A new cell for X-ray absorption spectroscopy study under high pressure

X-ray absorption fine structure （XAFS） spectroscopy is a powerful technique for the investigation of the local environment around selected atoms in condensed matter. XAFS under pressure is an important method for the synchrotron source. We design a cell for a high pressure XAFS experiment. Sintered boron carbide is used as the anvils of this high pressure cell in order to obtain a full XAFS spectrum free from diffraction peaks. In addition, a hydraulic pump was adopted to make in-suit pressure modulation. High quality XAFS spectra of ZrH2 under high pressure （up to 13 GPa） were obtained by this cell.     

X-ray absorption spectroscopy under high pressures in diamond anvil cells

Abstract

Although potentially extremely important for understanding the high-pressure microscopic behaviour of materials, over the years the area of high-pressure EXAFS in particular using diamond anvil cells has proved to be technically difficult. This has significantly hampered its development. The interference of X-ray dimaction from the diamonds in the diamond anvil cell with the absorption signal has proved to be a challenging problem to tackle, restricting the use of high-pressure EXAFS to energies below about 11 key Below 11 keV however the technique is also limited due to absorption of incident X-rays by the diamonds making it virtually impossible to conduct X-ray absorption experiments below about 9keV In this paper we describe in detail the methodology for scanriirig high-pressure EXAFS in diamond anvil cells and examine the origins of the associated problems and ways of dealing with them. We also demonstrate that it is possible to extend the useful range of studied absorption edges from 7keV up to at least 30keV This brings about new opportunities for high pressure EXAFS using diamond anvil cells.     

X-ray absorption spectroscopy and high pressure

Abstract

The difficulties of the adaptation of high pressure to x-ray absorption are presented. The advantages of the energy-dispersive geometry are discussed as well as the future improvements expected with the new synchrotron radiation sources.

Presented at the IUCr Workshop on ‘Synchrotron Radiation Instrumentation for High Pressure Crystallography’, Daresbury Laboratory 20-21 July 1991     

X-ray photoelectron spectroscopy study of cubic boron nitride single crystals grown under high pressure and high temperature

The defects, impurities and their bonding states of unintentionally doped cubic boron nitride (cBN) single crystals were investigated by X-ray photoelectron spectroscopy (XPS). The results indicate that nitrogen vacancy (V_N) is the main native defect of the cBN crystals since the atomic ratio of B:N is always larger than 1 before Ar ion sputtering. After sputter cleaning, around 6 at% carbon, which probably comes from the growth chamber, remains in the samples as the main impurity. Carbon can substitute nitrogen lattice site and form the bonding states of CBN or CB, which can be verified by the XPS spectra of C1s, B1s and N1s. The C impurity (acceptor) and N vacancy (donor) can compose the donor-acceptor complex to affect the electrical and optical properties of cBN crystals.     

Ferromagnetic materials under high pressure in a diamond-anvil cell:A magnetic study

A magnetic-parameter measurement system for study of ferromagnetic materials under high pressure using a diamondanvil cell is built. The factors affecting the measurement sensitivity are analyzed and the possibility of improving the sensitivity is mentioned. Based on the system, the magnetization curves of iron as a function of pressure are obtained. The start point and end point of pressure-induced magnetic transition of iron are observed at room temperature.     

Phase transition of solid bismuth under high pressure

As a widely used pressure calibrator, the structural phase transitions of bismuth from phase I, to phase II, to phase III,and then to phase V with increasing pressure at 300 K have been widely confirmed. However, there are different structural versions for phase III, most of which are determined by x-ray diffraction(XRD) technology. Using x-ray absorption fine structure(XAFS) measurements combined with ab initio calculations, we show that the proposed incommensurate composite structure of bismuth of the three configurations is the best option. An abnormal continuous increase of the nearest-neighbor distance of phase III with elevated pressure is also observed. The electronic structure transformation from semimetal to metal is responsible for the complex behavior of structure transformation.     

Raman spectroscopy of topiramate under high pressure conditions

Topiramate is a white crystalline solid with powerful anticonvulsant activity and is used to treat epilepsy. Drug manufacturing involves various physical and chemical processes, which may lead to the formation of an unexpected, or undesired, crystalline phase, in a phenomenon known as polymorphism. In this paper, the behavior of topiramate crystal is studied under pressures up to 10.8 GPa using Raman spectroscopy. Under the conditions employed, Raman spectra from topiramate under pressure showed no strong evidence of a phase change, although amorphization may be considered. This may be accounted for by its crystal structure, comprising oppositely running chains of topiramate molecules linked by asymmetric hydrogen bonds, which pose a kinetic barrier against a structural change. It is not yet safe to rule out the existence of topiramate polymorphs, which could possibly be obtained under special crystallization conditions, but not after compression, at least up to 10 GPa. Copyright © 2009 John Wiley & Sons, Ltd.     

A scanning fluorescence spectroscopy of decorin under high pressure

High pressure processing is able to tenderize not only meat but also intramuscular connective tissue, which is mainly composed of collagen. Decorin, one of the proteoglycans, binds to and stabilizes collagen fibrils. It has been suggested that structural weakening of intramuscular connective tissue may result from the disappearance of the decorin–collagen interaction. In this study, the fluorescence spectra and the surface hydrophobicity of decorin molecules were measured under high pressure in order to examine the resulting change in the tertiary structure. The fluorescence intensity and the surface hydrophobicity of decorin molecules both decreased with increasing applied pressure and with applied time at the constant applied pressure, respectively. The observations indicate that the native structure of decorin is maintained during 200 MPa pressurization for less than 30 min.     

