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Ubiquitous on Earth, \ensuremath{\alpha}-quartz plays an important role in modern science and technology. However, despite extensive research in the past, the mechanism of the polymorphic transitions of \ensuremath{\alpha}-quartz at high pressures remains poorly understood. Here, combining in situ single-crystal x-ray diffraction experiment and advanced ab initio modeling, we report two stability limits and competing transition pathways of \ensuremath{\alpha}-quartz under high pressure. Under near-equilibrium compression conditions at room temperature, \ensuremath{\alpha}-quartz transits to a new $P2/c$ silica phase via a structural intermediate. If the thermally activated transition is kinetically suppressed, the ultimate stability of \ensuremath{\alpha}-quartz is controlled by its phonon instability and \ensuremath{\alpha}-quartz collapses into a different crystalline phase. Our studies reveal that pressure-induced solid-state transformation of \ensuremath{\alpha}-quartz undergoes a succession of structural stability limits, due to thermodynamic and mechanical catastrophes, and exhibits a hierarchy of transition pathways contingent upon kinetic conditions.

The structural stability of methane hydrate under pressure at room temperature was examined by both in-situ single-crystal and powder X-ray diffraction techniques on samples with structure types I, II, and H in diamond-anvil cells. The diffraction data for types II (sII) and H (sH) were refined to the known structures with space groups Fd 3 m and P 6 3 / mmc , respectively. Upon compression, sI methane hydrate transforms to the sII phase at 120 MPa, and then to the sH phase at 600 MPa. The sII methane hydrate was found to coexist locally with sI phase up to 500 MPa and with sH phase up to 600 MPa. The pure sH structure was found to be stable between 600 and 900 MPa. Methane hydrate decomposes at pressures above 3 GPa to form methane with the orientationally disordered Fm 3 m structure and ice VII ( Pn 3 m ). The results highlight the role of guest (CH 4 )-host (H 2 O) interactions in the stabilization of the hydrate structures under pressure.

During the past decade, the radial x-ray diffraction method using a diamond anvil cell (DAC) has been developed at the X17C beamline of the National Synchrotron Light Source. The detailed experimental procedure used with energy dispersive x-ray diffraction is described. The advantages and limitations of using the energy dispersive method for DAC radial diffraction studies are also discussed. The results for FeO at 135 GPa and other radial diffraction experiments performed at X17C are discussed in this report.

The synchrotron radiation X-ray diffraction technique developed for in situ study at high pressure and temperature has also been used to investigate microscopic mineral inclusions in ultra-high-pressure metamorphic rocks and deep-mantle samples. Present study added two more examples of successful utilization of synchrotron radiation X-ray diffraction technique for in situ investigations of fine-grained (0.5―30 μm in size) minerals in very thin shock melt veins of the Suizhou meteorite: (i) X-ray diffraction measurement of extremely small-sized vein matrix minerals, and (ii) identification of the micron-sized new mineral tuite embedded in the vein matrix. It has been revealed that the fine-grained vein matrix consists of well crystallized garnet, kama-cite and troilite, and the powder diffraction pattern consisting of 17 lines with d-values, intensities ( I ), relative intensities ( I / I o ) and Miller indices, as well as the cell parameters for the new mineral tuite has also been successfully obtained. The result of present investigations has enriched the content of dynamic high-pressure mineralogy and that of Earth’s mantle geochemistry.

The high-pressure, high-temperature behavior of iron has been investigated to 161 GPa and 3000 K by in situ synchrotron X-ray diffraction with double-side laser-heated diamond anvil cells. We found that only α-, γ- and e-Fe can be clearly verified as the stable solid phase in the P–T range studied. Only e-Fe is observed from deep lower mantle (∼1500 km) to outer core conditions. Within the P–T range examined, we did not observe a significant change with pressure or temperature on the c/a ratio of e-Fe. The melting curve of iron has been determined to 105 GPa. A Lindeman law fit gives a melting point of iron at the inner core boundary of 5800 (±200) K, which provides an upper bound on the temperature at that depth. We also examine numerous experimental factors that may complicate the analysis of high P–T diffraction data, and discuss the effects of sample stress on the X-ray diffraction results.

