Variations of lattice constants and thermal expansion coefficients of indium at high pressure and high temperature

ABSTRACT

The effects of pressure and temperature on the lattice constants and thermal expansion coefficients of Indium were studied up to 18.6?GPa and 506?K based on in situ X-ray diffraction method with an externally heated diamond anvil cell. The results show that the measured axial ratio (c/a) decreases with increasing temperature and its temperature dependence decreases with increasing pressure. The thermal expansion coefficient of the a-axis decreases with increasing pressure up to 7?GPa and remains almost constant above 7?GPa, whereas that of the c-axis increases monotonously with pressure and changes from negative to positive at around 7?GPa. The observed behavior suggests that temperature reduces the tetragonal distortion on the lattice, and its effect is dominant below 7?GPa; in contrast, pressure enhances lattice distortion, and tends to have a stronger effect above 7?GPa.     

Investigating the thermal conductivity of materials by analyzing the temperature distribution in diamond anvils cell under high pressure

Investigating the thermal transport properties of materials is of great importance in the field of earth science and for the development of materials under extremely high temperatures and pressures. However, it is an enormous challenge to characterize the thermal and physical properties of materials using the diamond anvil cell (DAC) platform. In the present study, a steady-state method is used with a DAC and a combination of thermocouple temperature measurement and numerical analysis is performed to calculate the thermal conductivity of the material. To this end, temperature distributions in the DAC under high pressure are analyzed. We propose a three-dimensional radiative-conductive coupled heat transfer model to simulate the temperature field in the main components of the DAC and calculate in situ thermal conductivity under high-temperature and high-pressure conditions. The proposed model is based on the finite volume method. The obtained results show that heat radiation has a great impact on the temperature field of the DAC, so that ignoring the radiation effect leads to large errors in calculating the heat transport properties of materials. Furthermore, the feasibility of studying the thermal conductivity of different materials is discussed through a numerical model combined with locally measured temperature in the DAC. This article is expected to become a reference for accurate measurement of in situ thermal conductivity in DACs at high-temperature and high-pressure conditions.     

The dehydration kinetics of gypsum at high pressure and high temperature

An in situ dehydration kinetics study of gypsum under water-saturated condition was performed in the temperature and pressure ranges of 383–423?K and 343–1085?MPa by using a hydrothermal diamond anvil cell and Raman spectroscopy. Kinetic analysis shows that the dehydration rate k increases with pressure, suggesting a negative pressure dependence on dehydration rate. The elevation of temperature can contribute to the dehydration. The n values increase with pressure, indicating that the nucleation process becomes slower relative to the growth process. According to the n values of ～1.0, the dehydration of gypsum is dominated by an instantaneous nucleation and diffusion-controlled growth mechanism. The obtained average activation volume ?V is equal to 5.69?cm³/mol and the calculated activation energy E_a and the pre-exponential factor A are 66.9?kJ/mol and 4.66?×?10⁵?s^?1. The activation energy may be dependent upon grain size, shape, temperature and pressure, and surrounding water.     

Raman study of datolite CaBSiO4(OH) at simultaneously high pressure and high temperature

Using an in situ method of Raman spectroscopy and resistance‐heated diamond anvil cell, the system datolite CaBSiO₄(OH) – water has been investigated at simultaneously high pressure and temperature (up to Р ~5 GPa and Т ~250 °С). Two polymorphic transitions have been observed: (1) pressure‐induced phase transition or the feature in pressure dependence of Raman band wavenumbers at P = 2 GPа and constant T = 22 °С and (2) heating‐induced phase transition at T ~90 °С and P ~5 GPа. The number of Raman bands is retained at the first transition but changed at the second transition. The first transition is mainly distinguished by the changes in the slopes of pressure dependence of Raman peaks at 2 GPa. The second transition is characterized by several strong changes: the wavenumber jumps of major bands, the merging of strong doublets at 378 and 391 cm⁻¹ (values for ambient conditions), the splitting of the intermediate‐intensity band at 292 cm⁻¹, and the transformation of some low‐wavenumber bands at 160–190 cm⁻¹. No spectral and visual signs of overhydration and amorphization have been observed. No noticeable dissolution of datolite in the water medium occurred at 5 GPa and 250 °С after 3 h, which corresponds to typical conditions of the ‘cold’ zones of slab subduction. Copyright © 2014 John Wiley & Sons, Ltd.     

Synthesis of Ge-Sn at high pressure and high temperature in a laser-heated diamond anvil cell

Ge–Sn compound is predicted to be a direct band gap semiconductor with a tunable band gap. However, the bulk synthesis of this material by conventional methods at ambient pressure is unsuccessful due to the poor solubility of Sn in Ge. We report the successful synthesis of Ge–Sn in a laser-heated diamond anvil cell (LHDAC) at ~7.6 GPa &; ~2000 K. In situ Raman spectroscopy of the sample showed, apart from the characteristic Raman modes of Ge TO (Г) and β-Sn TO (Г), two additional Raman modes at ~225 cm^?1 (named Ge–Sn₁) and ~133 cm^?1 (named Ge–Sn₂). When the sample was quenched, the Ge–Sn₁ mode remained stable at ~215 cm^?1, whereas the Ge–Sn₂ mode had diminished in intensity. Comparing the Ge–Sn Raman mode at ~225 cm^?1 with the one observed in thin film studies, we interpret that the observed phonon mode may be formed due to Sn-rich Ge–Sn system. The additional Raman mode seen at ~133 cm^?1 suggested the formation of low symmetry phase under high P–T conditions. The results are compared with Ge–Si binary system.     

