High-pressure radial X-ray diffraction study of osmium to 58 GPa

Nonhydrostatic compression behavior of osmium (Os) was investigated up to 58.2 GPa using radial X-ray diffraction (RXRD) together with lattice strain theory in a diamond-anvil cell. The apparent bulk modulus of Os derived from RXRD data varies from 262 GPa to 413 GPa, depending on Ψ, the orientation of the diffraction planes with respect to the loading axis. Fitting to the third-order Birch-Murnaghan equation of state, the RXRD data obtained at Ψ = 54.7° yields a bulk modulus K₀ = 390 ± 6 GPa with pressure derivative K^′ ₀ fixed at 4. The ratio of differential stress to shear modulus t/G ranges from 0.024 to 0.029 at the pressures of 15.7–58.2 GPa. The yield strength was observed to increase with compression and reach the value of 11.7 GPa at the highest pressure. This confirms that Os is the strongest known pure metallic material compared with the reported stiff elemental metals such as W, Mo and Re. It was found that the apparent c/a ratio changed with the nonhydrostatic compression, as well as the orientation Ψ in our experiments. Moreover, the aggregate moduli of Os at high pressure were determined from the RXRD measurements.     

Compression behavior of NiO in a diamond cell

Abstract

The compressibility of synthetic polycrystalline NiO was studied in a diamond anvil cell at room temperature utilizing two different X-ray sources. A standard film with a conventional X-ray source and the energy dispersive X-ray diffraction (EDXRD) method with synchrotron radiation were used for data acquisition. In the film method, the sample was compressed in a 4:1 methanol to ethanol solution up to 7 GPa with ruby fluorescence as a pressure calibrant. In the energy dispersive method, NiO powder was mixed with gold and compressed in two different conditions: gasketed and ungasketed up to 30 GPa. In the gasketed run, water was used as the pressure transmitting medium while gold was used as pressure calibrant in both runs.

Hydrostatic compression of NiO in both diffraction methods yields a bulk modulus (K _o) of 187 ± 7 GPa assuming K′ = 4. The compression of gasketed NiO of the synchrotron experiment, however, showed an obvious break at pressure exceeding 4 GPa due to the loss of hydrostaticity. NiO in a nonhydrostatic condition behaves with less compressibility than the hydrostatic results with a nominal K _o of 238 ± 10 GPa. The lower compressibility of NiO in synchrotron runs is attributed to the uniaxial loading effect which was more easily detected by the EDXRD geometry. The discrepancy in the bulk modulus can be attributed to the contrast in the shear strength between the sample and pressure medium and the Poisson effect of the sample under uniaxial loading.     

High-pressure in-situ X-ray diffraction and Raman spectroscopy of Ca2AlFeO5 brownmillerite

The behavior of Ca₂AlFeO₅ brownmillerite was studied by in situ synchrotron X-ray diffraction and Raman spectroscopy at 300?K with pressures up to 26.5 and 32.1 GPa, respectively. A reversible structural phase transition was observed. The P–V data were fitted by a third-order Birch–Murnaghan equation of state, and the isothermal bulk modulus was obtained as K₀?=?181.9(76) GPa with K₀′_?=?4.4(17). If K₀′ was fixed to 4, K₀ was obtained as 183.8(20) GPa. Ca₂AlFeO₅ brownmillerite shows an axial elastic anisotropy since the b-axis is more compressible than a- and c-axis. Combined with previous results, the isothermal bulk modulus and axial compressibility of Ca₂AlFeO₅ brownmillerite increase with more Al incorporated in the structure. The Raman spectra of Ca₂AlFeO₅ brownmillerite were analyzed and the pressure coefficients vary from 2.23 to 4.90?cm^?1/GPa. The isothermal mode Grüneisen parameters range from 0.83 to 1.77 and the thermal Grüneisen parameter is determined as 1.08(11).     

High-pressure Raman and X-ray studies of barite,BaSO4

High-pressure Raman spectroscopic and X-ray diffraction experiments of barite, BaSO₄, were carried out in a diamond anvil cell up to 25?GPa at room temperature. On the basis of the changes in the diffraction patterns and the variation of lattice parameters with pressure, it is inferred that barite undergoes a phase transformation at 10?GPa. The phase transition accompanies the change in the force constant of vibrational modes in barite. Further compression beyond the phase transition causes the distortion of SO₄ tetrahedron as indicated by the splitting in the SO₄ stretching modes. Both X-ray and Raman data support that the phase transition in BaSO₄ is reversible. The compression data yield a bulk modulus of 63?±?2?GPa for barite. Barite shows anisotropic compressibility along three crystallographic axes with c being the most compressible axis.     

