Studies of local and intermediate range structure in crystalline and amorphous materials at high pressure using high-energy X-rays

2007 ◽  
Vol 22 (2) ◽  
pp. 108-112 ◽  
Author(s):  
Lars Ehm ◽  
Sytle M. Antao ◽  
Jiuhua Chen ◽  
Darren R. Locke ◽  
F. Marc Michel ◽  
...  
Keyword(s):  
Phase Transition ◽  
High Pressure ◽  
Atomic Structure ◽  
Amorphous Materials ◽  
High Energy ◽  
Liquid Gallium ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Current State

The method of high-energy total elastic X-ray scattering to determine the atomic structure of nanocrystalline, highly disordered, and amorphous materials is presented. The current state of the technique, its potential, and limitations are discussed with two successful studies on the pressure induced phase transition in mackinawite (FeS) and the high-pressure behavior of liquid gallium.

A multi-length-scale USAXS/SAXS facility: 10–50 keV small-angle X-ray scattering instrument

2013 ◽  
Vol 46 (5) ◽  
pp. 1508-1512 ◽  
Author(s):  
Byron Freelon ◽  
Kamlesh Suthar ◽  
Jan Ilavsky
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
And Performance ◽  
New Facility ◽  
Ray Scattering

Coupling small-angle X-ray scattering (SAXS) and ultra-small-angle X-ray scattering (USAXS) provides a powerful system of techniques for determining the structural organization of nanostructured materials that exhibit a wide range of characteristic length scales. A new facility that combines high-energy (HE) SAXS and USAXS has been developed at the Advanced Photon Source (APS). The application of X-rays across a range of energies, from 10 to 50 keV, offers opportunities to probe structural behavior at the nano- and microscale. An X-ray setup that can characterize both soft matter or hard matter and high-Zsamples in the solid or solution forms is described. Recent upgrades to the Sector 15ID beamline allow an extension of the X-ray energy range and improved beam intensity. The function and performance of the dedicated USAXS/HE-SAXS ChemMatCARS-APS facility is described.

In situ high pressure phase transition of alcohol intercalated zirconium phosphate observed by synchrotron X-ray scattering

2004 ◽  
Vol 65 (2-3) ◽  
pp. 615-618
Author(s):  
Ludvı́k Beneš ◽  
Vı́tězslav Zima ◽  
Klára Melánová ◽  
Miloš Steinhart ◽  
Manfred Kriechbaum ◽  
...  
Keyword(s):  
Phase Transition ◽  
High Pressure ◽  
Zirconium Phosphate ◽  
High Pressure Phase ◽  
X Ray ◽  
X Ray Scattering ◽  
High Pressure Phase Transition ◽  
Pressure Phase ◽  
Ray Scattering

High hydrostatic pressure small-angle X-ray scattering cell for protein solution studies featuring diamond windows and disposable sample cells

2008 ◽  
Vol 41 (1) ◽  
pp. 167-175 ◽  
Author(s):  
Nozomi Ando ◽  
Pascale Chenevier ◽  
Martin Novak ◽  
Mark W. Tate ◽  
Sol M. Gruner
Keyword(s):  
High Pressure ◽  
Small Angle ◽  
Ambient Pressure ◽  
X Rays ◽  
High Pressure Cell ◽  
X Ray ◽  
Pressure Cell ◽  
X Ray Scattering ◽  
Solution Studies ◽  
Ray Scattering

