How to detect melting in laser heating diamond anvil cell

Research on the melting phenomenon is the most challenging work in the high pressure/temperature field. Until now,large discrepancies still exist in the melting curve of iron, the most interesting and extensively studied element in geoscience research. Here we present a summary about techniques detecting melting in the laser heating diamond anvil cell.

Thermal conductivity of dense hcp iron:Direct measurements using laser heated diamond anvil cell

Thermal conductivity(k)of iron is measured up to about 134 GPa.The measurements are carried out using the single sided laser heated diamond anvil cell,where the power absorbed by a Fe metal foil at hotspot is calculated using a novel thermodynamical method.Thermal conductivity of fee(γ)-Fe increases up to a pressure of about46 GPa.We find thermal conductivity values in the range of 70-80 Wm-1K-1(with an uncertainty of 40%),almost constant with pressure,in the hcp(e)phase of Fe.We attribute the pressure independent k above 46 GPa to the strong electronic correlation effects driven by the electronic topological transition(ETT).We predict a value of thermal conductivity ofε-Fe of about 40±16 Wm-1K-1 at the outer core of Earth.

Laser-Heated Diamond-Anvil Cell (LHDAC) in Materials Science Research

Laser-heated diamond-anvil cell (LHDAC) is emerging as the most suitable, economical and versatile tool for the measurement of a large spectrum of physical properties of materials under extreme pressure and temperature conditions. In this review, the recent developments in the instrumentation, pressure and temperature measurement techniques, results of experimental investigations from the literature were discussed. Also, the future scope of the technique in various avenues of science was explored.

Application of Hydrothermal Diamond Anvil Cell to Homogenization Experiments of Silicate Melt Inclusions

The homogenization of silicate melt inclusions （SMIs）,small droplets of silicate melt trapped in magmatic minerals,is an important component of petrogenetic and magmatic research.Conventional homogenization experiments on SMIs use microscope-mounted heating stages capable of producing high temperatures at 1 atm and cold-seal high-pressure vessels.Heating stages are generally used for SMIs with low internal pressures and allow in situ observations of the homogenization processes.In contrast,cold-seal high-pressure vessels are generally used to heat SMIs that have high internal pressures,although the homogenized SMIs can only be observed after quenching in this approach.Here we outline an alternative approach that uses a hydrothermal diamond anvil cell （HDAC） apparatus to homogenize SMIs.This is the only current method wherein phase changes in high-internal-pressure SMIs can be observed in situ during homogenization experiments,which represents an advantage over other conventional methods.Using an HDAC apparatus prevents high-internal-pressure SMIs from decrepitating during heating by elevating their external pressure,in addition to allowing in situ observations of SMIs.The type-V HDAC that is currently being used has a shorter distance between the sample chamber and the observation window than earlier types,potentially enabling continuous observation of the processes involved in heating and SMI homogenization through an objective lens with a long working distance.Homogenization experiments using HDAC require that a number of steps,including HDAC preparation,sample preparation,sample loading,preheating,and formal heating,be carefully followed.Homogenization experiments on SMIs within granite samples from the Jiajika pegmatite deposit （Sichuan,China） are best performed using an HDAC-based approach,because the elevated proper external pressure of these SMIs,combined with a short heating duration,helps to suppress material leakage and any reactions within the SMIs,in addition to allowing in situ observations during homogenization experiments.Furthermore,using the HDAC approach has other benefits：heating rates can be precisely controlled,wafer oxidization can be prevented,and samples can be subjected to in situ microbeam analysis.In summary,homogenization using HDAC provides more reliable results than those obtained using conventional heating equipment.Future developments will include improvements to the quenching method and temperature controls for the HDAC apparatus,thereby improving the utility of this approach for SMI homogenization experiments.

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction（XRD） in diamond anvil cells（DACs） using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF（Beijing Synchrotron Radiation Facility） and some results are also presented.

