高温高压条件下液态氧的声速及弹性系数研究

 采用布里渊散射技术和金刚石对顶砧高压装置,对液态氧进行了高温高压实验研究。入射光采用波长为532 nm的单纵模二极管泵浦固体激光源,布里渊光谱由3+3通道法布里-珀罗干涉仪收集。采用电阻丝外加热方法产生高温,用四柱型金刚石对顶砧压机产生高压。分别在背向散射和60°对称散射配置下,研究了温度在298、367和423 K下液态氧的声速及弹性系数随压力的变化关系,实验的最高温度和压力为423 K、8.9 GPa。结果表明,通过实验测量所得到的声速值与理论计算值较接近,并发现在2.3~4.9 GPa的压力范围内,温度由298 K升高到367 K时,弹性系数并没有明显的减小,认为在这个压力范围内,当温度升高时,液氧的体积不膨胀,即基本保持不变。     

On-line laser heating setup for ED-XAS at ID24: preliminary optical design and test results

Double-sided laser heating (LH) combined with synchrotron X-ray radiation for in situ studies in the diamond anvil cell (DAC) has been the most productive and widely used high-temperature–high pressure technique in the past two decades. In the framework of the UPBL11 project (upgrade of ID24 beamline of European Synchrotron Radiation Facility), we developed a new on-line LH system for DACs. The preliminary optical scheme of the system is presented and discussed. Varying the settings, we are able to shape and to size the beam on the surface of the sample in the DAC. First pilot applications to the Fe case are shown.     

基于集成技术的金刚石对顶砧原位电学量测量

 金刚石对顶砧是应用最多的高压装置,能够产生超过400 GPa的超高压力,借助激光加温,还可以加载6 000 K的高温。近20年来,基于金刚石对顶砧的微小测量电路集成技术的突破,带动了高压原位电学量测量技术的发展,使常压下能够测量的电学量大部分都能在金刚石对顶砧中的高压环境下实现。全面回顾了基于集成技术的金刚石对顶砧高压原位电学量测量技术的发展历程,介绍了最新的技术进展。     

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.     

一套高温高压原位拉曼散射、布里渊散射测量系统

本文描述了一套利用激光加热技术、金刚石对顶砧高压技术,集成共聚焦拉曼光谱测量、六通道布里渊散射光谱测量、以及黑体辐射光谱测温,成功搭建起来的高温高压原位拉曼散射、布里渊散射的光学测量系统。利用该系统,并结合薄膜沉积金属、光刻技术改进了金刚石对顶砧中样品的装填方法,解决了样品透明不易加热的问题。已利用该系统得到液态氩在0.85 GPa常温状态下和14.58 GPa熔融状态下的体声速分别为1.85 Km/s和5.19 Km/s。     

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.     

Experimental system for X-ray magnetic diffraction under extreme conditions

An experimental system for X-ray magnetic diffraction (XMD) under extreme conditions was constructed on the beamline BL39XU at SPring-8. This system aims at studying magnetic properties of ferromagnets through the measurements of magnetic form factors under the conditions of low temperature (5 K), high magnetic field (6 T) and high pressure (10 GPa). This system consists of a superconducting magnet (SCM), a diamond anvil cell (DAC), a two-axis manipulator for the DAC, a five-axis goniometer for the SCM, and an X-ray polarizer with a phase plate. Details of this system are presented. Experimental results on uranium telluride are shown as a performance test with this instrumentation.     

金刚石压腔高温高压实验的压力标定方法及其现状

 介绍和评论了金刚石压腔中进行高温高压实验时的压力标定方法及其应用条件。其中红宝石和石英压标具有较高的准确度和精度,但前者不适合于高温和含饱和水条件下的标定,且在较低压力下误差较大,后者可用于高温且含水体系的压力标定,但仅适于低于2.0 GPa时的压力标定。矿物状态方程是较可靠的方法,但不方便且受条件限制。采用水的状态方程进行压力标定,可以解决压腔中不允许有压标矿物的问题,但在实验过程中要求压腔的体积保持恒定。因此,在采用金刚石压腔进行高温高压实验时,应根据研究需要决定合适的压力标定方法,而且寻找新的压力标定方法仍是金刚石压腔高压实验的基础工作。     

Amorphous boron composite gaskets for in situ high-pressure and high-temperature studies

The diamond anvil cell (DAC) is a fundamental device used to explore the properties of materials under extreme pressure and temperature (P/T) conditions. In the past years, simultaneous high P/T DAC experiments using the resistively heated DAC (RH-DAC) techniques have been developed for studying materials properties in a wide P/T range. However, the mechanical instability of metallic gaskets used for sample confinement at high P/T conditions remains a limiting factor for exploiting the accessible P/T range of the RH-DAC. In this study, we present a new gasket configuration that overcomes these limitations. It is based on an amorphous boron–epoxy mixture inserted in a rhenium gasket. We show how these gasket inserts stabilize the sample chamber over a wide P/T range, allowing monitoring sample properties using X-ray diffraction and absorption spectroscopy up to 50?GPa and 1620?K.     