A high-pressure cell for synchrotron small-angle X-ray scattering (SAXS) studies of protein solutions is described. The design was optimized for use at up to 400 MPa in liquid pressure and with 8−12 keV X-rays with particular emphasis on the ease of use. The high-pressure cell was fabricated from corrosion-resistant Inconel 725 (Special Metals Corporation, Huntington, WV, USA) and featured Poulter-type windows [Poulter (1932).Phys. Rev.40, 861–871]. Flat natural diamonds, 500 µm thick, were recycled from diamond anvil cells and were shown to perform well as high-pressure SAXS windows. For a simple and effective method of sample isolation, disposable plastic sample cells with a defined path length and reproducible parasitic scattering were designed. These sample cells enable efficient use of synchrotron time. The cells facilitate rapid and easy sample changes, eliminate the need to clean the cell between sample changes, and reduce the sample volume to as low as 12 µl. The disposable cells can also be used separately from the high-pressure cell for SAXS measurements at ambient pressure and temporary storage of samples. The performance of the apparatus is demonstrated with T4 lysozyme.

scholarly journals The GALAXIES inelastic hard X-ray scattering end-station at Synchrotron SOLEIL

2019 ◽  
Vol 26 (1) ◽  
pp. 263-271 ◽  
Author(s):  
J. M. Ablett ◽  
D. Prieur ◽  
D. Céolin ◽  
B. Lassalle-Kaiser ◽  
B. Lebert ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Polarized Light ◽  
Research Direction ◽  
High Energy ◽  
High Energy Resolution ◽  
X Rays ◽  
Circularly Polarized Light ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

GALAXIES is an in-vacuum undulator hard X-ray micro-focused beamline dedicated to the study of the electronic structure of materials with high energy resolution using both photoelectron spectroscopy and inelastic X-ray scattering and under both non-resonant (NR-IXS) and resonant (RIXS) conditions. Due to the penetrating power of hard X-rays and the `photon-in/photon-out' technique, the sample environment is not a limitation. Materials under extreme conditions, for example in diamond anvil cells or catalysis chambers, thus constitute a major research direction. Here, the design and performance of the inelastic X-ray scattering end-station that operates in the energy range from ∼4 keV up to 12 keV is reported, and its capabilities are highlighted using a selection of data taken from recently performed experiments. The ability to scan `on the fly' the incident and scattered/emitted X-ray energies, and the sample position enables fast data collection and high experimental throughput. A diamond X-ray transmission phase retarder, which can be used to generate circularly polarized light, will also be discussed in the light of the recent RIXS–MCD approach.

Two-dimensional focusing of high-energy X-rays by thermal-gradient crystals for small-angle X-ray scattering

2008 ◽  
Vol 41 (1) ◽  
pp. 185-190 ◽  
Author(s):  
Matthias Stockmeier ◽  
Matthias Petermair ◽  
Andreas Magerl
Keyword(s):  
Small Angle ◽  
Thermal Gradient ◽  
Focal Point ◽  
High Energy ◽  
Two Dimensions ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
High Penetration ◽  
Ray Scattering

A novel method for focusing X-rays in two dimensions by thermal-gradient crystals in symmetrical Laue geometry is described. A 225 kV stationary tungsten tube delivers an X-ray beam with a source diameter of about 1.0 mm (full width at half-maximum). The focal point at the detector at a distance up to 16 m from the source is of the same size. The beam at the focusing crystals at half the distance between the source and the detector has typical dimensions of 30 × 30 mm. The intensity of the focal point can be increased by more than 200 times by applying a thermal gradient of about 2.2 K mm−1on the focusing crystals. The described method and apparatus are designed for small-angle X-ray scattering at high photon energies up to 60 keV, where the high penetration power allows experiments on strongly absorbing materials in transmission mode. Particle sizes up to 3000 Å can be detected. First measurements on nanocrystalline tungsten carbide and Teflon yield radii of gyration of 540 Å and 815 Å, respectively.

