Deformation of two-phase aggregates with in situ X-ray tomography in rotating Paris-Edinburgh cell at GPa pressures and high temperature.

High-pressure (>1 GPa) torsion apparatus can be coupled with in situ X-ray tomography (XRT) to study microstructures in materials associated with large shear strains. Here, deformation experiments were carried out on multi-phase aggregates at ∼3-5 GPa and ∼300-500°C, using a rotational tomography Paris-Edinburgh press (RoToPEc) with in situ absorption contrast XRT on the PSICHE beamline at Synchrotron SOLEIL. The actual shear strain reached in the samples was quantified with respect to the anvil twisting angles, which is γ ≤ 1 at 90° anvil twist and reaches γ ≃ 5 at 225° anvil twist. 2D and 3D quantifications based on XRT that can be used to study in situ the deformation microfabrics of two-phase aggregates at high shear strain are explored. The current limitations for investigation in real time of deformation microstructures using coupled synchrotron XRT with the RoToPEc are outlined.

Quantitative 4D X-ray microtomography under extreme conditions: a case study on magma migration.

X-ray computed tomography (XCT) is a well known method for three-dimensional characterization of materials that is established as a powerful tool in high-pressure/high-temperature research. The optimization of synchrotron beamlines and the development of fast high-efficiency detectors now allow the addition of a temporal dimension to tomography studies under extreme conditions. Presented here is the experimental setup developed on the PSICHE beamline at SOLEIL to perform high-speed XCT in the Ultra-fast Tomography Paris-Edinburgh cell (UToPEc). The UToPEc is a compact panoramic (165° angular aperture) press optimized for fast tomography that can access 10 GPa and 1700°C. It is installed on a high-speed rotation stage (up to 360°â€…s-1) and allows the acquisition of a full computed tomography (CT) image with micrometre spatial resolution within a second. This marks a major technical breakthrough for time-lapse XCT and the real-time visualization of evolving dynamic systems. In this paper, a practical step-by-step guide to the use of the technique is provided, from the collection of CT images and their reconstruction to performing quantitative analysis, while accounting for the constraints imposed by high-pressure and high-temperature experimentation. The tomographic series allows the tracking of key topological parameters such as phase fractions from 3D volumetric data, and also the evolution of morphological properties (e.g. volume, flatness, dip) of each selected entity. The potential of this 4D tomography is illustrated by percolation experiments of carbonate melts within solid silicates, relevant for magma transfers in the Earth's mantle.

Argon-neon binary diagram and ArNe2 Laves phase.

Mixtures of argon and neon have been experimentally studied under high pressure. One stoichiometric compound, with ArNe2 composition, is observed in this system. It is a Laves phase with a hexagonal MgZn2 structure, stable up to at least 65 GPa, the highest pressure reached in the experiments. Its equation of state follows closely the one of an ideal Ar+2Ne mixture. The binary phase diagram of the Ar-Ne system resembles the diagram predicted for hard sphere mixtures with a similar atomic radius ratio, suggesting that no electronic interactions appear in this system in this pressure range. ArNe2 can be a convenient quasihydrostatic pressure transmitting medium under moderate pressure.

Synthesis of ß-Mg(2)C(3): a monoclinic high-pressure polymorph of magnesium sesquicarbide.

A new monoclinic variation of Mg2C3 was synthesized from the elements under high-pressure (HP), high-temperature (HT) conditions. Formation of the new compound, which can be recovered to ambient conditions, was observed in situ using X-ray diffraction with synchrotron radiation. The structural solution was achieved by utilizing accurate theoretical results obtained from ab initio evolutionary structure prediction algorithm USPEX. Like the previously known orthorhombic Pnnm structure (α-Mg2C3), the new monoclinic C2/m structure (ß-Mg2C3) contains linear C3(4-) chains that are isoelectronic with CO2. Unlike α-Mg2C3, which contains alternating layers of C3(4-) chains oriented in opposite directions, all C3(4-) chains within ß-Mg2C3 are nearly aligned along the crystallographic c-axis. Hydrolysis of ß-Mg2C3 yields C3H4, as detected by mass spectrometry, while Raman and NMR measurements show clear C═C stretching near 1200 cm(-1) and (13)C resonances confirming the presence of the rare allylenide anion.

