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.     

Deformation textures produced in diamond anvil experiments, analysed in radial diffraction geometry

Diamond anvil cells may not only impose pressure upon a sample but also a compressive stress that produces elastic and plastic deformation of polycrystalline samples. The plastic deformation may result in texture development if the material deforms by slip or mechanical twinning, or if grains have a non-equiaxed shape. In radial diffraction geometry, texture is revealed by variation of intensity along Debye rings relative to the compression direction. Diffraction images (obtained by CCD or image plate) can be used to extract quantitative texture information. Currently the most elegant and powerful method is a modified Rietveld technique as implemented in the software package MAUD. From texture data one can evaluate the homogeneity of strain in a diamond anvil cell, the strain magnitude and deformation mechanisms, the latter by comparing observed texture patterns with results from polycrystal plasticity simulations. Some examples such as olivine, magnesiowuestite, MgSiO(3) perovskite and ε-iron are discussed.     

Quantitative Rietveld texture analysis of CaSiO(3) perovskite deformed in a diamond anvil cell

The Rietveld method is used to extract quantitative texture information from a single synchrotron diffraction image of a CaSiO(3) perovskite sample deformed in axial compression in a diamond anvil cell. The image used for analysis was taken in radial geometry at 49?GPa and room temperature. We obtain a preferred orientation of {100} lattice planes oriented perpendicular to the compression direction and this is compatible with [Formula: see text] slip.     

High pressure studies using two-stage diamond micro-anvils grown by chemical vapor deposition

Ultra-high static pressures have been achieved in the laboratory using a two-stage micro-ball nanodiamond anvils as well as a two-stage micro-paired diamond anvils machined using a focused ion-beam system. The two-stage diamond anvils’ designs implemented thus far suffer from a limitation of one diamond anvil sliding past another anvil at extreme conditions. We describe a new method of fabricating two-stage diamond micro-anvils using a tungsten mask on a standard diamond anvil followed by microwave plasma chemical vapor deposition (CVD) homoepitaxial diamond growth. A prototype two-stage diamond anvil with 300?µm culet and with a CVD diamond second stage of 50?µm in diameter was fabricated. We have carried out preliminary high pressure X-ray diffraction studies on a sample of rare-earth metal lutetium sample with a copper pressure standard to 86?GPa. The micro-anvil grown by CVD remained intact during indentation of gasket as well as on decompression from the highest pressure of 86?GPa.     

In situ conductivity measurement of matter under extreme conditions by film fabrication on diamond anvil cell

The film-fabricating technology has been used to prepare the microcircuit on diamond anvil for resistivity measurement under extreme conditions. We chose molybdenum as the electrode material and alumina as the insulator and protective material. The sample thickness measurement was conducted and then the resistivity correction was performed under different thickness. The experimental error was proved to be less than 10%. By mounting alumina film between diamond anvil and microcircuit, high-temperature performance of a laser heating diamond anvil cell was improved obviously, which is available for in situ resistivity measurement under high pressure and high temperature. Meanwhile, the impedance spectroscopy of a powdered semiconductor sample was detected. Through the impedance arcs obtained, the grain boundary contribution to the resistivity can be well distinguished.     

Elastic and plastic deformation of NaCl and Ni3Al polycrystals during compression in a multi-anvil apparatus

Abstract

The compression behaviour in a multi-anvil apparatus of pure NaCl and of a foil of Ni₃Al embedded in a pressure medium of NaCl has been studied by energy-dispersive X-ray diffraction. At ambient temperature, the pressure and stresses, determined from line positions of NaCl, were constant throughout the sample chamber. Line positions and line widths of NaCl reflections were reversible on pressure release. A saturation of microstrains observed in NaCl at 2 GPa is thus attributed to brittle fracture setting in at uniaxial stresses of around 0.3 GPa. Ni₃Al polycrystals, in contrast, undergo extensive (ductile) plastic deformation above 4 GPa. The compression behaviour of both Ni₃Al and NaCl is identical to that previously determined in a diamond anvil cell. While a multi-anvil device thus has the advantage, compared with a diamond anvil cell, of constant pressure and stress throughout the sample chamber, microstrains in poly-crystalline samples arise in both devices. Samples in a multi-anvil apparatus thus need to be mixed with a pressure medium and to consist of essentially single crystals just as in a diamond anvil cell. Annealing experiments at high pressures confirm that the release of the uniaxial stress component in the pressure medium does not cause a release of microstrains in the embedded sample if the latter has been plastically deformed. Annealing for the purpose of attaining hydrostatic conditions in compression studies thus has to be carried out with care.     