P–V–T equation of state of rhodium oxyhydroxide

A high pressure X-ray diffraction study of RhOOH was carried out up to 17.44?GPa to investigate the compression behavior of an oxyhydroxide with an InOOH-related structure. A fit to the third-order Birch–Murnaghan equation of state gave K₀?=?208?±?6?GPa, and K′?=?9.4?±?1.3. The temperature derivative of the bulk modulus was found to be ?K/?T?=??0.06?±?0.02?GPa K^?1. The refined parameters for volume thermal expansion were α₀?=?2.7?±?0.3?×?10^?5 K^?1; α₁?=?1.7?±?1.1?×?10^?8 K^?2 in the polynomial form (α(T)?=?α_0?+?α₁(T?300)). Our results show that RhOOH is very incompressible, and has a higher bulk modulus than other InOOH-structured oxyhydroxides (e.g. δ-AlOOH, ε-FeOOH, and γ-MnOOH).     

Dual mode ultrasonic interferometry in multi-anvil high pressure apparatus using single-crystal olivine as the pressure standard

Acoustic measurements of compressional (P) and shear (S) wave travel times were performed in a 1000-ton uniaxial split-cylinder apparatus (USCA-1000) of the Kawai-type up to 10?GPa at room temperature, using dual mode lithium niobate transducers and ultrasonic interferometry. The cell pressures were calibrated continuously by in-situ measurements of the travel times in a single crystal San-Carlos olivine buffer rod inside the cell assembly. Elastic compressional and shear wave velocities in a dense, fine-grained polycrystalline Al₂O₃ were measured simultaneously to 10?GPa; from these data, the elastic moduli and their pressure derivatives were obtained for the longitudinal modulus {L ₀?=?461(3)?GPa, L ₀′?=?7.0(1)}, the shear modulus {G ₀?=?162(2)?GPa, G ₀′?=?1.9(1)} and the bulk modulus {K ₀?=?245(3)?GPa, K ₀′?=?4.5(1)}.     

In situ high-pressure X-ray diffraction experiments and ab initio calculations of Co2P

In situ high-pressure experiments of Co2P are carried out by means of angle dispersive X-ray diffraction with diamond anvil cell technique. No phase transition is observed in the present pressure range up to 15 GPa at room temperature, even at high temperature and 15 GPa. Results of compression for Co2P are well presented by the second-order Birch-Murnaghan equation of state with V0 = 130.99(2)3 (1=0.1 nm) and K0 = 160(3) GPa. Axial compressibilities are described by compressional modulus of the axis: Ka = 123(2) GPa, Kb = 167(8) GPa and Kc = 220(7) GPa. Theoretical calculations further support the experimental results and indicate that C23-type Co2P is stable at high pressure compared with the C22-type phase.     

Studies on Im-3-type KSbO3 using high pressure X-ray diffraction and Raman spectroscopy

In situ X-ray diffraction and Raman scattering experiments using a diamond anvil cell revealed that Im-3-type KSbO₃ remains stable up to 40.5?GPa with a bulk modulus K₀?=?101.6 (7)?GPa. Rietveld structure refinements and mode Grüneisen parameters suggested that the stability mechanism of this three-dimensional cubic tunnel structure was attributed to the isotropic compression for all types of Sb–O bonding in the unit of SbO₆ octahedron. Isotropic structure adjustment with external pressure reflected the nature that Im-3-type KSbO₃ model structure has a high ionic tolerance with a change in the chemical pressure in the isomorphous substitutions.     

In-situ X-ray diffraction study on β-CrOOH at high pressure and high-temperature

ABSTRACT

High pressure hydrous phases with distorted rutile-type structure have attracted much interest as potential water reservoirs in the Earth’s mantle. An in-situ X-ray diffraction study of β-CrOOH was performed at high pressures of up to 6.2?GPa and high-temperatures of up to 700?K in order to clarify the temperature effect on compression behaviors of β-CrOOH. The P-V-T data fitted to a Birch–Murnaghan equation of state yielded the following results: isothermal bulk modulus K_T0?=?191(4)?GPa, temperature derivative (?K_T/?T)_P?=??0.04(2)?GPa?K^?1, and volumetric thermal expansion coefficient α?=?3.3(2)?×?10^?5?K^?1. In this study, at 300?K, the a-axis became less compressible at pressures above 1–2?GPa. We found that the pressure where the slopes of a/b and a/c ratios turned positive increased with temperature. This is the first experimental study indicating the temperature dependence of the change in the axial compressibility in distorted rutile-type M³⁺OOH.     