Effect of deformation of diamond anvil and sample in diamond anvil cell on the thermal conductivity measurement

Studies show that the sample thickness is an important parameter in investigating the thermal transport properties of materials under high-temperature and high-pressure (HTHP) in the diamond anvil cell (DAC) device. However, it is an enormous challenge to measure the sample thickness accurately in the DAC under severe working conditions. In conventional methods, the influence of diamond anvil deformation on the measuring accuracy is ignored. For a high-temperature anvil, the mechanical state of the diamond anvil becomes complex and is different from that under the static condition. At high temperature, the deformation of anvil and sample would be aggravated. In the present study, the finite volume method is applied to simulate the heat transfer mechanism of stable heating DAC through coupling three radiative-conductive heat transfer mechanisms in a high-pressure environment. When the temperature field of the main components is known in DAC, the thermal stress field can be analyzed numerically by the finite element method. The obtained results show that the deformation of anvil will lead to the obvious radial gradient distribution of the sample thickness. If the top and bottom surfaces of the sample are approximated to be flat, it will be fatal to the study of the heat transport properties of the material. Therefore, we study the temperature distribution and thermal conductivity of the sample in the DAC by thermal-solid coupling method under high pressure and stable heating condition.     

原位高压微米氧化锌电学性质的研究

利用集成有金属薄膜电极的金刚石对顶砧,对微米氧化锌样品进行了原位高压电导率测量.结果表明,在919 GPa时样品电导率达到最小值,在919—1122 GPa时样品电导率急剧增大,说明此时样品从纤锌矿结构向岩盐矿结构转变直至完全相变,1122　GPa为相变点.通过测量不同条件下高温退火处理的样品电导率,明显看到氧空位对电导率的影响. 关键词： 高压 微米氧化锌 电导率 金刚石对顶砧     

Laser heating in diamond anvil cells: developments in pulsed and continuous techniques

Developments in continuous and pulsed laser‐heating techniques, and finite‐element calculations for diamond anvil cell experiments are reported. The methods involve the use of time‐resolved (5 ns gated) incandescent light temperature measurements to determine the time dependence of heat fluxes, while near‐IR incandescent light temperature measurements allow temperature measurements to as low as 500 K. Further optimization of timing in pulsed laser heating together with sample engineering will provide additional improvements in data collection in very high P–T experiments.     

金刚石对顶砧中触点位置误差对样品电阻率测量精度的影响

利用有限元分析方法,研究了金刚石对顶砧中电极与样品接触点位置变化对范德堡法测量样品电阻率精度的影响.结果表明:当电极中心与样品边缘的间距b≤d/9(d为样品直径)时能得到精确的电阻率测量结果;当电极位置远离样品边缘而逐渐接近样品中心时,其位置变化对电阻率测量精度的影响迅速增大;相同的电极位置变化对具有较大电阻率的半导体样品电阻率测量精度的影响更明显. 关键词： 电阻率 有限元方法 金刚石对顶砧     

Electrical conductivity anisotropy in alkali feldspar at high temperature and pressure

The electrical conductivity of alkali feldspar along different orientations was determined at 1.0 GPa and at temperatures of 823–1286 K in a cubic anvil apparatus using alternating current impedance spectroscopy. Impedance arcs representing crystal conductivity occur in the frequency range of ～10³–10⁶ Hz. The electrical conductivity of alkali feldspar increases with increasing temperature. The highest electrical conductivities in alkali feldspars were measured along the a-axis, with somewhat lower conductivities along the b-axis, and the lowest conductivities along the c-axis, suggesting minor anisotropy. The activation enthalpies ranged from 100 to 110 kJ/mol. The anisotropic results were combined to yield an isotropic model with an activation enthalpy of 102 kJ/mol. By comparing these results with previous results, we suggest that the dominating charge carriers for alkali feldspars are alkali ions. The minor anisotropy in conductivity for alkali feldspar may not account for the anisotropy of the crust.     

Magnetic transition of ferromagnetic material at high pressure using a novel system

A system for the investigation of the magnetic properties of materials under high pressure is fabricated based on diamond anvil cell （DAC） technology. The system is designed with an improved coil arranged around the diamond of a non-magnetic DAC. Using this system, the magnetic transition of ferromagnetic （Fe） sample under increasing pressure can be observed. We successfully obtain the evolution of magnetic properties as a function of applied pressure reaching 26.9 GPa in the Fe sample. A magnetic transition is observed at approximately 13 GPa, which is consistent with the theoretical prediction.     