Recent advances in high-pressure diamond anvil cell experiments include high-energy synchrotron x-ray techniques as well as new cell designs and gasketing procedures. The success of high-pressure experiments usually depends on a well-prepared sample, in which the gasket plays an important role. Various gasket materials such as diamond, beryllium, rhenium, and stainless steel have been used. Here we introduce amorphous boron as another gasket material in high-pressure diamond anvil cell experiments. We have applied the boron gasket for laser-heating x-ray diffraction, radial x-ray diffraction, nuclear resonant inelastic x-ray scattering, and inelastic x-ray scattering. The high shear strength of the amorphous boron maximizes the thickness of the sample chamber and increases the pressure homogeneity, improving the quality of high-pressure data. Use of amorphous boron avoids unwanted x-ray diffraction peaks and reduces the absorption of incident and x rays exiting the gasket material. The high quality of the diffraction patterns makes it possible to refine the cell parameters with powder x-ray diffraction data under high pressure and high temperature. The reactivity of boron prevents its use at high temperatures, however. When heated, boron may also react with the specimen to produce unwanted phases. The relatively porous boron starting material at ambient conditions also poses some challenges for sample preparation.

New high-pressure measurements reveal the coupling of strain and order parameter in the pressure-induced ferroelastic transition in dense SiO2. Single-crystal X-ray diffraction measurements in quasi-hydrostatic media reversibly probe the spontaneous strain in the vicinity of the P42=mnm! Pnnm transition near 50 GPa, and indicate weak first-order character. A Landau model is developed that quantitatively relates all of the spectroscopic, elastic, structural, and thermodynamic data for the system. The elastic instability at the transition gives rise to anomalies in the Raman spectrum, which are expected to be a general feature of such pressure-induced transitions. q 2000 Elsevier Science Ltd. All rights reserved.

Solid methane (CH(4)) was compressed up to 202 GPa at 300 K in a diamond-anvil cell. The crystal structure and equation of state over this entire range were determined from angle dispersive X-ray diffraction results. CH(4) undergoes phase transitions from rhombohedral to a simple cubic phase at 19 GPa and from simple cubic to a higher pressure cubic phase at approximately 94 GPa. This higher pressure cubic phase was stable to the maximum pressure investigated. Combined with previous optical measurements, it was found that at room temperature compressed CH(4) remains an insulator with cubic structure to 202 GPa. (C) 2009 Elsevier B. V. All rights reserved.

Lattice strains were measured as a function of the angle ψ between the diffracting plane normal and the stress axis of a diamond anvil cell in a layered sample of molybdenum and gold. The sample was compressed over the range 5–24 GPa and the lattice strains were measured using energy-dispersive x-ray diffraction. As ψ is varied from 0° to 90°, the mean lattice parameter of molybdenum increases by up to 1.2% and that of gold increases by up to 0.7%. A linear relationship between Q(hkl), which is related to the slope of the measured d spacing versus 1−3 cos2 ψ relation, and 3Γ(hkl), a function of the Miller indices of the diffracting plane, is observed for both materials as predicted by theory. The pressure dependence of the uniaxial stress t for gold from this and other recent studies is given by t=0.06+0.015P, where P is the pressure in GPa. The uniaxial stress in molybdenum can be described by t=0.46+0.13P. Using gold as an internal pressure standard, the equation of state of molybdenum depends strongly ...

The equations for the lattice strains produced by nonhydrostatic compression are presented for all seven crystal systems in a form convenient for analyzing x-ray diffraction data obtained by newly developed methods. These equations have been used to analyze the data on cubic (bcc α-Fe) and hexagonal (hcp e-Fe) systems. The analysis gives information on the strain produced by the hydrostatic stress component. A new method of estimating the uniaxial stress component from diffraction data is presented. Most importantly, the present analysis provides a general method of determining single crystal elastic constants to ultrahigh pressures.