High-pressure powder diffraction study of TaO2F

TaO₂F, with a ReO₃-type structure, has been studied at up to 12.8 GPa using monochromatic synchrotron powder diffraction and diamond anvil cells. Two-phase transitions at ∼0.7 and 4 GPa were observed on compression. Below ∼0.7 GPa the cubic material was found to have a bulk modulus (K₀) of 36(3) GPa (K_p fixed at 4.0), similar to that reported for NbO₂F but much smaller than that of ReO₃. Immediately above 0.7 GPa on compression, the diffraction data were not fully consistent with a VF₃-type structure as previously proposed for NbO₂F. On decompression, the data between 8 and 4 GPa could be satisfactorily attributed to a single R-3c phase with a VF₃-type structure and an average bulk modulus of 60(2) GPa.     

Elastic moduli of η‐Ta2N3, a tough self‐healing material,via laser ultrasonics

The elastic moduli of the dense polycrystalline oxygen‐bearing η‐Ta₂N₃, a novel hard and tough high‐pressure (HP) material, were measured using the laser ultrasonic technique. The bulk modulus was determined to be B₀ = 281(15) GPa which is only ～11% below that from HP compression measurements. Our value of the shear modulus G₀ = 123(2) GPa is below those ones predicted theoretically for model structures. The discrepancies in G₀ could be due to a substitution of an‐ ions and the formation of cation vacancies in η‐Ta₂N₃. Self‐healing behaviour of η‐Ta₂N₃ by mechanical polishing was observed and confirmed by two independent experimental methods. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Equal compressibility structural phase transition of molybdenum at high pressure

We have studied the high-pressure compression behavior of molybdenum up to 60 GPa by synchrotron radial x-ray diffraction (RXRD) in a diamond anvil cell (DAC). It is found that all diffraction peaks of molybdenum undergo a split at around 27 GPa, and we believe that a phase transition from a body-centered cubic structure to a rhombohedral structure at room pressure has occurred. The slope of pressure-volume curve shows continuity before and after this phase transition, when fitting the pressure-volume curves of the body-centered cubic structure at low pressure and the rhombohedral structure at high pressure. A bulk modulus of 261.3 (2.7) GPa and a first-order derivative of the bulk modulus of 4.15 (0.14) are obtained by using the nonhydrostatic compression data at the angle ψ = 54.7° between the diffracting plane normal and stress axis.     

Single-crystal elasticity of the rhodochrosite at high pressure by Brillouin scattering spectroscopy

ABSTRACT

The sound velocity properties of single-crystal rhodochrosite (MnCO₃) were determined up to 9.7?GPa at ambient temperature by Brillouin scattering spectroscopy. Six elastic constants were calculated by a genetic algorithm method using the Christoffel's equations at each pressure. The elastic constants increased linearly as a function of pressure and its pressure derivatives ?Cij/?P for C₁₁, C₃₃, C₄₄, C₁₂, C₁₃, C₁₄ were 5.86 (±0.36), 3.82 (±0.44), 2.06 (±0.39), 5.07 (±0.27), 5.34 (±0.44), 1.52 (±0.24), respectively. Based on the derived elastic constants of rhodochrosite, the aggregate adiabatic bulk and shear moduli (K_s and G) were calculated using the Voigt-Reuss-Hill averages and the linear fitting coefficients (?K_s/?P)_T and (?G/?P)_T were 5.05(±0.26) and 0.73(±0.05), respectively. The aggregate V_p of rhodochrosite increased clearly as a function of pressure and its pressure derivative ?V_p/?P was 7.99(±0.53)?×?10^?2?km/(s?GPa), while the aggregate V_s increased slowly and ?V_s/?P was only 1.19(±0.12)?×?10^?2?km/(s?GPa). The anisotropy factor for As of rhodochrosite increased from ～40% at 0.8?GPa to ～48% at 9.7?GPa, while A_p decreased from ～19% to ～16% at the corresponding pressure.     

Synthesis of NaxMoO3 crystals through high pressure solid-state reaction

We report growth of high-purity single crystals of the sodium molybdenum bronzes Na_xMoO₃ through high pressure solid-state reaction routes. Our results demonstrate that the crystallite sizes of Na_xMoO₃ can rapidly grow to ～25?μm under a moderate pressure of 4.0?GPa in just 10?min. This discovery provides a starting point for the growth of large single crystals of alkali metal molybdenum bronzes under high pressure.     

