Laboratory set-up for X-ray diffraction at high pressures

We describe here a simple set-up for X-ray diffraction under high pressure using a diamond anvil cell employing a sealed tube. The set-up works in angular dispersive geometry and is built using rather common components that are available in a research laboratory. We show that using this set-up one can routinely acquire good-quality data for the determination of structural properties under pressure and the equations of state. Technical details are presented along with examples of experimental results for sodium chloride and LiV₂O₄.     

Diamond anvils with a spherical support designed for X-ray and neutron diffraction experiments in DAC

Here, we present new diamond anvils with a spherical support designed for applications in diamond anvil cell (DAC) technique. The main feature of the anvils is the diamond crown of a spherical shape. The assembly of the spherical diamond fixed within a spherical support of a seat made of tungsten carbide or hard metals provides enhanced stability, simple alignment, and large optical and X-ray aperture that makes it very useful for broad applications in DAC technique, particularly for single crystal X-ray and powder neutron diffraction. The anvils were tested in various experiments conducted in a wide pressure–temperature range and showed a very good performance.     

Three-dimensional X-ray diffraction in the diamond anvil cell: application to stishovite

Three-dimensional X-ray diffraction can be used for characterizing the orientation, position, and strain tensor of single grains in a polycrystalline aggregate. Here, we show how the method is well suited for diamond anvil cell data with heterogeneous grain sizes, with an application to two samples of stishovite at 15 and 26 GPa. For each grain, we obtain a well-defined orientation matrix and cell parameters. Center of mass position can also be adjusted to the experimental data, with errors in the present experiment. Finally, strain tensors are adjusted for the individual grains. The stress distribution obtained is in agreement with expectations from the diamond anvil cell geometry and previous measurements of stishovite strength. Advantages and potential for improvement of the method are then discussed.     

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.     

High-energy X-ray diffraction of a hydrous silicate liquid under conditions of high pressure and temperature in a modified hydrothermal diamond anvil cell

In situ high-energy X-ray diffraction measurements were made for the first time on a water-saturated silicate melt at high pressure and temperature. A modified hydrothermal diamond anvil cell (HDAC), designed to minimize the path length of the X-ray beam within a diamond anvil and to increase the solid angle of the diffracted beam, was used to reduce high background contributions and extend X-ray diffraction data collection in Q space. Quantitative differential pair distribution function (PDF) analysis of X-ray diffraction data show that the first measurable (Si–O) peak is 0.095 Å greater in length in the hydrous melt than in the starting glass. Contributions from the H₂O O–O correlations, as well as from the second nearest neighbor O–O correlations within the silicate melt, are evident within the second peak of the differential PDF. The procedure described opens new opportunities to directly investigate volatile-rich melts at high pressure and temperature.     

Strength and equation of state of molybdenum triboride under 80 GPa pressure,using radial X-ray diffraction

The strength and equation of state of molybdenum triboride have been determined under nonhydrostatic compression up to 80?GPa, using an angle-dispersive radial X-ray diffraction technique in a diamond anvil cell (DAC). The RXD data yield a bulk modulus and its pressure derivative as K_0?=?342(6)?GPa with K₀′?=?2.11(17) at ψ?=?54.7°. Analysis of diffraction data using the strain theory indicates that the ratio of differential stress to shear modulus (t/G) ranges from 0.002 to 0.050 at pressures of 4–80?GPa. Together with theoretical results on the high pressure shear modulus, our results here show that molybdenum triboride sample under uniaxial compression can support a differential stress of ～10?GPa when it started to yield with plastic deformation at ～30?GPa. In addition, we draw a conclusion that MoB₃ is not a superhard material but a hard material.     

同步辐射X射线光源在高压科学研究中的应用

同步辐射X射线光源已经成功地应用到高压科学研究的诸多领域.文章简要回顾了同步辐射高压技术的发展历史,简要介绍了同步辐射X射线衍射技术在高压状态方程、强关联体系、地球内部物质以及早期生命起源等研究中的应用.介绍了同步辐射X射线光谱技术(包括晶格振动声子谱的测量)在高压研究中的应用,此外,还介绍了时间分辨的同步辐射技术在冲击压缩研究中的应用,最后展望了未来先进光源应用于高压科学研究的前景.     

Preparation of a macrocrystalline pressure calibrant SrB4O7:Sm 2+ suitable for the HP-HT powder diffraction

A new simplified synthesis of monocrystalline chips of SrB₄O₇: Sm²⁺ pressure calibrant, well-suited for the diamond anvil cell (DAC) powder diffraction experiments, is proposed. It consists of ordinary solid-state synthesis of fine-grained SrB₄O₇: Sm²⁺ and subsequent annealing near melting temperature. The obtained material was characterized and tested in HP-HT DAC experiment.     

High resolution X-ray diffraction studies at high pressures

Abstract

The principal sources of systematic error in high-pressure x-ray structure determination with a diamond anvil cell have been studied in detail. The results of these studies have been used to develop techniques to minimise or correct for these effects.     