High-pressure energy dispersive X-ray diffraction of wustite has been obtained with three types of diamond cells; each one is designed to optimize a type of in situ study, namely single-crystal X-ray diffraction, deviatoric strain measurement, or simultaneous high-P-T experimentation. The results demonstrate that above 17 GPa at 300 K wustite undergoes a displacive transition from B1 to a rhombohedral structure, and above 90 GPa at 600 K, a second transition to the NiAs structure. Many of the earlier inconsistencies concerning the structure and properties of wustite at high pressures can be attributed to the extreme softening of the C44 elastic modulus at pressures above 10 GPa.

Using in situ high-pressure x-ray diffraction methods, the compressibility of 30nm 3C–SiC nanocrystals was studied under hydrostatic conditions while helium was used as pressure transmitting medium, as well as under nonhydrostatic conditions without pressure medium. No threshold pressure phenomenon was observed for the compressibility of the nanocrystals during compression in hydrostatic conditions, while the critical pressure around 10.5GPa was observed during nonhydrostatic compression. These indicate that the threshold pressure phenomena, recently reported that the nanocrystals initially exhibited much higher bulk modulus below the threshold pressure during compression [Appl. Phys. Lett. 83, 3174 (2003); J. Phys. Chem. 107, 14151 (2003)], were mainly caused by the nonhydrostatic effect instead of a specific feature of nanocrystals upon compression. The bulk modulus of 3C–SiC nanocrystals is estimated as 220.6±0.6GPa based on the hydrostatic compression data.

Two experiments were conducted compressing Ta, Re, Pt, and an Fe-Si alloy to ultrahigh pressures using single-crystal chemical vapor deposition (CVD) and natural diamonds. In situ energy-dispersive and angle-dispersive x-ray diffraction were used to determine pressure from known equations of state. We demonstrate that CVD diamonds can be used in diamond anvil cells to reach pressures of nearly 200 GPa.

Compressed under ambient temperature, graphite undergoes a transition at approximately 17 gigapascals. The near K-edge spectroscopy of carbon using synchrotron x-ray inelastic scattering reveals that half of the pi-bonds between graphite layers convert to sigma-bonds, whereas the other half remain as pi-bonds in the high-pressure form. The x-ray diffraction pattern of the high-pressure form is consistent with a distorted graphite structure in which bridging carbon atoms between graphite layers pair and form sigma-bonds, whereas the nonbridging carbon atoms remain unpaired with pi-bonds. The high-pressure form is superhard, capable of indenting cubic-diamond single crystals.

We report the first experimental observation of a liquid-liquid phase transition in the monatomic liquid metal cerium, by means of in situ high-pressure high-temperature x-ray diffraction experiments. At 13 GPa, upon increasing temperature from 1550 to 1900 K high-density liquid transforms to a low-density liquid, with a density difference of 14%. Theoretic models based on ab initio calculations are built to investigate the observed phase behavior of the liquids at various pressures. The results suggest that the transition primarily originates from the delocalization of $f$ electrons and is deemed to be of the first order that terminates at a critical point.

Effects of pressure on lattice parameters and molar volume of diaspore were studied to 25.5 GPa at 300 K by polycrystalline X-ray diffraction techniques. The pressure-volume data fit with a second-order Birch-Murnaghan equation of state give a bulk modulus K 0 = 167.5 GPa by Ruoff and previously reported, but unsubstantiated, value of K 0 = 85 GPa by Ruoff and Vanderborgh [ Phys. Rev. Lett. 66, 754 (1991)]. Thermodynamic calculation indicates that hydrogen and ruby are stable relative to diaspore and aluminum to pressures above 200 GPa.