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.     

Resistively heated,high pressure,membrane and screw driven diamond anvil cell

ABSTRACT

High temperature is of paramount importance in high pressure science. One of the leading tools in this respect is the resistively heated diamond anvil cell (DAC), where the heat is provided by small heaters, positioned close to the diamond/gasket/sample region (internally heated DAC, IHDAC) or by wrapping the DAC body into bigger heaters (externally heated DAC, EHDAC). Although IHDACs can reach sample temperatures higher than 1000?K, they are difficult to handle and the heater/diamond/gasket/sample region may be affected by strong thermal gradients potentially hindering accurate temperature measurements. Here we present a novel EHDAC, which overcomes these issues by uniquely joining: (i) high mechanical precision for multi-Mbar, (ii) high temperature alloys for operating to 1000?K, (iii) membrane or screw driven, easily switchable between each other, (iv) operation into a vacuum chamber, (v) uniform temperature, (vi) facile handling, and (vii) possibility to add internal heaters for achieving even higher temperatures.     

Neutron diffraction experiments in diamond and sapphire anvil cells

Diamond anvil cells (DAC) provide the highest static pressures ≥1?Mbar. Because of the low intensity of neutron sources, for a long time it was thought impossible to use DAC or other anvil cells in neutron experiments. We describe pressure cells with diamond and sapphire anvils and neutron instrumentation allowing neutron diffraction experiments to be carried out under pressures as high as 50?GPa, temperatures down to 0.1?K, and applied magnetic fields up to 7.5?T.     

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.     

压电驱动金刚石对顶砧加压装置的研制和应用

金刚石对顶砧加压装置广泛用于物理、化学、材料等许多科学领域。自Bridgman发明金属对顶砧及随后发展金刚石对顶砧以来,对顶砧装置设计和加压技术得到不断发展。文章介绍采用压电驱动金刚石对顶砧来产生高压,实现低温20 K下原位连续加压,连续加压范围约2—4 GPa。该加压装置具有体积小、操作方便,可装在小型低温恒温器中使用等优点。     

环庚烷的高压拉曼光谱研究

 利用金刚石对顶砧（DAC）装置产生高压,在室温下对环庚烷进行了高压原位拉曼光谱研究。实验的最高压力是17.00 GPa。研究结果表明,在实验的压力范围内,室温常压下为液态的环庚烷在0.53 GPa发生了液-固相变;在3.45~5.58 GPa压力区间,环庚烷的拉曼频移随压力变化的曲线和拉曼峰的半高宽随压力的变化曲线都出现了拐点,由此判断,环庚烷可能发生了固-固相变。     

High Pressure and High Temperature Studies on Manganese Oxides

High pressure and high temperature quench experiments on f -MnO 2 , Mn 2 O 3 and sol gel derived manganese oxides have been carried out to identify any new phases to which the materials may transform under high pressure and high temperature conditions. Results of ESR, DTA and TGA investigations on sol gel derived manganese oxide have shown it to be hausmannite Mn 3 O 4 , instead of n -Mn 2 O 3 as reported earlier in the literature. The sol gel derived manganese oxide transforms to n -Mn 2 O 3 when heated above 700°C. Sol gel derived Mn 3 O 4 , when quenched from 5 GPa and temperature range 800-1200°C, gives a mixture of Mn 3 O 4 (hausmannite) and a phase having CaMn 2 O 4 (marokite)-type structure. f -MnO 2 undergoes partial amorphization when pressure-quenched from 8 GPa at room temperature. The high pressure and high temperature quench experiments up to 5 GPa and 700°C showed that the decomposition temperature of f -MnO 2 increases with pressure. The new phase reported by Liu (1976) from diamond-anvil cell (DAC) experiments on pyrolusite MnO 2 is identified to be a low-density polymorph f -MnO 2 . This unusual result of formation of low-density f -MnO 2 , having an open structure at high pressure and high temperature, is probably due to quenching of a non-equilibrium phase in Liu's (1976) laser-heated DAC experiment.     