Ruby fluorescence lifetime measurements for temperature determinations at high (p,T)

The lifetime of the ruby R₁ fluorescence line was measured as a function of pressure (up to about 20 GPa) and temperature (550 K) in an externally heated diamond anvil cell (DAC). At constant temperatures, the lifetime is increasing linearly with increasing pressure. The slope of the pressure dependence is constant up to a temperature of 450 K and it is decreasing at higher temperatures. At constant pressure, the lifetime is exponentially decreasing with increasing temperature. The (p, T)-dependence can be parametrized by the combination of a linear and an exponential function. This allows an accurate p, T-determination by the combination of fluorescence spectroscopy using Sm²⁺-doped strontium tetraborate and lifetime measurements of ruby, as the energy of the Sm²⁺ fluorescence is nearly temperature-independent.     

电驱动金刚石对顶砧低温连续加压装置

采用电驱动压电陶瓷取代传统机械螺丝给金刚石对顶砧施加压力,设计制备了低温下可连续增加流体静压的金刚石对顶砧压力装置,实现了低温(19±1)K连续加压达到4.41 GPa.该装置具有电驱动方便灵活、调谐精度高的低温连续加压功能.利用该装置实现了InAs单量子点发光与微腔腔模的共振耦合调谐过程.该装置将在原位压力精确调谐及测量样品信号跟踪等实验得到应用.     

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.     

Thermal conductivity and thermal diffusivity of tantalum in the temperature range from 293 to 1800 K

Thermal diffusivity of polycrystalline tantalum at the temperature range from 293 to 1800 K has been measured by the laser flash method with the error of 2–4 %. Thermal conductivity has been calculated with the use of reference data on density and heat capacity. Approximating equations and tables of reference data for the temperature dependence of heat transfer coefficients have been obtained; comparison with the published data has been carried out. The work was financially supported by the Russian Foundation for Basic Research (Grant No. 07-08-00071).     

Diamond cleavage: importance to high pressure research

The extraordinary properties of diamond make it the number-one choice for anvils in high pressure experiments involving anvil cells. In much of the literature on the properties of diamond the only cleavage mentioned is {111}. However, experience has shown that diamond anvils made with their [001] axis oriented in line with the principal stress axis of the anvil or at a small angle to it often failed with flat faces having {110} orientations; a cleavage plane is reported in some publications. Analysis of the anisotropy of strength and Poisson ratio in diamond has shown that such orientations do, indeed, favor initial failure on {110} cleavage planes. This analysis, in conjunction with stereographic projections of the {111} and {110} cleavage planes, suggests that a 27° tilt of the [001] axis with respect to the linear stress axis by rotation around the [100] or [010] axis should provide significantly greater resistance to failure by cleaving.     

基于拉曼频移的白宝石压腔无压标系统高温高压实验标定

在高压实验科学中, 各类宝石压腔是最为常见的高压设备之一, 其样品腔中压力的精确标定是实验的关键. 目前, 人们主要通过加入红宝石等压标物质来进行定压, 但压标物质的加入会增加实验的装样难度, 改变样品腔中的物理化学环境, 甚至直接与实验样品发生反应, 从而对实验结果产生影响. 在0–6.3 GPa和300–573 K下, 利用共聚焦拉曼显微镜, 根据白宝石压砧砧面的ν₁₂ 拉曼频移与温度和压力的变化关系, 建立了一套适用于高温高压水热体系的无压标白宝石压腔系统. 实验结果表明: 白宝石砧面的ν₁₂ 峰随着压力的升高发生线性蓝移, 而随着温度升高则发生线性红移, 且温度和压力对拉曼频移的影响存在耦合效应. 利用本实验结果, 可在高温高压下根据白宝石砧面的拉曼频移计算出样品腔的压力P=(Δλ-0.01913×ΔT)/(1.9158-0.00105×ΔT), 在物理学、材料学和地球科学等领域具有重要应用.     

Gold under high pressure

Abstract

First principle predictions for the equation of state of gold using solid and liquid state theories are compared up to combined pressures and temperatures of 600 GPa and 17 000 K with static diamond anvil cell compression, ultrasonic measurements and shock Hugoniot data which include a recent laser driven shock Hugoniot points at 600 GPa. Excellent agreement between theoretical and experimental data is observed. The theoretically estimated 300 K isotherm agrees to within 2 GPa with the isotherm that has been measured to 70 GPa using the diamond anvil cell. The structural energy estimates show that the normal f.c.c. phase remains stable under pressure. The estimate of the shock Hugoniot temperature of gold at 600 GPa based on a liquid state model is consistent with the measurements of laser induced shock luminescence, which in fact provides an experimental determination of the temperature of gold above its Hugoniot melting point. The powerful means provided by theory in the prediction of material properties of gold at ultra high pressures and temperatures is significant because gold is an efficient converter of laser energy into soft X-rays and is a potential candidate as a standard for high pressure, high temperature work.