顽火辉石的高温高压同步辐射研究

 采用同步辐射能量色散X射线衍射技术、激光加热技术和金刚石对顶砧（DAC）高压装置,在温度为2 000 K和压力为23 GPa的范围内,对采自地幔二辉橄榄岩中的顽火斜方辉石,进行了原位的高温高压能量色散X射线衍射（EDXRD）测量。实验结果表明：当压力为15.3 GPa、温度为1 600 K时（相当于地球内部410 km处的地震波不连续界面的温压环境）,顽火斜方辉石转变为橄榄石的β相——瓦兹利石（Wadsleyite）相;继续加温加压至2 000 K、23 GPa时（相当于地球内部670 km处的地震波不连续界面的温压环境）,顽火斜方辉石相变为钛铁矿（Ilmenite）结构和钙钛矿（Perovskite）结构的混和相。实验结果进一步证明,在地幔中存在的两个地震波不连续界面是由橄榄石、顽火斜方辉石等矿物的相变引起的。     

Pressure-induced phase transformation of CsPbI3 by X-ray diffraction and Raman spectroscopy

The structural transformation of cesium lead iodine (CsPbI₃) has been investigated in diamond anvil cells up to ～15 GPa at room temperature by employing synchrotron radiation X-ray diffraction and Raman spectroscopy. One reversible transformation from orthorhombic (Pnma) to monoclinic (P2₁/m) phase has been observed at 3.9 GPa. Isothermal pressure–volume relationship of orthorhombic CsPbI₃ is well fitted by the third-order Birch–Murnaghan equation of state with K₀ = 14(3) GPa, K′₀ = 6(2) and V₀ = 891(7) ų. The ultralow value of bulk modulus K₀ demonstrates the high compressible nature of CsPbI₃, similar to those of organic–inorganic metal halide perovskites. The present results provide essential information on the intrinsic properties and stability of CsPbI₃, which may be applied in photovoltaic devices.     

Combined X-ray absorption and X-ray diffraction under high pressure

ABSTRACT

X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) are two complementary structural techniques. Their combination improves the understanding of the effect of pressure on materials as illustrated by examples taken from studies on different types of materials (semiconductors, molecular solid, ferroelectric perovskite and gas mixture). The introduction of nanopolycrystalline diamonds anvils has extended XAS to high-energy edges with the possibility to use energy-scanning XAS beamlines where XRD can be performed in addition to XAS experiments.     

Rietveld analysis of high pressure powder diffraction data

Abstract

X-ray and neutron powder diffraction data obtained from samples contained within high pressure cells are generally of lower quality than data collected from samples at ambient conditions. The far smaller sample size as well as possible contamination of the pattern by the pressure cell means that Rietveld refinement techniques must be adapted to extract the maximum useful information from the data. These problems become paramount as larger structures at high pressure are attempted. Techniques such as “leBail extraction”, “soft restraints” and “rigid body refinement” will be discussed with application to analysis of high pressure neutron powder diffraction data.     

White-beam X-ray diffraction and radiography studies on high-boron-containing borosilicate glass at high pressures

ABSTRACT

Multi-angle energy-dispersive X-ray diffraction studies and white-beam X-ray radiography were conducted with a cylindrically shaped (1?mm diameter and 0.7?mm high) high-boron-content borosilicate glass sample (17.6% B₂O₃) to a pressure of 13.7?GPa using a Paris-Edinburgh (PE) press at Beamline 16-BM-B, HPCAT of the Advanced Photon Source. The measured structure factor S(q) to large q?=?19 Å^?1 is used to determine information about the internuclear bond distances between various species of atoms within the glass sample. Sample pressure was determined with gold as a pressure standard. The sample height as measured by radiography showed an overall uniaxial compression of 22.5% at 13.7?GPa with 10.6% permanent compaction after decompression to ambient conditions. The reduced pair distribution function G(r) was extracted and Si–O, O–O and Si–Si bond distances were measured as a function of pressure. Raman spectroscopy of the pressure recovered sample as compared to starting material showed blue-shift and changes in intensity and widths of Raman bands associated with silicate and four-coordinated boron.     

A system for doing low temperature-high pressure single crystal X-ray diffraction with a synchrotron source

Abstract

A new diamond anvil cell and a helium flow cryostat have been developed for X-ray diffraction on single crystals at low temperatures and high pressures using white radiation of a synchrotron beam. This novel instrument especially enables continuous change of temperature and pressure of the sample without any adjustment of alignment. Automatic search for diffraction peaks can be performed since less than 30 pm eccentricity can be maintained during the rotation of the cell in the cryostat and the rotation of the cryostat on the goniometer head. The minimum temperature reached is 46 K. Measurements of solid 4He at 11.8 GPa are presented which confirm the stability of the hcp phase on this isobar.     

镁铝石榴子石的高压X射线衍射研究

 对于天然镁铝石榴子石（Pyrope）,在0～25.3 GPa压力条件下,在美国布鲁克海汶（Brookhaven）国家实验室国家同步辐射实验站,利用金刚石压腔装置（DAC）,进行了角散X 射线粉末衍射的高压原位测量,获得了天然镁铝石榴子石随压力变化的衍射图谱。采用Materials Studio软件的Refinement模块对衍射图谱进行了分析,得到了镁铝石榴子石的晶胞参数及其随压力的变化,进而利用Birch-Murnaghan状态方程进行数值拟合,得到了镁铝石榴子石的零压体弹模量B₀＝199 GPa（B′₀＝4）。     

碳化硅压腔和高压下的中子衍射

使用宝石级碳化硅晶体作为压砧材料,成功研制出了碳化硅压腔（MAC）,并应用全景式MAC进行了高压下物质的中子衍射实验研究.结果表明,MAC是一种既能产生高的压力又具有大的高压样品室的装置,特别适合于高压下的中子衍射研究.