Deep mantle origin of large igneous provinces and komatiites.

Large igneous provinces (LIPs) resulted from intraplate magmatic events mobilizing volumes of magma up to several million cubic kilometers. LIPs and lavas with deep mantle sources have compositions ranging from komatiites found in Archean greenstone belts to basalts and picrites in Phanerozoic flood basalt and recent oceanic islands. In this study, we identify the mantle conditions appropriate to each type of lava based on an experimental study of the melting of pyrolite. The depth of the mantle source decreases from 600 to 700 km for the oldest komatiites to 100 to 300 km for picrites and basalts, and the extent of mantle melting ranges from 10 to 50%. We develop a geodynamical model that explains the origin of the hot mantle plumes capable of generating these melting P-T conditions. Within a superadiabatic temperature gradient persisting in the deep mantle, the ascent of hot mantle plumes creates excess temperatures up to 250 to 300 K by adiabatic decompression.

A new high-pressure technique for the measurement of low frequency seismic attenuation using cyclic torsional loading.

We report a new technique for torsional testing of materials under giga-pascal pressures, which uses a shearing module in a large-volume Paris-Edinburgh press in combination with high-resolution fast radiographic x-ray imaging. The measurement of the relative amplitude and phase lag between the cyclic displacement in the sample and a standard material (Al2O3) provides the effective shear modulus and attenuation factor for the sample. The system can operate in the 0.001-0.01 Hz frequency range and up to 5 GPa and 2000 K although high-temperature measurements may be affected by grain growth and plastic strain. Preliminary experimental results on San Carlos olivine are in quantitative agreement with previously reported Q-1 factors at lower pressure. This cyclic torsional loading method opens new directions to quantify the viscoelastic properties of minerals/rocks at seismic frequencies and under pressure-temperature conditions relevant to the Earth's mantle for a better interpretation of seismological data.

Stability and equation of state of face-centered cubic and hexagonal close packed phases of argon under pressure.

The compression of argon is measured between 10 K and 296 K up to 20 GPa and and up to 114 GPa at 296 K in diamond anvil cells. Three samples conditioning are used: (1) single crystal sample directly compressed between the anvils, (2) powder sample directly compressed between the anvils, (3) single crystal sample compressed in a pressure medium. A partial transformation of the face-centered cubic (fcc) phase to a hexagonal close-packed (hcp) structure is observed above 4.2-13 GPa. Hcp phase forms through stacking faults in fcc-Ar and its amount depends on pressurizing conditions and starting fcc-Ar microstructure. The quasi-hydrostatic equation of state of the fcc phase is well described by a quasi-harmonic Mie-Grüneisen-Debye formalism, with the following 0 K parameters for Rydberg-Vinet equation: [Formula: see text] = 38.0 Å[Formula: see text]/at, [Formula: see text] = 2.65 GPa, [Formula: see text] = 7.423. Under the current experimental conditions, non-hydrostaticity affects measured P-V points mostly at moderate pressure ([Formula: see text] 20 GPa).

High melting points of tantalum in a laser-heated diamond anvil cell.

In situ x-ray diffraction has been used to characterize the structural modifications of tantalum samples under intense laser irradiation, up to 135 GPa in a diamond anvil cell. Melting data points are obtained that do not confirm the previously reported anomalously low melting curve. Two effects are identified that might alter the melting determination of refractory metals such as Ta under high static pressures. First, a strong chemical reactivity of Ta with the pressure transmitting media and with carbon diffusing out from the surface of the anvils is observed. Second, pyrometry measurements can be distorted when the pressure medium melts. The strong divergence between ab initio calculations, shock measurements and static determination is resolved here and hence many theoretical interpretations are ruled out. Finally, the body-centered cubic phase is stable over the pressure-temperature range investigated.