Development of High-Pressure Multigrain X-Ray Diffraction for Exploring the Earth’s Interior

The lower mantle makes up more than a half of our planet’s volume. Mineralogical and petrological experiments on realistic bulk compositions under high pressure–temperature (P–T) conditions are essential for understanding deep mantle processes. Such high P–T experiments are commonly conducted in a laser-heated diamond anvil cell, producing a multiphase assemblage consisting of 100 nm to submicron crystallite grains. The structures of these lower mantle phases often cannot be preserved upon pressure quenching;thus, in situ characterization is needed. The X-ray diffraction (XRD) pattern of such a multiphase assemblage usually displays a mixture of diffraction spots and rings as a result of the coarse grain size relative to the small X-ray beam size (3–5 lm) available at the synchrotron facilities. Severe peak overlapping from multiple phases renders the powder XRD method inadequate for indexing new phases and minor phases. Consequently, structure determination of new phases in a high P–T multiphase assemblage has been extremely difficult using conventional XRD techniques. Our recent development of multigrain XRD in high-pressure research has enabled the indexation of hundreds of individual crystallite grains simultaneously through the determination of crystallographic orientations for these individual grains. Once indexation is achieved, each grain can be treated as a single crystal. The combined crystallographic information from individual grains can be used to determine the crystal structures of new phases and minor phases simultaneously in a multiphase system. With this new development, we have opened up a new area of crystallography under the high P–T conditions of the deep lower mantle. This paper explains key challenges in studying multiphase systems and demonstrates the unique capabilities of high-pressure multigrain XRD through successful examples of its applications.

Applications for Nanoscale X-ray Imaging at High Pressure

Coupling nanoscale transmission X-ray microscopy (nanoTXM) with a diamond anvil cell (DAC) has exciting potential as a powerful three-dimensional probe for non-destructive imaging at high spatial resolution of materials under extreme conditions. In this article, we discuss current developments in high-resolution X-ray imaging and its application in high-pressure nanoTXM experiments in a DAC with third-generation synchrotron X-ray sources, including technical considerations for preparing successful measurements. We then present results from a number of recent in situ high-pressure measurements investigating equations of state (EOS) in amorphous or poorly crystalline materials and in pressureinduced phase transitions and electronic changes. These results illustrate the potential this technique holds for addressing a wide range of research areas, ranging from condensed matter physics and solidstate chemistry to materials science and planetary interiors. Future directions for this exciting technique and opportunities to improve its capabilities for broader application in high-pressure science are discussed.

Structural stability and vibrational characteristics of CaB6 under high pressure

In situ Raman spectroscopy and x-ray diffraction measurements are used to explore the structural stability of CaB6 at high pressures and room temperature. The results show no evidence of structural phase transitions up to at least 40 GPa.The obtained equation of state with smooth pressure dependencies yields a zero-pressure isothermal bulk modulus B0=170(5) GPa, which agrees well with the previous measurements. The frequency shifts for A1g, Eg, and T2g vibrational modes of polycrystalline CaB6 are obtained with pressure uploading. As the pressure increases, all the vibration modes have smooth monotonic pressure dependence. The Gr¨uneisen parameter of Eg modes is the largest, indicating its largest dependence on the volume of a crystal lattice.

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 angleψ=54.7°between the diffracting plane normal and stress axis.

High-pressure synergetic measurement station(HP-SymS)

In the High-Pressure Synergetic Measurements Station （HP-SymS） of the Synergic Extreme Condition User Facility （SECUF）, we will develop ultrahigh-pressure devices based on diamond-anvil cell （DAC） techniques, with a target pressure up to 300 GPa. With the use of cryostat and magnet, we will reach 300 GPa4.2 K-9 T and conduct simultaneous measurements of the electrical-transport property and Raman/Brillouin spectrascopy. With resistance heating and laser heating, we will reach temperatures of at least 1000 and 3000 K, respectively, coupled with Raman/Brillouin spectroscopy measurements. Some designs of supporting devices, such as a femtosecond laser gasket-drilling device, electrode-deposition device, and the gas-loading device, are also introduced in this article. Finally, we conclude by providing some perspectives on the applications of the DAC in related research fields.