光散射谱学在地球内部物质弹性波速测量中的应用与展望

高温高压下地球内部物质弹性波速的实验测量数据,可直接与地震波观测结果相结合,对地球内部的组成、状态和物质运移方式等进行反演,是了解地球深部信息的重要手段。在金刚石压砧(diamond anvil cell, DAC) 中利用布里渊散射对矿物波速进行原位测量,是人们研究地球各圈层弹性性质的重要方法。随着DAC实验技术发展,一方面,可以获得模拟地球各圈层的极高温压条件;另一方面,DAC的光学特性使得各种光学分析和测试方法得到了广泛的应用。要获得高温高压下的弹性波速,首先需要对样品腔中的实验压力和加热温度进行精确的标定和测量;其次需对散射信号进行处理,通过布里渊散射频移,求出样品中的波速;最后结合X射线技术获得的晶格常数,可由固体弹性理论解出矿物的各弹性参数。重点介绍了布里渊散射和拉曼散射等光谱学方法在弹性波速实验研究中的应用,阐述了它们在波速测量、压力和温度标定等方面的基本原理和研究进展。分析了两种光谱学定压方法(荧光光谱压标和拉曼光谱压标) 的定压方式和适用范围,以及两种主要的光谱学温标(黑体辐射温标和拉曼光谱温标) 在温度测量中的应用。最后,回顾了基于光谱学测量建立起来的布里渊散射系统对下地幔主要矿物(钙钛矿、方镁铁矿、斯石英等) 弹性波速测量取得的新成果,深入讨论了它们的地球物理意义,并对其未来的发展进行了展望。     

Review on Application of Optical Scattering Spectroscopy for Elastic Wave Velocity Study on Materials in Earth's InteriorSCIEI北大核心CSCD

In-situ experimental results on the elastic wave velocity of Earth materials at high pressure and high temperature in combination with data from seismic observation can help to inverse the chemical composition, state and migration of materials in Earth's interior, providing an important approach to explore information of deep earth. Applying the Brillouin scattering into the Diamond Anvil Cell (DAC) to obtain the in situ elastic wave velocities of minerals, is the important approach to investigate elastic properties of Earth's Interior. With the development of DAC technology, on the one hand, the high temperature and high pressure experimental environment to simulate different layers of the earth can be achieved; on the other hand, the optical properties of DAC made many kinds of optical analysis and test methods have been widely applied in this research field. In order to gain the elastic wave velocity under high temperature and high pressure, the accurate experimental pressure and heating temperature of the sample in the cavity should be measured and calibrated first, then the scattering signal needs to dealt with, using the Brillouin frequency shift to calculate the velocity in the sample. Combined with the lattice constants obtained from X ray technique, by a solid elastic theory, all the elastic parameters of minerals can be solved. In this paper, firstly, application of methods based on optical spectrum such as Brillouin and Raman scattering in elasticity study on materials in Earth's interior, and the basic principle and research progress of them in the velocity measurement, pressure and temperature calibration are described in detail. Secondly, principle and scope of application of two common methods of spectral pressure calibration (fluorescence and Raman spectral pressure standard) are analyzed, in addition with introduce of the application of two conventional means of temperature calibration (blackbody radiation and Raman temperature scale) in temperature determination. Lastly, geophysical applications of mineral elasticity are discussed on the basis of the recent research results derive from Brillouin scattering system of wave velocities for major minerals in Earth's lower mantle (perovskite, ferropericlase, etc.), and the future research work is inspected.     

温度和压力对Au反射特性影响及动高压下的测温应用分析

基于金属电子气模型,进行了温度、压力对Au反射率变化影响的研究与分析。利用DAC装置开展了压力对Au反射率变化测量实验,以及激光加热的动态温升条件下温度对Au反射率变化测量实验,获得了探测光束波长为488 nm条件下,温度(室温至350 ℃)和压力(11 GPa范围内)对Au反射特性影响的实验结果。结果表明:在11 GPa压力范围内,与温度因素相比,压力对Au的反射率变化影响可忽略;Au对488 nm波长激光的反射率变化趋势为单调递增,变化幅值达约10%,且具有反射率与温度的一一对应特性。通过动高压加载下材料温度瞬态测量要求分析,认为基于Au在488 nm波长下的反射变化特性,可建立一种适用于动高压加载下低温段(低于1000 K)的瞬态测温方法,用于解决材料动高压领域的瞬态测温技术难点。     

温度和压力对Au反射特性影响及动高压下的测温应用分析

基于金属电子气模型,进行了温度、压力对Au反射率变化影响的研究与分析。利用DAC装置开展了压力对Au反射率变化测量实验,以及激光加热的动态温升条件下温度对Au反射率变化测量实验,获得了探测光束波长为488 nm条件下,温度(室温至350 ℃)和压力(11 GPa范围内)对Au反射特性影响的实验结果。结果表明：在11 GPa压力范围内,与温度因素相比,压力对Au的反射率变化影响可忽略;Au对488 nm波长激光的反射率变化趋势为单调递增,变化幅值达约10%,且具有反射率与温度的一一对应特性。通过动高压加载下材料温度瞬态测量要求分析,认为基于Au在488 nm波长下的反射变化特性,可建立一种适用于动高压加载下低温段(低于1000 K)的瞬态测温方法,用于解决材料动高压领域的瞬态测温技术难点。