High-pressure x-ray diffraction station at the beijing synchrotron radiation facility

Abstract

In the second phase construction of further insertion devices, beamlines and experimental stations at the Beijing Synchrotron Radiation Facility, a dedicated high-pressure x-ray diffraction station will be constructed. We outline the synchrotron radiation source, beamline optics and high-pressure x-ray diffraction apparatus. This facility is planned to operate for users in 1994.

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

Polarization effects in resonant nuclear scattering

Polarization phenomena are present in every radiative transition, whether it is of atomic or nuclear origin. Nuclear resonant scattering of synchrotron radiation is an ideal technique for their study because (a) the probing radiation is in a well characterized polarization state, in most cases linear, (b) the scattered radiation can be efficiently analyzed with polarization filters, and (c) synchrotron pulses are very short compared to the lifetime of a nuclear resonance, resulting in a clean signal. In the following article we describe experimental and theoretical studies of the 14.4 keV Mössbauer resonance of ⁵⁷Fe and its transitions with linear and circular polarization. After introducing the required instrumentation a formalism to calculate time dependent polarization phenomena is derived. With the help of different scattering geometries we illustrate various aspects, such as polarization mixing and selective excitation of subsets of the resonance. Perhaps the most fascinating example is the Faraday geometry where the E-vector rotates several 360^ο turns during the lifetime of the resonant scattering. A comparison of this phenomenon with the optical Faraday effect is given. New powerful synchrotron radiation sources will enable researchers to exploit polarization phenomena in nuclear resonant scattering to detect subtle changes in physically and chemically relevant systems.

     

High-pressure Mössbauer spectroscopy with nuclear forward scattering of synchrotron radiation

Abstract

Using a diamond anvil cell, high-pressure ⁵⁷Fe Mössbauer spectroscopy has been performed with the nuclear forward scattering of synchrotron radiation. A pressure-induced magnetic hyperfine interaction at ⁵⁷Fe in SrFeO_{2, 97} has been detected at 44 GPa and 300 K for a first time by a quantum-beat modulation of the decay rate after collective nuclear excitation by the synchrotron pulse. The basic concept and method used to detect nuclear forward scattering with synchrotron radiation are discussed.     

Current progress and future developments in sychrotron radiation instrumentation for high-pressure research including the esrf programme

Abstract

The field of synchrotron radiation instrumentation and techniques for high-pressure research is reviewed. Current state-of-the-art, recent developments, main directions of progress and areas with the greatest need for further developments are discussed. Large volume devices, diamond-anvil cells, temperature variation, detectors, all diffraction techniques and dispersive x-ray absorption are covered. Theplanned ESRF high-pressure facilities and programme are presented.     

Application of Advanced Synchrotron Radiation–Based and Conventional Molecular Techniques in Recent Research on Molecular Structure,Metabolic Characteristics,and Nutrition in Coproducts from Biofuel Processing

Abstract

Advanced synchrotron radiation infrared microspectroscopy, as a nondestructive and rapid analytical technique, is able to simultaneously reveal the structural, chemical, and environmental features of biomaterials at cellular and molecular levels within intact tissue. However, to date, this advanced synchrotron-based technique is still seldom used by feed and nutrition scientists. This article aims to provide detailed information regarding how to apply advanced synchrotron radiation–based and conventional molecular techniques to research in coproducts from biofuel processing on the molecular structure, metabolic characteristics, and nutrition. The information described in this article provides better insight on coproduct research progress and updates with advanced synchrotron radiation-based and globar-based (conventional) molecular spectroscopy.     

A large volume pressure cell for high temperatures

Abstract

Studies of matter under very high pressure at synchrotron radiation sources are mostly done using pressure cells with single-crystal diamond anvils. In some cases the available volume (≤ 10^?3mm³)in such cells causes problems especially at high temperature and for crystal synthesis. To ensure sufficient homogeneity of pressure and temperature, the use of cells with large sample volumes (≥ 1 mm³) is necessary.

Existing devices for such measurements are compared with a novel setup which consists of a toroidal anvil arrangement and a lightweight (50 kg) press with 250 tonnes (2.5 MN) capacity. Preliminary tests of this instrument with synchrotron radiation are reported.