高压下二元富氢超导体的实验研究进展

自从1911年著名物理学家Onnes发现超导电性以来,人们不断努力提高超导转变温度,室温超导体是人类追逐的百年梦想。在近百年的研究历程中,铜基超导体、铁基超导体及麦克米兰极限MgB_(2)超导体的发现不断刷新了人们对超导领域的认知,也增强了人们进一步提高超导转变温度和挖掘高温超导机制的信心。最近,理论预测并被实验验证的新型富氢化合物显示了高温乃至室温超导电性的巨大潜力,成为室温超导体的最佳候选体系之一。值得注意的是,高压下硫氢化物和镧氢化物均具有超过200 K的超导转变温度,引领了富氢化合物的研究热潮,涌现了一些重要的理论和实验成果。本文聚焦于目前富氢化合物超导体的实验研究进展,从不同氢结构单元及氢成键特征的角度总结和归纳新型富氢化合物的晶体结构性质及超导性能。主要介绍了5种在实验上成功获得的富氢化合物超导体:间隙型、离子型、共价型、笼型及分子型。通过对比分析不同类型的富氢化合物超导体,总结出一些影响超导转变温度的普适规律,并提出目前实验上亟待解决的问题和未来主攻的实验方向。

高压下金属卤素钙钛矿的结构和性质演化研究进展

过去10年里,金属卤素钙钛矿作为一种性能优异的新型功能材料被广泛应用,其研究取得了很多重要进展。压力作为一个基本的热力学变量,可以显著地影响材料的微观结构、原子间相互作用、电子轨道和化学键,是调节材料结构和性能的一个强大工具。与此同时,压力也为研究结构与性质之间的关系提供了新路径。结合金刚石对顶砧高压装置以及原位高压表征技术,总结了金属卤素钙钛矿在高压下的结构及性质变化,包括高压驱动结构相变,有序-无序转变,非晶化,局部结构演化,带隙、光致发光、光响应、电阻等性质在压力作用下的变化,以及高压下特有的奇特性质如金属化转变,系统分析了此类材料的结构-性质关系,并对未来的新型材料设计做出了展望。

高压极端条件下的富氢高温超导体

自从在汞中发现4.2 K的超导转变温度以来,寻找室温超导体一直是凝聚态物理领域的研究热点。近年来,科学家在高压极端条件下发现了以共价型H_(3)S(T_(c)=203 K)和离子型LaH_(10)(T_(c)=250 K)、CaH_(6)(T_(c)=215 K)为代表的系列高温超导体,先后刷新了超导转变温度纪录,这些工作开启了学界在富氢化合物中寻找室温超导体的新篇章。本文重点介绍了目前高压下二元和三元富氢高温超导体的理论模拟以及实验制备和表征方面的相关研究进展,分析在富氢化合物中发现室温超导体面临的挑战和可能途径,为实现室温超导做出基础性贡献。

微秒到秒时间尺度的高压相变动力学和物性研究:回顾、进展及展望

近年来,基于金刚石对顶砧的快速加载技术(如动态金刚石对顶砧)和时间分辨探测技术的快速发展为高压科学研究开辟了新的研究方向和思路。这些技术使得科学家能够探索微秒到秒级时间尺度的高压非平衡物理过程,填补了静高压与动态冲击波实验之间的空白。本文回顾并总结了近年来在快速加载和时间分辨探测技术上的进展,详细探讨了依赖于加载速率的结构相变动力学、相变途径、亚稳相的形成、微结构、力致发光等现象。希望通过深入思考和系统归纳微秒至秒级时间尺度的高压科学问题和技术挑战,为高压科学领域的研究者提供新的启示和参考。

New measurement of melting and thermal conductivity of iron close to outer core conditions

The amount of literature on both melting and thermal conductivity of iron at Earth’s core conditions is overwhelming and the discrepancies are very large.There is a broad range of experimental techniques each of which is flawed to a certain degree,which may explain the discrepancy.In this report,we present new data using a different method for determining the phase behavior and resistivity of iron in the laser-heated diamond cell by measuring the electrical resistance of both solid and liquid iron wires.The experiment avoids some of the major flaws of previous experiments,the most important of which is the detection of the onset of melting.These measurements confirm a shallow melting curve found earlier and the resistivity data imply a trend towards low thermal conductivity in the liquid outer core.

