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

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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Ultra-small-angle X-ray scattering at the Advanced Photon Source

Journal of Applied Crystallography ◽

10.1107/s0021889809008802 ◽

2009 ◽

Vol 42 (3) ◽

pp. 469-479 ◽

Cited By ~ 199

Author(s):

Jan Ilavsky ◽

Pete R. Jemian ◽

Andrew J. Allen ◽

Fan Zhang ◽

Lyle E. Levine ◽

...

Keyword(s):

Cross Sections ◽

Small Angle ◽

National Laboratory ◽

Argonne National Laboratory ◽

X Ray ◽

X Ray Scattering ◽

Operational Energy ◽

Scattering Cross Sections ◽

Photon Source ◽

Ray Scattering

The design and operation of a versatile ultra-small-angle X-ray scattering (USAXS) instrument at the Advanced Photon Source (APS) at Argonne National Laboratory are presented. The instrument is optimized for the high brilliance and low emittance of an APS undulator source. It has angular and energy resolutions of the order of 10−4, accurate and repeatable X-ray energy tunability over its operational energy range from 8 to 18 keV, and a dynamic intensity range of 108to 109, depending on the configuration. It further offers quantitative primary calibration of X-ray scattering cross sections, a scattering vector range from 0.0001 to 1 Å−1, and stability and reliability over extended running periods. Its operational configurations include one-dimensional collimated (slit-smeared) USAXS, two-dimensional collimated USAXS and USAXS imaging. A robust data reduction and data analysis package, which was developed in parallel with the instrument, is available and supported at the APS.

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Investigation of microstructural changes in impacted polyurea coatings using small angle X-ray scattering (SAXS)

Powder Diffraction ◽

10.1154/1.3590738 ◽

2011 ◽

Vol 26 (2) ◽

pp. 149-154 ◽

Cited By ~ 3

Author(s):

Edward Balizer ◽

Jeffry Fedderly ◽

Gilbert Lee ◽

Susan Bartyczak ◽

Willis Mock

Keyword(s):

Strain Hardening ◽

Small Angle ◽

High Speed ◽

Soft Segment ◽

National Laboratory ◽

Argonne National Laboratory ◽

Steel Cylinder ◽

X Ray ◽

X Ray Scattering ◽

Ray Scattering

Three polyureas with decreasing soft segment molecular weights of 1000, 650, and a 250/1000 blend were molded onto circular steel plates and then impacted with a high speed (275 m/s) conical-shaped steel cylinder. The polyurea layer of the post mortem bilayers was characterized on a molecular level by small angle synchrotron X-ray scattering (SAXS) at the Advanced Photon Source at the Argonne National Laboratory. Analysis revealed that the hard domains of the polyureas with lower molecular weight soft segments reformed and oriented over a greater area of the coating, thus increasing the polymer strain hardening and resulting in visibly less out of plane bilayer deformation. This agrees with the hypothesis that polymer strain hardening is a mechanism that retards necking failure of the metal plate.

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

Catalysts ◽

10.3390/catal11060730 ◽

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.

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Design and characterization of an undulator beamline optimized for small-angle coherent X-ray scattering at the Advanced Photon Source

Journal of Synchrotron Radiation ◽

10.1107/s0909049599009590 ◽

1999 ◽

Vol 6 (6) ◽

pp. 1174-1184 ◽

Cited By ~ 56

Author(s):

A. R. Sandy ◽

L. B. Lurio ◽

S. G. J. Mochrie ◽

A. Malik ◽

G. B. Stephenson ◽

...

Keyword(s):

Small Angle ◽

X Ray ◽

X Ray Scattering ◽

Photon Source ◽

Ray Scattering

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

Journal of Applied Crystallography ◽

10.1107/s0021889813021900 ◽

2013 ◽

Vol 46 (5) ◽

pp. 1508-1512 ◽

Cited By ~ 11

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.

