghan equation of state to lattice parameters are: K ₀=86.2±1.9 GPa, K ₀(a)=56.0±0.9 GPa, K ₀(b)=85.3±2.4 GPa, and K ₀(c)=146.1±3.2 GPa with a fixed K′=4. Analysis of axial compressible modulus shows that the a-axis is 2.61 times more compressible than the c-axis and 1.71 times more compressible than the b-axis. The beta angle decreases smoothly between room pressure and 17 GPa from 93.78° to 90.90°.