Thermal equation of state of goethite (α-FeOOH)

ABSTRACT

The pressure–volume–temperature (P–V–T) equation of state (EoS) of natural goethite (α-FeOOH) has been determined by an X-ray diffraction study using synchrotron radiation. Fitting the volume data to the third-order Birch–Murnaghan EoS yielded an isothermal bulk modulus, B₀ of 85.9(15)?GPa, and a pressure derivative of the bulk modulus, B′, of 12.6(8). The temperature derivative of the bulk modulus, (?B/?T)_P, was –0.022(9)?GPa?K^?1. The thermal expansion coefficient α₀ was determined to be 4.0(5)?×?10^?5?K^?1.     

冲击加载下铝的剪切模量

分别用Steinberg-Cochran-Guinan (SCG)模型、修正的SCG模型和有限应变理论对材料的剪切模量做了数值计算，并与一维平面应变加载下铝的实验结果进行了比较.结果表明，修正的SCG模型与实验结果较为符合.在10—80GPa的压力范围下，剪切模量随冲击压力的增加而逐渐增大，这是由于压力的影响占主要地位，发生了加工硬化.在80—125GPa的压力范围下，剪切模量随冲击压力的增大快速减小，这是因为温度的影响比较严重，发生了高温软化现象.剪切模量最终在冲击压力为125GPa处趋于零，这是由于在该压力点冲击熔化发生，剪切强度消失. 关键词： 剪切模量 Steinberg-Cochran-Guinan模型 有限应变理论 铝     

X-ray diffraction study of molybdenum diselenide to 35.9 GPa

In situ high-pressure angle dispersive synchrotron X-ray diffraction studies of molybdenum diselenide (MoSe₂) were carried out in a diamond-anvil cell to 35.9 GPa. No evidence of a phase transformation was observed in the pressure range. By fitting the pressure-volume data to the third-order Birch-Murnaghan equation of state, the bulk modulus, K_0T, was determined to be 45.7±0.3 GPa with its pressure derivative, K′_0T, being 11.6±0.1. It was found that the c-axis decreased linearly with pressure at a slope of −0.1593 when pressures were lower than 10 GPa. It showed different linear decrease with the slope of a −0.0236 at pressures higher than 10 GPa.     

First-principles study of elastic and electronic properties of layered ternary nitride SrZrN2 under pressure

The structural, elastic, and electronic properties of SrZrN₂ under pressure up to 100?GPa have been carried out with first-principles calculations based on density functional theory. The calculated lattice parameters at 0?GPa and 0?K by using the GGA-PW91-ultrasoft method are in good agreement with the available experimental data and other previous theoretical calculations. The pressure dependence of the elastic constants and the elastic-dependent properties of SrZrN₂, such as bulk modulus B, shear modulus G, Young's modulus E, Debye temperature Θ, shear and longitudinal wave velocity V_S and V_L, are also successfully obtained. It is found that all elastic constants increase monotonically with pressure. When the pressure increases up to 140?GPa, the obtained elastic constants do not satisfy the mechanical stability criteria and a phase transition might has occurred. Moreover, the anisotropy of the directional-dependent Young's modulus and the linear compressibility under different pressures are analysed for the first time. Finally, the pressure dependence of the total and partial densities of states and the bonding property of SrZrN₂ are also investigated.     

X-ray diffraction and Raman spectra of merrillite at high pressures

ABSTRACT

The compressibility and effect of pressure on the vibrations of merrillite, Ca₉NaMg(PO₄)₇, were studied by using diamond anvil cell at room temperature combined with in-situ synchrotron X-ray diffraction and Raman spectroscopy up to about 18 and 15?GPa, respectively. The pressure-volume data was fitted by a third-order Birch–Murnaghan equation of state to determine the isothermal bulk modulus as K₀ ?=?87.2(32) GPa with pressure derivative K₀′?=?3.2(4). If K₀′?=?4, the isothermal bulk modulus was obtained as 81.6(10) GPa. The axial compressibility was estimated and an axial elastic anisotropy exists since a-axis is less compressible than the c-axis. The Raman frequencies of all observed modes for merrillite continuously increase with pressure, and the pressure dependences of stretching modes (v ₃ and v ₁) are larger than those of the bending modes (v ₄ and v ₂) and external modes. The isothermal mode Grüneisen parameters and intrinsic anharmonicity of merrillite were also calculated.     

High pressure X-ray diffraction study of Fe2B

We report the results of a synchrotron based X-ray diffraction study of bct-Fe₂B under quasi-hydrostatic conditions from 0 to 50 GPa. Over this pressure range, no phase change or disproportionation has been observed. A weighted fit of the data to the Birch-Murnaghan equation of state yields a value of the bulk modulus, K, of 164±14 GPa and the first pressure derivative of the bulk modulus, K′, of 4.4±0.5. The compression is found to be anisotropic, with the a-axis being more incompressible than the c-axis.