Boron-MgO composite as an X-ray transparent pressure medium in the multi-anvil apparatus.

X-ray transparent materials are very beneficial for in situ X-ray experiments in the multi-anvil apparatus. We sintered machinable blocks of boron-MgO composites at 800-1000 °C under atmospheric pressure from a mixture of amorphous boron and brucite or Mg(OH)2. The machinability of composite blocks improved with an increase in the brucite content in the starting material; a brucite content higher than 15 wt. % showed reasonable machinability in forming various shapes such as octahedron, cylinder, and sleeve. We confirmed the feasibility of the boron-MgO pressure medium by successfully generating lower mantle pressure (>23 GPa); its pressure generation efficiency is comparable to that of a Cr2O3 doped MgO pressure medium. The boron-MgO composite is expected to be an excellent thermal insulator owing to the extremely low thermal conductivity of amorphous boron; we confirmed its better thermal insulation performance through a comparative heating test with a zirconia sleeve in a Cr2O3 doped MgO pressure medium. Constituting light elements, the boron-MgO composite has high X-ray transparency, which enables us to conduct various cutting edge X-ray measurements in the large volume multi-anvil apparatus.

Formation of bridgmanite-enriched layer at the top lower-mantle during magma ocean solidification.

Thermochemical heterogeneities detected today in the Earth's mantle could arise from ongoing partial melting in different mantle regions. A major open question, however, is the level of chemical stratification inherited from an early magma-ocean (MO) solidification. Here we show that the MO crystallized homogeneously in the deep mantle, but with chemical fractionation at depths around 1000 km and in the upper mantle. Our arguments are based on accurate measurements of the viscosity of melts with forsterite, enstatite and diopside compositions up to ~30 GPa and more than 3000 K at synchrotron X-ray facilities. Fractional solidification would induce the formation of a bridgmanite-enriched layer at ~1000 km depth. This layer may have resisted to mantle mixing by convection and cause the reported viscosity peak and anomalous dynamic impedance. On the other hand, fractional solidification in the upper mantle would have favored the formation of the first crust.

Dissociative melting of ice VII at high pressure.

We have used x-ray diffraction to determine the structure factor of water along its melting line to a static pressure of 57 GPa (570 kbar) and a temperature of more than 1500 K, conditions which correspond to the lower mantle of the Earth, and the interiors of Neptune and Uranus up to a depth of 7000 km. We have also performed corresponding first principles and classical molecular dynamics simulations. Above a pressure of 4 GPa the O-O structure factor is found to be very close to that of a simple soft sphere liquid, thus permitting us to determine the density of liquid water near the melting line. By comparing these results with the density of ice, also determined in this study, we find that the enthalpy of fusion (DeltaH(f)) increases enormously along the melting line, reaching approximately 120 kJ/mole at 40 GPa (compared to 6 kJ/mole at 0 GPa), thus revealing significant molecular dissociation of water upon melting. We speculate that an extended two-phase region could occur in planetary processes involving the adiabatic compression of water.

Pressure-induced chemical decomposition and structural changes of boric acid.

A combined synchrotron X-ray diffraction, Raman scattering, and infrared spectroscopy study of the pressure-induced changes in H(3)BO(3) to 10 GPa revealed a new high-pressure phase transition between 1 and 2 GPa followed by chemical decomposition into cubic HBO(2), ice-VI, and ice- VII at approximately 2GPa. The layered triclinic structure of H(3)BO(3) exhibits a highly anisotropic compression with maximum compression along the c direction, accompanied by a strong reduction of the interlayer spacing. The large volume variation and structural changes accompanying the decomposition suggest high activation energy. This yields a slow reaction kinetics at room temperature and a phase composition that is highly dependent on the specific pressure-time path followed by the sample. The combined results have been used to propose a mechanism for pressure-induced dehydration of H(3)BO(3) that implies a proton disorder in the system.