Compressing glassy carbon above 40 GPa, we have observed a new carbon allotrope with a fully $s{p}^{3}$-bonded amorphous structure and diamondlike strength. Synchrotron x-ray Raman spectroscopy revealed a continuous pressure-induced $s{p}^{2}$-to-$s{p}^{3}$ bonding change, while x-ray diffraction confirmed the perseverance of noncrystallinity. The transition was reversible upon releasing pressure. Used as an indenter, the glassy carbon ball demonstrated exceptional strength by reaching 130 GPa with a confining pressure of 60 GPa. Such an extremely large stress difference of $g70\text{ }\text{ }\mathrm{GPa}$ has never been observed in any material besides diamond, indicating the high hardness of this high-pressure carbon allotrope.

The use of nanoscale x-ray probes overcomes several key limitations in the study of materials up to multimegabar (> 200) pressures, namely, the spatial resolution of measurements of multiple samples, stress gradients, and crystal domains in micron to submicron size samples in diamond-anvil cells. Mixtures of Fe, Pt, and W were studied up to 282 GPa with 250–600 nm size synchrotron x-ray absorption and diffraction probes. The probes readily resolve signals from individual materials, between sample and gasket, and peak pressures, in contrast to the 5-μm-sized x-ray beams that are now becoming routine. The use of nanoscale x-ray beams also enables single-crystal x-ray diffraction studies in nominally polycrystalline samples at ultrahigh pressures, as demonstrated in measurements of (Mg,Fe)SiO 3 postperovskite. These capabilities have potential for driving a push toward higher maximum pressures and further miniaturization of high-pressure devices, in the process advancing studies at extreme conditions.

Recent high-pressure studies have shown that an electronic spin transition of iron in ferropericlase, an expected major phase of Earth's lower mantle, results in changes in its properties, including density, incompress- ibility, radiative thermal conductivity, electrical conduc- tivity, and sound velocities. To understand the rheology of ferropericlase across the spin transition, we have used in situ radial X-ray diffraction techniques to examine ferro- periclase, (Mg0.83,Fe0.17)O, deformed non-hydrostatically in a diamond cell up to 81 GPa at room temperature. Compared with recent quasi-hydrostatic studies, the range of the spin transition is shifted by approximately 20 GPa as a result of the presence of large differential stress in the sample. We also observed a reduction in incompressibility and in the unit cell volume of 3% across the spin transition. Our radial X-ray diffraction results show that the {0 0 1} texture is the dominant lattice preferred orientation in ferropericlase across the spin transition and in the low-spin state. Viscoplastic self-consistent polycrystal plasticity simulations suggest that this preferred orientation pattern is produced by {1 1 0}\1-10( slip. Analyzing our radial X-ray diffraction patterns using lattice strain theory, we evaluated the lattice d-spacings of ferropericlase and Mo as a function of the w angle between the compression direc- tion and the diffracting plane normal. These analyses give the ratio between the uniaxial stress component (t) and the shear modulus (G) under constant stress condition, which represents a proxy for the supported differential stress and elastic strength. This ratio in the mixed-spin and low-spin states is lower than what is expected from previous studies of high-spin ferropericlase, indicating that the spin transi- tion results in a reduced differential stress and elastic strength along with the volume reduction. The influence of the spin transition on the differential stress and strength of ferropericlase is expected to be less dominant across the wide spin transition zone at high pressure-temperature conditions relevant to the lower mantle.

[1] We present a multitechnique approach to experimentally determine the elastic anisotropy of polycrystalline hcp Fe at high pressure. Directional phonon measurements from inelastic X-ray scattering on a sample with lattice preferred orientation at 52 GPa in a diamond anvil cell were coupled with X-ray diffraction data to determine the elastic tensor. Comparison of the results from this new method with the elasticity determined by lattice strain analysis of radial X-ray diffraction measurements showed significant differences, highlighting the importance of strength anisotropy in hcp Fe. At 52 GPa, we found that a method which combines results from inelastic scattering and pressure-volume measurements gives a shape in the velocity anisotropy close to sigmoidal (with a faster c and slower a axis) a smaller magnitude in the anisotropy and compared to velocities based on the lattice strain method which gives a bell shape velocity distribution with the fast direction between the c and a axes. We used additional results from nuclear resonant inelastic X-ray scattering to constrain errors and provide additional validation of the accuracy of our results.