Methodology for in situ synchrotron X-ray studies in the laser-heated diamond anvil cell

ABSTRACT

A review of some important technical challenges related to in situ diamond anvil cell laser heating experimentation at synchrotron X-ray sources is presented. The problem of potential chemical reactions between the sample and the pressure medium or the carbon from the diamond anvils is illustrated in the case of elemental tantalum. Preliminary results of a comparison between reflective and refractive optics for high temperature measurements in the laser-heated diamond anvil cell are briefly discussed. Finally, the importance of the size and relative alignment of X-ray and laser beams for quantitative X-ray measurements is presented.     

Diamond anvil Raman gauge in multimegabar pressure range

The first-order Raman band of diamond anvils has been investigated at pressure up to 380 GPa in order to develop an optical pressure determination method. The high frequency edge of the band was calibrated by the pressure scale of the equation of state of Pt. The universality of the relationship between the sample pressure and the edge-frequency was confirmed up to 370 GPa and the usefulness of the diamond anvil Raman gauge was demonstrated. Using the diamond anvil Raman spectroscopy, the stress-state of the anvil culet was directly observed in the multimegabar pressure range. Obtained pressure dependence of the shear stress suggested further extension of feasible pressure beyond 400 GPa.     

Diamond anvil cell, 50th birthday

The year 2008 marked the fiftieth birthday of the diamond anvil cell. Its birth took place when Alvin Van Valkenburg, while working with his colleagues, Charles E. Weir, Ellis R. Lippincott, and Elmer N. Bunting, first realized that he could look right through one of the diamond anvils and see a sample while it was at high pressure. In the following years, these scientists and many others adapted the diamond anvil cell to a wide variety of analytical techniques that have provided an impressive amount of information about materials at high pressures and high temperatures. But, virtually all of those techniques start with looking into the diamond anvil cell.     

Conical support for double-stage diamond anvil apparatus

ABSTRACT

Both micro-paired and conical support type double-stage diamond anvil cells (ds-DAC) were tested using a newly synthesized ultra-fine nano-polycrystalline diamond (NPD). Well-focused X-ray sub-micron beam and the conically supported 2nd stage anvils (micro-anvils) with 10?μm culet enable us to obtain good quality X-ray diffraction peaks from the sample at around 400?GPa. The relationship between confining pressure and sample pressure depends heavily on the initial height (thickness) of micro-anvils, the difference of a few micrometers leads to a quite different compression path. The conical support type is a solution to retain both enough thickness and strength of micro-anvils at higher confining pressure conditions. All conical support ds-DAC experiments terminated by the failure of the 1st stage anvil instead of 2nd one. The combination of ultra-fine NPD 2nd stage anvil and NPD 1st stage anvil opens a new frontier for measurement of the X-ray absorption spectrum above 300?GPa.     

On intensities in high pressure neutron powder diffraction using single and polycrystalline diamond anvils: small versus large sample volumes

We report a quantitative comparison of measured intensities of neutron powder diffraction data collected in a single-crystal diamond anvil cell and in large-volume sintered diamond anvils. As expected from the difference in sample volumes, the latter provides 1–2 orders of magnitude higher intensities, depending on the anvil material. The remaining differences are due to effects of absorption and angular aperture.     

Hybrid Bridgman anvil design: an optical window for in situ spectroscopy in large volume presses

The absence of in situ optical probes for large volume presses (LVPs) often limits their application to high-pressure materials research. In this article, we present a unique anvil/optical window design for use in LVPs, which consists of an inverted diamond anvil seated in a Bridgman-type anvil. A small cylindrical aperture through the Bridgman anvil ending at the back of diamond anvil allows optical access to the sample chamber and permits direct optical spectroscopy measurements, such as ruby fluorescence (in situ pressure) or Raman spectroscopy. The performance of this anvil design has been demonstrated by loading KBr to a pressure of 14.5 GPa.     

高温高压下硬水铝石状态方程研究

 在金刚石压砧装置上,用氧化铝膜作绝热层,借助同步辐射和双面激光加温系统,分析了硬水铝石在高温高压下的结构变化,并分别用理论和实验的方法得出了其结构参数,得到了样品在不同压力温度下的体模量。这对于人们认识和研究地壳结构和地球内部物质的演化具有重要意义。研究发现,在常温和高温时其压缩率有明显不同,在高温高压范围内,其晶格常数和晶胞体积的变化非常接近样品在高压常温下的情况;而在高温低压范围内,情形和常温时有较大差别。在实验过程中并没有发现相变的产生。     

静-动加载相结合的材料状态方程实验平台的研制

根据神光-Ⅱ第九路高功率激光加载的特点,对传统静高压金刚石压砧装置进行了改进和优化设计,研制出了适合高功率激光加载条件下材料宽域状态方程研究的新型静高压靶.在神光-Ⅱ高功率激光装置上建立了基于静高压金刚石压砧和动高压激光相结合的材料宽域状态方程研究平台.利用这一平台开展了超纯水的宽域状态方程实验探索,获得了较好的实验结果.     

