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.

Instrumental developments for anomalous small-angle X-ray scattering from soft matter systems

2010 ◽  
Vol 43 (6) ◽  
pp. 1479-1487 ◽  
Author(s):  
Michael Sztucki ◽  
Emanuela Di Cola ◽  
Theyencheri Narayanan
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
High Energy ◽  
Detection Sensitivity ◽  
High Energy Resolution ◽  
Anomalous Scattering ◽  
X Ray ◽  
X Ray Scattering ◽  
Counter Ions ◽  
Ray Scattering

An optimized instrument for anomalous small-angle X-ray scattering from charged soft matter is described. The experimental setup takes special care for single-photon detection sensitivity, high energy resolution of the monochromator,in situcalibration of intensity and energy, and the avoidance of radiation damage. Measured intensities are normalized to an absolute scale online, which can be further decomposed to resonant and non-resonant contributions. The performance of the instrument is demonstrated by an example involving cationic surfactant micelles with bromide counter-ions. The counter-ion profile around the micelle is deduced from the analysis of anomalous scattering near theK-absorption edge of bromine. Two different approaches yield similar results for the radial profile of the counter-ions, showing strong condensation of the counter-ions on the micellar surface, in agreement with the inference from electrochemical methods.

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.

scholarly journals High-throughput biological small-angle X-ray scattering with a robotically loaded capillary cell

2012 ◽  
Vol 45 (2) ◽  
pp. 213-223 ◽  
Author(s):  
S. S. Nielsen ◽  
M. Møller ◽  
R. E. Gillilan
Keyword(s):  
Data Processing ◽  
Small Angle ◽  
High Energy ◽  
Flow Cell ◽  
Creeping Flow ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Ray Scattering

With the rise in popularity of biological small-angle X-ray scattering (BioSAXS) measurements, synchrotron beamlines are confronted with an ever-increasing number of samples from a wide range of solution conditions. To meet these demands, an increasing number of beamlines worldwide have begun to provide automated liquid-handling systems for sample loading. This article presents an automated sample-loading system for BioSAXS beamlines, which combines single-channel disposable-tip pipetting with a vacuum-enclosed temperature-controlled capillary flow cell. The design incorporates an easily changeable capillary to reduce the incidence of X-ray window fouling and cross contamination. Both the robot-control and the data-processing systems are written in Python. The data-processing code,RAW, has been enhanced with several new features to form a user-friendly BioSAXS pipeline for the robot. The flow cell also supports efficient manual loading and sample recovery. An effective rinse protocol for the sample cell is developed and tested. Fluid dynamics within the sample capillary reveals a vortex ring pattern of circulation that redistributes radiation-damaged material. Radiation damage is most severe in the boundary layer near the capillary surface. At typical flow speeds, capillaries below 2 mm in diameter are beginning to enter the Stokes (creeping flow) regime in which mixing due to oscillation is limited. Analysis within this regime shows that single-pass exposure and multiple-pass exposure of a sample plug are functionally the same with regard to exposed volume when plug motion reversal is slow. The robot was tested on three different beamlines at the Cornell High-Energy Synchrotron Source, with a variety of detectors and beam characteristics, and it has been used successfully in several published studies as well as in two introductory short courses on basic BioSAXS methods.

Mirror to measure small angle x-ray scattering signal in high energy density experiments

2020 ◽  
Vol 91 (12) ◽  
pp. 123501
Author(s):  
M. Šmíd ◽  
C. Baehtz ◽  
A. Pelka ◽  
A. Laso García ◽  
S. Göde ◽  
...  
Keyword(s):  
Energy Density ◽  
Small Angle ◽  
High Energy ◽  
High Energy Density ◽  
X Ray ◽  
X Ray Scattering ◽  
Scattering Signal ◽  
Ray Scattering

scholarly journals Synthesis and Advanced Characterization of Polymer-Protein Core-Shell Nanoparticles

Catalysts ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 730
Author(s):  
Erik Sarnello ◽  
Tao Li
Keyword(s):  
Particle Size ◽  
Small Angle ◽  
Core Shell ◽  
Assembly Process ◽  
Shell Nanoparticles ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Core Shell Nanoparticles ◽  
Ray Scattering

Enzyme immobilization techniques are widely researched due to their wide range of applications. Polymer–protein core–shell nanoparticles (CSNPs) have emerged as a promising technique for enzyme/protein immobilization via a self-assembly process. Based on the desired application, different sizes and distribution of the polymer–protein CSNPs may be required. This work systematically studies the assembly process of poly(4-vinyl pyridine) and bovine serum albumin CSNPs. Average particle size was controlled by varying the concentrations of each reagent. Particle size and size distributions were monitored by dynamic light scattering, ultra-small-angle X-ray scattering, small-angle X-ray scattering and transmission electron microscopy. Results showed a wide range of CSNPs could be assembled ranging from an average radius as small as 52.3 nm, to particles above 1 µm by adjusting reagent concentrations. In situ X-ray scattering techniques monitored particle assembly as a function of time showing the initial particle growth followed by a decrease in particle size as they reach equilibrium. The results outline a general strategy that can be applied to other CSNP systems to better control particle size and distribution for various applications.