A phase transition was observed at 63-69 GPa and room temperature in vanadium with synchrotron x-ray diffraction. The transition is characterized as a rhombohedral lattice distortion of the body-centered-cubic vanadium without a discontinuity in the pressure-volume data, thus representing a novel type of transition that has never been observed in elements. Instead of driven by the conventional s-d electronic transition mechanism, the phase transition could be associated with the softening of C44 trigonal elasticity tensor that originates from the combination of Fermi surface nesting, band Jahn-Teller distortion, and electronic topological transition.

When subjected to high pressure and extensive x-radiation, water (H 2 O) molecules cleaved, forming O–O and H–H bonds. The oxygen (O) and hydrogen (H) framework in ice VII was converted into a molecular alloy of O 2 and H 2 . X-ray diffraction, x-ray Raman scattering, and optical Raman spectroscopy demonstrated that this crystalline solid differs from previously known phases. It remained stable with respect to variations in pressure, temperature, and further x-ray and laser exposure, thus opening new possibilities for studying molecular interactions in the hydrogen-oxygen binary system.

A natural chromite single crystal was compressed in a helium pressure medium to just above 35 GPa at ambient temperature and studied with energy-dispersive x-ray diffraction. The volume compression of the cubic, spinel-type structure was fit to a third-order Birch-Murnaghan equation of state with parameters a0= 8.338(4) Å, V0 = 579.6(9) Å3, K0 =179(10) GPa, and K' = 3.9(9) up to 29 GPa. A distortive phase transition was discovered at higher pressures to a CaAl2O4-type orthorhombic structure, with two cubic unit-cell axes increasing and the third decreasing with increasing pressure. The transition can be fit to a Landau-type strain-order formulism with approximately 5% volume decrease from the cubic phase at 35 GPa. The transition may be triggered by electronic or magnetic transitions in the 3d elements Fe and Cr cations.

International audience; The elasticity and plasticity of materials at high pressure are of great importance for the fundamental insight they provide on bonding properties in dense matter and for applications ranging from geophysics to materials technology. We studied pressure-solidified argon with a boron–epoxy–beryllium composite gasket in a diamond anvil cell (DAC). Employing monochromatic synchrotron x-radiation and imaging plates in a radial diffraction geometry (Singh et al 1998 Phys. Rev. Lett. 80 2157; Mao et al 1998 Nature 396 741), we observed low strength in solid argon below 20 GPa, but the strength increases drastically with applied pressure, such that at 55 GPa, the shear strength exceeded 2.7 GPa. The elastic anisotropy at 55 GPa was four times higher than the extrapolated value from 30 GPa. Extensive (111) slip develops under uniaxial compression, as manifested by the preferred crystallographic orientation of (220) in the compression direction. These macroscopic properties reflect basic changes in van der Waals bondings under ultrahigh pressures.

The pressure dependence of the internal structural parameter u of the wurtzite phase of ZnO was studied using high resolution angular dispersive x-ray diffraction up to 12 GPa in a helium pressure medium. The u parameter increases with pressure up to about 0.430 at about 5.6 GPa, and then rapidly decrease to about 0.380 during the phase transition. Two models of the phase transition path were proposed recently by first-principles calculations [A. M. Saitta and F. Decremps, Phys. Rev. B 70, 035214 (2004); S. Limpijumnong and S. Jungthawan, Phys. Rev. B 70, 054104 (2004)]. These possible mechanisms responsible for the wurtzite-to-rocksalt phase transition under high pressure are experimentally evaluated based on our results. The bulk moduli of the wurtzite and rocksalt phase at zero pressure were estimated as 135.3 {+-} 1.8 and 177.4 {+-} 4.6 GPa, respectively.