Synthesis of Ta C and Ta_2C from tantalum and graphite in the laser-heated diamond anvil cell

The pressure dependence of the onset of the formation of Ta C and Ta2 C from the elements has been investigated by in situ X-ray diffraction and pyrometry.Ta C has been synthesized by the reaction of Ta and graphite at pressures between 8.6 and 14.3 GPa and at temperatures up to 2,300 K using a laser-heated diamond anvil cell. The products were characterized by X-ray diffraction. Ta and graphite begin to react around 1,100 K at ambient pressure conditions, and the reaction temperature increases with increasing pressure. A linear extrapolation of these data is consistent with recent observations of the formation of Ta C at 90 GPa and 3,600 K. We show that diffusion of carbon into tantalum significantly changes the lattice parameter of up to 2 % in the pressure range of up to19 GPa. In some experiments, Ta2 C was formed concomitantly. The experimentally determined bulk modulus of Ta2 C is B0;exp:= 286(5) GPa. Other tantalum carbide phases were not observed.

Li_(2)MnO_(3 )的高压状态方程和电输运研究

Li_(2)MnO_(3)在室温下金刚石对顶砧中通过同步辐射X射线衍射实验获得了其在高压下的状态方程。高压压缩实验的最高压力为28.00 Gpa。高压同步辐射衍射数据得到的体弹模量为(106.20±4.20)GPa,体弹模量的一阶导数为16.92±1.28。此外,Li_(2)MnO_(3)到21.00 GPa的高压电输运性质表明,Li_(2)MnO_(3)的电阻随压力增大而减小,且呈指数连续变化规律。

高压力学方法及研究进展

高压力学研究在材料学领域和地学领域掀起了交叉科学研究的热潮,为高难度材料制备、材料力学性能改善、地震波各向异性成因及地球内部动力学过程研究等科学问题提供了解决方案。针对高压力学领域的研究方法,介绍了金刚石对顶砧结合X射线径向衍射法、旋转型金刚石对顶砧施加剪切应变法、高压扭转型压机施加剪切应变法、D-DIA型大腔体压机形变法和冲击压缩产生塑性形变法及其研究进展,展示了压应力与剪切力的耦合作用在调控材料的结构、性能及宏观力学行为方面的独特效应,揭示了高压力学研究的价值与应用潜力。

金刚石压腔高温高压原位谱学研究的评述

金刚石压腔 (DAC)已经可以达到 5 5 0 GPa的压力和 6 0 0 0 K的温度 ,其高温高压谱学原位测量已经成为现代科学的一种重要的手段和方法。目前利用 DAC可以进行光谱学 (拉曼光谱、红外光谱、荧光光谱 )、衍射 (X射线衍射和 XAFS)、布里渊散射、核磁共振 (NMR)以及穆斯堡尔谱的高温高压原位研究。设计用于各种不同需要的便宜的压腔、合适的谱学测量方法以及压力内标物质是进一步拓宽 DAC应用的发展方向。

流体包裹体压力计研究之一:高温高压下Na_2SO_4溶液的拉曼光谱

用金刚石压腔研究了Na2S04溶液在温度30—400℃、压力90—2400MPa条件下的拉曼光谱特征。结果表明：温度相同时，SO4^2-的对称伸缩振动随压力增大向高频方向偏移；而在压力基本相同时，随温度升高则向低频方向偏移。经过数据拟合得到了SO4^2-对称伸缩振动的拉曼位移与温度、压力的关系为：ρ=190.44△vp＋0．0027t^2＋2．9019t-111．68。该公式可以用来作为流体包裹体的压力计。