苯甲酸脱羧反应过程的拉曼光谱研究

应用水热金刚石压腔结合拉曼光谱技术研究了升温过程中苯甲酸在水中的变化及拉曼谱图。结果表明：低温升温过程中,苯甲酸的拉曼谱图中各个特征振动谱峰没有变化,苯甲酸没有与水反应。随着温度的继续升高,苯甲酸的拉曼谱图中的特征振动峰逐渐变弱。升至150 ℃时,羧基的拉曼特征谱峰消失,说明此过程中苯甲酸发生了脱羧反应。继续升温至170 ℃,苯甲酸溶解消失。随后将体系降至常温,发现有晶体析出。由其拉曼谱图可知,重结晶的晶体含有苯环的特征峰,说明有芳香烃析出。但是没有测到羧基的特征拉曼谱峰,说明重结晶的晶体不是苯甲酸。整个过程可以说明,芳香烃在溶解重结晶过程中是可逆的,羧基是不可逆的。     

复合型多晶金刚石末级压砧的制备并标定六面顶压机6-8型压腔压力至35GPa

通过分析二级6-8型大腔体静高压装置八面体压腔的受力状况, 研制了一种使用成本低、尺寸大且易于加工的多晶金刚石-硬质合金复合二级(末级)顶锤(压砧). 采用原位电阻测量观测Zr在高压下相变(α-ω, 7.96 GPa; ω-β, 34.5 GPa)的方法, 标定了由多晶金刚石-硬质合金复合末级压砧构建的5.5/1.5(传压介质边长/二级顶锤锤面边长, 单位: mm)组装的腔体压力. 实验表明, 自行研制的多晶金刚石-硬质合金复合末级压砧可使基于国产六面顶压机构架的二级加压系统的压力产生上限从约20 GPa提高到35 GPa以上, 拓展了国内大腔体静高压技术的压力产生范围. 应用这一技术, 我们期望经过末级压砧材料与压腔设计的进一步优化, 在基于国产六面顶压机的二级6-8 型大腔体静高压装置压腔中产生超过50 GPa的高压. 关键词： 二级6-8型大腔体静高压装置 多晶金刚石-硬质合金复合末级压砧 压力标定     

金刚石对顶砧中四点探针法精确测量样品电阻率的电极因素

 为了解金刚石对顶砧上电阻率高压原位测量中的电极效应,使用有限元分析方法,对样品中的稳恒电流场进行了模拟计算,发现电极的几何尺寸以及电极与样品电阻率的差别都会对测量误差产生影响。结果发现：电极的尺寸越大,误差越大;电极与样品电阻率数值差越大,误差越大。由此给出了减小电极效应以及减小测量误差的方法。     

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.     

Thermal conductivity of hcp iron at high pressure and temperature

Results of steady-state heat transfer experiments on iron in laser-heated diamond anvil cell, combined with numerical simulation using finite-element method are reported. Thermal boundary conditions, dimensions of sample assemblage, heating-laser beam characteristics and relevant optical properties have been well defined in the course of experiments. The thermal conductivity of the polycrystalline hexagonal-iron foil has been determined up to pressure 70 GPa and temperature 2000 K. At these conditions, the conductivity value of 32±7 W/m K was found. Sources of errors arising from uncertainties in input parameters and applied experimental procedures are discussed. Considering results of earlier preferred-orientation studies in diamond anvil cell, an averaging effect of polycrystalline texture on the intrinsic anisotropy is assumed. The obtained conductivity is interpreted as an effective value, falling in between the upper and lower bounds on the average conductivity of a random aggregate of uniaxial crystals.     

Mechanical, structural, and spectroscopic properties of C70 fullerite phases produced under high pressure and shear

X-ray diffraction patterns, Raman spectra, and the hardness of C₇₀ fullerite subjected to a high pressure with shear are investigated. It is shown that these conditions favor the phase transformation of molecular fullerite into the hard amorphous phase. The hardness of a specimen removed from a diamond anvil cell loaded up to 26 GPa under shear deformation applied is found to be equal to 30 GPa.