International audience; Room temperature investigations of the single-crystal elastic moduli and anisotropy of the phase of iron are performed up to 30.3 GPa using the radial X-ray diffraction technique. The accuracy of the calculated elastic moduli has improved compared to previous measurements using similar techniques because of an increase in accuracy of the measurement, confinement of the sample to limit the effect of plasticity, and better calibration of the stress conditions. The aggregate shear modulus that we obtain is in good agreement with a variety of other experimental deductions but differs from first-principles calculations. The effects of the calibration of stress and micromechanical model on the deduction of elastic moduli and elastic anisotropy are discussed in detail. The anisotropy we obtain has the same order of magnitude as first-principles calculations but the direction is reversed, with a weaker amplitude that previous measurements.

[1] We studied the nuclear resonant x-ray scattering of iron hydride (FeHx) up to 52 GPa. Coupled with hydrostatic x-ray diffraction data, the partial phonon density of states measured by nuclear resonant inelastic x-ray scattering provides information on sound velocities and the Fe contribution to thermodynamic parameters. In particular it constrains the aggregate shear velocity and shear modulus for comparison to seismic observations. We found that VS (km/sec) = 0.023*P (GPa) + 3.2. A loss of magnetism was observed with synchrotron Mossbauer spectroscopy at 22 GPa, lower than theoretically predicted but consistent with the observed anomalous velocity behavior. Results confirm that FeHx could be a major light element bearing phase for explaining the core density deficit relative to pure Fe. Formation of FeHx by reaction with water would be expected to leave a signature in the mantle.

Attributed to their specific atomic bonding, the soft, graphite-like, hexagonal boron nitride (h-BN) and its superhard, diamond-like, cubic polymorph (c-BN) are important technological materials with a wide range of applications1. At high pressure and temperature, h-BN can directly transform to a hexagonal close-packed polymorph (w-BN)2 that can be partially quenched after releasing pressure. Previous theoretical calculations3,4,5 and experimental measurements (primarily on quenched samples)6,7,8,9 provided substantial information on the transition, but left unsettled questions due to the lack of in situ characterization at high pressures. Using inelastic X-ray scattering to probe the boron and nitrogen near K-edge spectroscopy, here we report the first observation of the conversion process of boron and nitrogen sp2- and p-bonding to sp3 and the directional nature of the sp3 bonding. In combination with in situ X-ray diffraction probe, we have further clarified the structure transformation mechanism. The present archetypal example opens two enormous, element-specific, research areas on high-pressure bonding evolutions of boron and nitrogen; each of the two elements and their respective compounds have displayed a wealth of intriguing pressure-induced phenomena10 that result from bonding changes, including metallization11,12, superconductivity13,14, semiconductivity15, polymerization16 and superhardness2,17,18.

X-ray diffraction measurements have been carried out above 300 GPa for the first time using Pt as a primary pressure standard. The equations of state of iron up to 304 GPa and of CsI up to 302 GPa have been obtained. These materials can therefore be used as secondary pressure calibrants.

Single-crystal brucite, Mg(OH)2, was studied to 14 GPa in a quasi-hydrostatic pressure medium using a diamond anvil cell and energy-dispersive synchrotron x-ray diffraction. The parameters of a third-order Birch-Murnaghan equation of state fit to the data are: K OT=42(2) GPa, and (∂K OT/∂P)T= 5.7(5). The bulk modulus is significantly lower than that obtained in recent shock compression and powder x-ray diffraction experiments under non-hydrostatic conditions. No evidence was found for a transition involving the Mg -O sub-structure over the pressure range of these experiments. This implies that the structural change previously identified at high pressure by Raman spectroscopy probably involves rearrangement of hydrogen atoms, leaving the Mg — O substructure largely unaffected.