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

High-Pressure Phase Relationships for FeS

Phase relationships for FeS polymorph have been studied at the pressure of 16-20 GPa and temperature of 300-1350 K by in situ X-ray observation using a large volume high-pressure apparatus and a synchrotron radiation. Contrary to Fei's prediction [1], we found the stability field of NiAs-type phase of FeS extending at least to 18 GPa. Results of in situ X-ray observation correspond with the NiAs-hexagonal phase boundary determined by Kusaba et al . [2, 3]. Assuming the straight NiAs-hexagonal phase boundary, we estimate that the NiAs-hexagonal-liquid triple junction is located at 39.5 GPa and 2300 K.     

Energy dispersive x-ray diffraction of micro-crystals at ultrahigh pressures

Abstract

Ultrahigh pressures and temperatures in diamond-anvil cells are achieved at the expense of reducing sample volume. The capability of x-ray diffraction with high spatial resolution is most fundamental for probing microscopic samples at the maximum P-T and for minimizing the effect of gradients. Polychromatic synchrotron radiation with energy dispersive x-ray diffraction is ideal for the development of new classes of structural microprobes. Primary x-ray beams down to 3 microns can be produced with microbeam slit systems and microfocusing optical devices. The microprobe can be routinely used for a variety of high-pressure experiments, including single-crystal x-ray diffraction above 50 GPa, polycrystal-line diffraction above 300 GPa, deviatoric strain measurements, and diffraction at simultaneous high pressure and temperature.     

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     

High-pressure Mössbauer studies of magnetism in RFe2 Laves phases and Eu-chalcogenides

A review is given on current high-pressure studies of magnetism employing the new method of nuclear forward scattering of synchrotron radiation as well as the conventional Mössbauer effect. Comparative studies of the magnetic properties of intermetallic RFe₂ Laves phases and Eu(II)-chalcogenides are described. We present as examples the pressure induced changes in YFe₂ and ScFe₂ at pressures up to 100 GPa as well as studies of EuTe in the NaCl-type and the CsCl-type high-pressure phase. Future high-pressure applications of nuclear resonant scattering will be discussed.     

Phase transitions and equations of state at multimegabar pressures

Abstract

Review of phase transitions and equations of state at multimegabar pressures (100–300 GPa) is presented. Energy dispersive x-ray diffraction techniques in conjunction with synchrotron radiation sources are used. Besides several transition metals, Pt to 282 GPa, Re to 251 GPa, W to 209 GPa, and Fe to 255 GPa, the special focus is on Group IVA elements and isoelectronic III-V compounds. At high pressure, the isoelectronic materials are isostructural and exhibit similar equation of state.     

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.     

Protein crystallography with the PILATUS 1M detector at the Swiss Light Source

The last few years have seen an increase in the demand of automation at synchrotron radiation facilities. The main driving forces behind this quest are the Structural Genomics Centers and related projects [1], with their need for large throughput of samples and an increasing number of relatively unskilled users with ever increasing demands.

In order to meet the needs of this diverse community, the structure determination process must be streamlined. A production pipeline for high volume determination of structures requires optimization and automation of current processes in use at synchrotron facilities. The ultimate goal is to arrive at a system that, with little more input than a sample, will provide the researcher with the final molecular structure.     

2-d data collection in high pressure powder diffraction studies-applications to semiconductors

Abstract

Using angle-dispersive diffraction techniques and synchrotron radiation, we have made a detailed re-examination of the high-pressure behaviour of a number of core II-VI, III-V and group IV semiconductors. Despite much previous work on these materials, the good resolution afforded by angle-dispersive techniques, and the high-sensitivity of the image-plate area detector have yielded many new results which reveal that the accepted structural systematics have to be modified quite substantially. In this paper, we summarise the newly emerging structural systematics, and use the results to show how access to full 2-d powder patterns has proved essential in determining correct crystal structures.     