Influence of high energy electron irradiation on the network structure of gelatin hydrogels as investigated by small-angle X-ray scattering (SAXS)

2017 ◽  
Vol 19 (19) ◽  
pp. 12064-12074 ◽  
Author(s):  
Emilia I. Wisotzki ◽  
Paolo Tempesti ◽  
Emiliano Fratini ◽  
Stefan G. Mayr
Keyword(s):  
Electron Irradiation ◽  
Network Structure ◽  
Small Angle ◽  
High Energy ◽  
Energy Electron ◽  
High Energy Electron ◽  
X Ray ◽  
X Ray Scattering ◽  
Structural Differences ◽  
Ray Scattering

Small-angle X-ray scattering revealed ranging structural differences in physically entangled and irradiation-crosslinked gelatin hydrogels.

Microfluidics of soft matter investigated by small-angle X-ray scattering

2005 ◽  
Vol 12 (6) ◽  
pp. 745-750 ◽  
Author(s):  
Alexander Otten ◽  
Sarah Köster ◽  
Bernd Struth ◽  
Anatoly Snigirev ◽  
Thomas Pfohl
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

A new high-resolution small-angle X-ray scattering apparatus using a fine-focus rotating anode, point-focusing collimation and a position-sensitive proportional counter

1984 ◽  
Vol 17 (5) ◽  
pp. 337-343 ◽  
Author(s):  
O. Yoda
Keyword(s):  
High Resolution ◽  
Small Angle ◽  
Proportional Counter ◽  
Anisotropic Scattering ◽  
Photon Flux ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Position Sensitive ◽  
Ray Scattering

A high-resolution small-angle X-ray scattering camera has been built, which has the following features. (i) The point collimation optics employed allows the scattering cross section of the sample to be directly measured without corrections for desmearing. (ii) A small-angle resolution better than 0.5 mrad is achieved with a camera length of 1.6 m. (iii) A high photon flux of 0.9 photons μs−1 is obtained on the sample with the rotating-anode X-ray generator operated at 40 kV–30 mA. (iv) Incident X-rays are monochromated by a bent quartz crystal, which makes the determination of the incident X-ray intensity simple and unambiguous. (v) By rotation of the position-sensitive proportional counter around the direct beam, anisotropic scattering patterns can be observed without adjusting the sample. Details of the design and performance are presented with some applications.

scholarly journals An Optimized Table-Top Small-Angle X-ray Scattering Set-up for the Nanoscale Structural Analysis of Soft Matter

2014 ◽  
Vol 4 (1) ◽  
Author(s):  
T. Sibillano ◽  
L. De Caro ◽  
D. Altamura ◽  
D. Siliqi ◽  
M. Ramella ◽  
...  
Keyword(s):  
Structural Analysis ◽  
Small Angle ◽  
Soft Matter ◽  
X Ray ◽  
X Ray Scattering ◽  
Set Up ◽  
Ray Scattering

scholarly journals Development of combined microstructure and structure characterization facility forin situandoperandostudies at the Advanced Photon Source

2018 ◽  
Vol 51 (3) ◽  
pp. 867-882 ◽  
Author(s):  
Jan Ilavsky ◽  
Fan Zhang ◽  
Ross N. Andrews ◽  
Ivan Kuzmenko ◽  
Pete R. Jemian ◽  
...  
Keyword(s):  
Small Angle ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Incident Beam ◽  
Evolutionary Development ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Photon Source ◽  
Ray Scattering

Following many years of evolutionary development, first at the National Synchrotron Light Source, Brookhaven National Laboratory, and then at the Advanced Photon Source (APS), Argonne National Laboratory, the APS ultra-small-angle X-ray scattering (USAXS) facility has been transformed by several new developments. These comprise a conversion to higher-order crystal optics and higher X-ray energies as the standard operating mode, rapid fly scan measurements also as a standard operational mode, automated contiguous pinhole small-angle X-ray scattering (SAXS) measurements at intermediate scattering vectors, and associated rapid wide-angle X-ray scattering (WAXS) measurements for X-ray diffraction without disturbing the sample geometry. With each mode using the USAXS incident beam optics upstream of the sample, USAXS/SAXS/WAXS measurements can now be made within 5 min, allowingin situandoperandomeasurement capabilities with great flexibility under a wide range of sample conditions. These developments are described, together with examples of their application to investigate materials phenomena of technological importance. Developments of two novel USAXS applications, USAXS-based X-ray photon correlation spectroscopy and USAXS imaging, are also briefly reviewed.

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