Applications of nano-polycrystalline diamond anvils to X-ray absorption spectroscopy under high pressure

ABSTRACT

Recently, nano-polycrystalline diamond (NPD) anvils have been widely applied in high pressure research using X-ray absorption spectroscopy (XAS). The nanometer-sized polycrystallization in NPD anvils enables us to obtain glitch-free X-ray absorption spectra. This advantage of NPD anvils drastically improves the experimental conditions of XAS, which has previously used conventional single-crystal diamond (SCD) anvils. Distorted spectra due to the glitches from the SCD anvils have been an inevitable problem of XAS. This paper reviews recent studies of XAS and related spectroscopic techniques using the NPD anvils, which have mainly been performed on BL39XU of SPring-8. We demonstrate how NPD anvils are useful when using XAS for high pressure research.     

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.     

Synchrotron X-ray diffraction study of phenacite at high pressure

We report the results of a natural phenacite from 0 to 30.9 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at the National Synchrotron Light Source, Brookhaven National Laboratory. Over this pressure range, no phase change or disproportionation has been observed. The isothermal equation of state was determined. The values of V₀, K₀, and K₀′ refined with a third-order Birch-Murnaghan equation of state are V₀=1116.1±1.2 ų, K₀=223±9 GPa, and K₀′=5.5±0.8. Furthermore, we confirm that the linear compressibilities (β) along a and c directions of phenacite are elastically isotropic (β_a=1.50×10^-3 and β_c=1.34×10^-3 GPa^-1). Consequently, it can be concluded that the compressibility of phenacite under high pressures has been accurately constrained.     

X-ray absorption study of Cu,Zn SOD under high pressure

Abstract

We have investigated Cu, Zn Superoxide Dismutase (Cu, Zn SOD) metal sites at high pressure using X-ray absorption. XAS (X-ray Absorption Spectroscopy) gives information on local structure and it is particularly suited to metal site investigation. To the best of our knowledge, this is the first time that protein conformational states have been investigated using the high pressure XAS technique. Cu, Zn SOD catalyses the dismutation of toxic oxygen radicals produced in cells; this reaction occurs at the copper metal site. Structural changes around the copper, induced by pressure, can be directly related to protein substates. Their characterisation is thus important in the understanding of protein activity.

The high-pressure device was a Paris-Edinburgh large volume cell.

Experiments were performed on lyophilised Cu, Zn SOD between 0 and 48 kbar at the copper and zinc K-edges. The two metal local atomic environments have a different behaviour as pressure increases: copper exhibits a more flexible environment; on the contrary, zinc shows small structural modifications. We have identified a state, formed between 3 and 8 kbar, which is stable up to 48 kbar.     

A study on the electrical property of HgSe under high pressure

Using a microcircuit fabricated on a diamond anvil cell, we have measured in-situ conductivity of HgSe under high pressures, and investigated the temperature dependence of conductivity under several different pressures. The result shows that HgSe has a pressure-induced transition sequence from a semimetal to a semiconductor to a metal, similar to that in HgTe. Several discontinuous changes in conductivity are observed at around 1.5, 17, 29 and 49GPa, corresponding to the phase transitions from zinc-blende to cinnabar to rocksalt to orthorhombic to an unknown structure, respectively. In comparison with HgTe, it is speculated that the unknown structure may be a distorted CsCl structure. For the cinnabar-HgSe, the energy gap as a function of pressure is obtained according to the temperature dependence of conductivity. The plot of the temperature dependence of conductivity indicates that the unknown structure of HgSe has an electrical property of a conductor.     

高压电导研究

高压下物质结构和性质会发生很大的改变，电导对于认识压力的作用效应和寻找新的导电材料具有重要意义．高压电导研究所采用的设备主要有金刚石压腔、超高压大腔体装置(大压机)以及高压电导池三种．金刚石压腔可达550GPa压力；超高压大腔体装置压力一般在30GPa以下，可以提供较大体积的样品；高压电导池主要进行流体的电导研究，压力在400MPa以下，有静止和流动两种类型，流动式高压电导池是近年来才发展起来的，其准确方便．文章对目前高压电导的研究进行简单的介绍和分析．     

高压电导研究

高压下物质结构和性质会发生很大的改变,电导对于认识压力的作用效应和寻找新的导电材料具有重要意义.高压电导研究所采用的设备主要有金刚石压腔、超高压大腔体装置（大压机）以及高压电导池三种.金刚石压腔可达550GPa压力;超高压大腔体装置压力一般在30GPa以下,可以提供较大体积的样品;高压电导池主要进行流体的电导研究,压力在400MPa以下,有静止和流动两种类型,流动式高压电导池是近年来才发展起来的,其准确方便.文章对目前高压电导的研究进行简单的介绍和分析.     

Compressibility of Fe1.087Te: a high pressure X-ray diffraction study

Fe_1.087Te exhibits three phases in the pressure range from ambient to 16.6?GPa and becomes amorphous at higher pressures. All three phases have tetragonal symmetry. The low pressure T-phase is stable in the pressure range 0≤P<4.1?GPa and is found to be relatively soft having zero pressure bulk modulus B ₀=36(1)?GPa. The intermediate cT-phase is less compressible with B ₀=88(5)?GPa and stable in the pressure range 4.1≤P<10?GPa while a more compressible phase was observed between 10 and 16.6?GPa.