Optics and beamlines for high-pressure research at the european synchrotron radiation facility

Abstract

The European Synchrotron Radiation Facility (ESRF) is the first high-energy, high-brilliance synchrotron radiation source in operation today and it is ideally suited to high pressure research. White-beam and monochromatic diffraction techniques are being optimized in particular for structural studies of low-Z materials and poor scatterers generally, the best example being hydrogen single crystals at very high pressures. Most high pressure measurements are carried out on a versatile beamline equipped with a wiggler and an undulator. Focusing and image plates are used in all monochromatic angle-dispersive studies. The success of the high pressure programme has so far been achieved on a non-optimized beamline, but the next phase of the programme needs an optimized facility. A beamline is being constructed to fully exploit the intrinsic qualities of this unique source and insertion devices for high pressure studies. Its main design concepts are presented.     

Energy - dispersive X - ray diffraction of the ammonium - halides under pressure

Abstract

The structure of the ammonium halides NH₄X (X = Cl, Br, I) has been studied under pressure up to 40 GPa by energy dispersive X-ray diffraction using synchrotron radiation. Equations of state and a discussion on the possible structure of phase V will be presented.     

ESRF 11th users' meeting and workshops

More than 90 participants from Europe, the US and Japan gathered from April 27 to 29, 2005, in Zeuthen, near Berlin, to hold a lively international meeting on time-resolved soft X-ray science. The meeting continued the series of preceding workshops held in 2002 in Napa (California, USA) and in 2003 in Montreux (Switzerland). It was organized by the three synchrotron radiation sources BESSY (Berlin, Germany), the Swiss Light Source SLS (Villigen) and the French synchrotron radiation source SOLEIL (Orsay).

The aim of the workshop was to bring together the existing ultrafast laser community and the emerging ultrafast X-ray community in order to discuss recent scientific highlights from both fields and to outline new directions for the application of ultrafast X-rays.     

Ultrafast X-ray science at the advanced light source

On May 19, 2004, 250 guests from all over the world joined the DESY research center to celebrate 40 years of research with synchrotron radiation at DESY in Hamburg. “The first measurements with the light beam from the DESY ring accelerator started in 1964. DESY was one of the seed laboratories in which the worldwide success story of research with synchrotron radiation began,” Albrecht Wagner, chairman of the DESY Board of Directors, explained in his welcoming address. “Today, more than 1,900 scientists from 31 countries come to DESY every year to carry out experiments with synchrotron radiation.”

Forty years ago, synchrotron radiation at DESY started from scratch. At the beginning of the 1960s, the radiation generated by the electrons in the bending magnets of their new 6 GeV electron synchrotron was regarded by DESY particle physicists as an unwanted, disruptive effect.     

Pressure effect on the electromotive force of the type R thermocouple

ABSTRACT

The pressure effect on the electromotive force (EMF) of a Pt13Rh–Pt (type R) thermocouple was examined to determine the temperature measurement accuracy of solid pressure medium apparatuses in high-pressure experiments. Single-wire EMFs were measured up to pressure of 13?GPa and temperature of 1173?K with a Kawai-type multi-anvil apparatus for Pt13Rh and Pt based on the single-wire method. The pressure conditions along the wires were evaluated by in situ X-ray diffraction using synchrotron X-ray radiation. The pressure effect of the Seebeck coefficients of Pt13Rh and Pt were determined by the analysis of the single-wire EMFs and pressure–temperature profiles along the wires and was virtually consistent with those determined in previous studies at lower pressures and temperatures. For type R thermocouple, the difference between the nominal and real temperatures was determined to be as large as –75?K at 13?GPa and 873?K.     

The spring-8 project and the high pressure group in japan

Abstract

Two major synchrotron radiation projects are presented, the conversion of the 30GeV TRISTAN collider into an ultra-high-brilliance machine and Spring-8, the 8 GeV Japanese third generation source. The Japanese high-pressure group is introduced and its plans for Spring-8 are described in the context of the proposed scientific programme which covers physics and chemistry, earth and planetary science, material science and shock wave compression. The equipment programme and requirements include multianvil presses with high-temperature capability, diamond-anvil cells with low- or high-temperature capabilities, shock compression apparatus and image-plate systems. The latest developments include a high-sensitivity ruby fluorescence detector and a fan-type multiple slit system to allow the use of position-sensitive detectors with multianvil devices.

Presented at (he IUCr Workshop on ‘Synchrotron Radiation Instrumentation for HighPressure Crystallography’. Daresbury Laboratory 20-21 July 1991