Polycrystalline rhenium in the form of a powder contained in a two-stage gasket was compressed in a diamond anvil cell. No pressure medium was used to ensure that maximum nonhydrostatic stresses that rhenium can support were produced. The pressure was increased in steps to a maximum of 250 GPa and the diffraction pattern recorded at each pressure using energy dispersive technique. The differential stress t, a measure of the compressive strength, was determined at any given pressure from the offset between the measured unit cell volume and volume computed from the pressure-volume relation under hydrostatic pressure. The data suggest that t is 2.5 GPa at a pressure of 5 GPa and increases linearly to 26 GPa at 250 GPa. The present data agree well with those obtained from the radial diffraction data to 37 GPa in an earlier study but differ significantly from the results of another study. Though comparable with the theoretical strength of ideal solids, the observed strengths are extremely large for a polycrystalline aggregate of a solid. The pure pressure effect on the strength described by the shear modulus scaling is inadequate to account for such a large increase of strength with pressure . It is suggested that the major contribution to strength comes from the strain hardening of rhenium that arises due to plastic deformat ion of the sample during nonhydrostatic compression in a diamond anvil cell.

An energy dispersive x‐ray diffraction technique employing superconducting wiggler synchrotron radiation for high‐pressure research is described. The incident beam is controlled by a double slit system capable of producing uniform beam sizes of 5 to 10 μm impinging on diamond‐anvil cell samples. Alignment of the incident beam, sample, and diffracted beam is achieved by an automated θ−2θ system with positional accuracy of 0.001 mm and angle accuracy of 0.001°. Internal x‐ray standards and ruby fluorescence are used for pressure measurement. Crystal structures, equations of state, and phase transitions of polycrystalline and single‐crystal samples to multimegabar pressure and at temperatures of 50 to 1100 K have been studied.

The high pressure behavior of titanium nitride (TiN) was investigated using synchrotron radial x-ray diffraction (RXRD) under nonhydrostatic compression up to 45.4 GPa in a diamond-anvil cell. We obtained the hydrostatic compression equation of state of TiN. Fitting to the third-order Birch–Murnaghan equation of state, the bulk modulus derived from nonhydrostatic compression data varies from 232 to 353 GPa, depending on angle ψ, the orientation of the diffraction planes with respect to the loading axis. The RXRD data obtained at ψ=54.7° yield a bulk modulus K0=282±9 GPa with pressure derivative K0′ fixed at 4. We have analyzed the deformation mechanisms by analyzing the (111), (200), (220), (311), and (222) peaks in the x-ray diffraction under pressures. The ratio of uniaxial stress component to shear modulus t/G ranges from 0.007–0.027 at the pressure of 6.4–45.4 GPa. It was found that the TiN sample could support a maximum uniaxial stress component t of 8.6 GPa, when it started to yield at 45.4 GPa under uniaxial compression. And the aggregate elastic moduli of TiN at high pressure were determined from the synchrotron RXRD measurements.

The lattice parameter of magnesiowustite (Mg0.6Fe0.4)O has been measured up to a pressure of 30 GPa and a temperature of 800 K, using an external heated diamond anvil cell and diffraction using X-rays from a synchrotron source. The experiments were conducted under quasi-hydrostatic condition, using neon as a pressure transmitting medium. The experimental P-V-T data were fitted to a thermal-pressure model with the isothermal bulk modulus at room temperature K T0 = 157 GPa, (∇K TO /∇P) T =4, (∇K T /∇T) P =-2.7(3) × 10-2 GPa/K, (∇K T /∇T) v =-0.2(2) × 10-2 GPa/K and the Anderson-Gruneisen parameter δ T =4.3(5) above the Debye temperature. The data were also fitted to the Mie-Gruneisen thermal equation of state. The least-squares fit yields the Debye temperature θ DO = 500(20) K, the Gruneisen parameter γ 0=1.50(5), and the volume dependence q=1.1(5). Both thermal-pressure models give consistent P-V-T relations for magnesiowustite to 140 GPa and 4000 K. The P-V-T relations for magnesiowustite were also calculate by using a modified high-temperature Birch-Murnaghan equation of state with a δ t of 4.3. The results are consistent with those calculated by using the thermal-pressure model and the Mie-Gruneisen relation to 140 GPa and 3000 K.