High-energy X-ray diffuse scattering using Weissenberg flat-cone geometry

2000 ◽  
Vol 33 (4) ◽  
pp. 1046-1050 ◽  
Author(s):  
B. D. Butler ◽  
D. R. Haeffner ◽  
P. L. Lee ◽  
T. R. Welberry
Keyword(s):  
Diffuse Scattering ◽  
High Energy ◽  
Reciprocal Space ◽  
Irregular Shape ◽  
X Rays ◽  
Storage Phosphor ◽  
X Ray ◽  
Image Plate ◽  
X Ray Scattering ◽  
Disordered Crystal

A technique for the measurement of diffuse X-ray scattering on individual reciprocal-space planes using high-energy X-ray photons is described. The method is demonstrated using a disordered crystal of the compound TlSbOGeO4and compared to data collected with a sealed-tube Cu anode source. Measurements were made on a synchrotron undulator beamline at an energy of 45 keV using Weissenberg flat-cone geometry and a storage phosphor (image) plate to detect the scattered X-rays. Advantages of the method include: extension of the accessible diffraction space to both higherandlower wavevectors, the ability to use crystals of irregular shape without the need for complicated absorption corrections, less need to prepare sample surfaces carefully, and the ability to filter fluorescence simply.

scholarly journals High-pressure small-angle X-ray scattering cell for biological solutions and soft materials

2021 ◽  
Vol 54 (1) ◽  
Author(s):  
Durgesh K. Rai ◽  
Richard E. Gillilan ◽  
Qingqiu Huang ◽  
Robert Miller ◽  
Edmund Ting ◽  
...  
Keyword(s):  
High Pressure ◽  
Small Angle ◽  
High Pressures ◽  
Protein Denaturation ◽  
Soft Materials ◽  
High Energy ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

Pressure is a fundamental thermodynamic parameter controlling the behavior of biological macromolecules. Pressure affects protein denaturation, kinetic parameters of enzymes, ligand binding, membrane permeability, ion transduction, expression of genetic information, viral infectivity, protein association and aggregation, and chemical processes. In many cases pressure alters the molecular shape. Small-angle X-ray scattering (SAXS) is a primary method to determine the shape and size of macromolecules. However, relatively few SAXS cells described in the literature are suitable for use at high pressures and with biological materials. Described here is a novel high-pressure SAXS sample cell that is suitable for general facility use by prioritization of ease of sample loading, temperature control, mechanical stability and X-ray background minimization. Cell operation at 14 keV is described, providing a q range of 0.01 < q < 0.7 Å−1, pressures of 0–400 MPa and an achievable temperature range of 0–80°C. The high-pressure SAXS cell has recently been commissioned on the ID7A beamline at the Cornell High Energy Synchrotron Source and is available to users on a peer-reviewed proposal basis.

A Pressure-Induced Phase Transition in a Ternary Microemulsion with an Assembly of a New High-Pressure Cell and Small-Angle X-Ray Scattering Apparatus

1999 ◽  
Vol 38 (Part 1, No. 2A) ◽  
pp. 951-956 ◽  
Author(s):  
Hideki Seto ◽  
Daisuke Okuhara ◽  
Michihiro Nagao ◽  
Shigehiro Komura ◽  
Takayoshi Takeda
Keyword(s):  
Phase Transition ◽  
High Pressure ◽  
Small Angle ◽  
High Pressure Cell ◽  
X Ray ◽  
Pressure Cell ◽  
X Ray Scattering ◽  
Ray Scattering

X-Ray Scattering above 100KeV

1988 ◽  
Vol 143 ◽  
Author(s):  
J. B. Hastings
Keyword(s):  
High Energy ◽  
X Rays ◽  
Synchrotron Source ◽  
X Ray ◽  
High Energies ◽  
X Ray Scattering ◽  
Very High ◽  
Ray Scattering

Conventional x-ray scattering studies have been limited to photon energies (wavelengths) in the 5 to 20 KeV (approx. 2A to 0..5A) regime. With these energies absorption lengths limit the volume of illumination to the first tens of microns of samples. If it were possible to use x-rays of very high energies, true bulk (tens of millimeters) samples could be studied. The availability, intensity and resolution possible with high energies will be discussed and their role in the expanding field of x-ray scattering presented. Preliminary studies at the Cornell High Energy Synchrotron Source (CHESS) will form the basis of these discussions.

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