Attention is given to the lattice parameters of beta phase (Mg(0.84)Fe(0.16))2SiO4 determined by X-ray diffraction using synchrotron radiation under simultaneous high-pressure and high-temperature conditions. The experiments were conducted up to a pressure of 26 GPa and a temperature of 900 K. High pressures were generated in a Mao-Bell type diamond anvil cell using neon gas as a pressure medium. The sample was heated with an external Ni80Cr20 wire heater. Gold was used as an internal high-pressure calibrant at high temperature. The experimental data indicated the anisotropic behavior of the beta phase at high pressure and temperature, i.e., the c axis is about 35-percent more expansible and about 25-percent more compressible than the a and b axes. A value of 5.1 +/-0.8 was found for the Anderson-Grueneisen parameter. The derived thermodynamic parameters for the beta phase are summarized.

Results are reported on a room temperature static compression study of iron and the Fe(0.8)Ni(0.2) alloy to above 260 GPa, which provide direct pressure-volume measurements on geophysically important materials at the conditions close to those at the inner core boundary. The diffraction patterns obtained by XRD indicate that pure iron remains in the hcp structure to 304 GPa and that Fe(0.8)Ni(0.2) is stable to at least 255 GPa. The results of this study, in conjunction with work at higher temperatures, will make it possible to address directly the question of the composition of the inner core with a level of certainty that were previously applicable only to the mantle.

X-ray diffraction measurements have been carried out on cesium iodide (CsI) to 302 gigapascals with a platinum pressure standard. The results indicate that above 200 gigapascals CsI at 300 K has a hexagonal close-packed crystal structure with the ideal c / a ratio of 1.63 ± 0.01. The crystal structure and pressure-volume relations converge at high pressure with those of solid xenon, which is isoelectronic with CsI. The results indicate a significant loss of ionic bonding in the hexagonal close-packed metallic phase of CsI at ultrahigh pressure.

Using energy-dispersive x-ray diffraction techniques together with the theory describing lattice strains under nonhydrostatic compression, the behavior of a layered sample of gold and rhenium has been studied at pressures of 14--37 GPa. For gold, the uniaxial stress component t is consistent with earlier studies and can be described by $t=0.06+0.015P$ where P is the pressure in GPa. The estimated single-crystal elastic moduli are in reasonable agreement with trends based on extrapolated low-pressure data. The degree of elastic anisotropy increases as $\ensuremath{\alpha},$ the parameter which characterizes stress-strain continuity across grain boundaries, is reduced from 1.0 to 0.5. For rhenium, the apparent equation of state has been shown to be strongly influenced by nonhydrostatic compression, as evidenced by its dependence on the angle $\ensuremath{\psi}$ between the diffracting plane normal and the stress axis. The bulk modulus obtained by inversion of nonhydrostatic compression data can differ by nearly a factor of 2 at angles of $0\ifmmode^\circ\else\textdegree\fi{}$ and $90\ifmmode^\circ\else\textdegree\fi{}.$ On the other hand, by a proper choice of $\ensuremath{\psi},$ d spacings corresponding to quasihydrostatic compression can be obtained from data obtained under highly nonhydrostatic conditions. The uniaxial stress in rhenium over the pressure range from 14--37 GPa can be described by $t=2.5+0.09P.$ The large discrepancy between x-ray elastic moduli and ultrasonic data and theoretical calculations indicates that additional factors such as texturing or orientation dependence of t need to be incorporated to more fully describe the strain distribution in hexagonal-close-packed metals.