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Collimating Montel mirror as part of a multi-crystal analyzer system for resonant inelastic X-ray scattering

Journal of Synchrotron Radiation ◽

10.1107/s1600577516007426 ◽

2016 ◽

Vol 23 (4) ◽

pp. 880-886 ◽

Cited By ~ 6

Author(s):

Jungho Kim ◽

Xianbo Shi ◽

Diego Casa ◽

Jun Qian ◽

XianRong Huang ◽

...

Keyword(s):

Energy Resolution ◽

Incident Beam ◽

X Rays ◽

X Ray ◽

X Ray Scattering ◽

Angular Acceptance ◽

Crystal Analyzer ◽

Present Design ◽

Photon Source ◽

Ray Scattering

Advances in resonant inelastic X-ray scattering (RIXS) have come in lockstep with improvements in energy resolution. Currently, the best energy resolution at the IrL3-edge stands at ∼25 meV, which is achieved using a diced Si(844) spherical crystal analyzer. However, spherical analyzers are limited by their intrinsic reflection width. A novel analyzer system using multiple flat crystals provides a promising way to overcome this limitation. For the present design, an energy resolution at or below 10 meV was selected. Recognizing that the angular acceptance of flat crystals is severely limited, a collimating element is essential to achieve the necessary solid-angle acceptance. For this purpose, a laterally graded, parabolic, multilayer Montel mirror was designed for use at the IrL3-absorption edge. It provides an acceptance larger than 10 mrad, collimating the reflected X-ray beam to smaller than 100 µrad, in both vertical and horizontal directions. The performance of this mirror was studied at beamline 27-ID at the Advanced Photon Source. X-rays from a diamond (111) monochromator illuminated a scattering source of diameter 5 µm, generating an incident beam on the mirror with a well determined divergence of 40 mrad. A flat Si(111) crystal after the mirror served as the divergence analyzer. From X-ray measurements, ray-tracing simulations and optical metrology results, it was established that the Montel mirror satisfied the specifications of angular acceptance and collimation quality necessary for a high-resolution RIXS multi-crystal analyzer system.

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Scatterless hybrid metal–single-crystal slit for small-angle X-ray scattering and high-resolution X-ray diffraction

Journal of Applied Crystallography ◽

10.1107/s0021889808031129 ◽

2008 ◽

Vol 41 (6) ◽

pp. 1134-1139 ◽

Cited By ~ 98

Author(s):

Youli Li ◽

Roy Beck ◽

Tuo Huang ◽

Myung Chul Choi ◽

Morito Divinagracia

Keyword(s):

High Resolution ◽

Single Crystal ◽

Small Angle ◽

Incident Beam ◽

Single Crystal Substrate ◽

X Ray Diffraction ◽

Metal Base ◽

X Ray ◽

X Ray Scattering ◽

Ray Scattering

A simple hybrid design has been developed to produce practically scatterless aperture slits for small-angle X-ray scattering and high-resolution X-ray diffraction. The hybrid slit consists of a rectangular single-crystal substrate (e.g.Si or Ge) bonded to a high-density metal base with a large taper angle (> 10°). The beam-defining single-crystal tip is oriented far from any Bragg peak position with respect to the incident beam and hence produces none of the slit scattering commonly associated with conventional metal slits. It has been demonstrated that the incorporation of the scatterless slits leads to a much simplified design in small-angle X-ray scattering instruments employing only one or two apertures, with dramatically increased intensity (a threefold increase observed in the test setup) and improved low-angle resolution.

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Implementation and performance of SIBYLS: a dual endstation small-angle X-ray scattering and macromolecular crystallography beamline at the Advanced Light Source

Journal of Applied Crystallography ◽

10.1107/s0021889812048698 ◽

2013 ◽

Vol 46 (1) ◽

pp. 1-13 ◽

Cited By ~ 126

Author(s):

Scott Classen ◽

Greg L. Hura ◽

James M. Holton ◽

Robert P. Rambo ◽

Ivan Rodic ◽

...

Keyword(s):

Data Collection ◽

Light Source ◽

Small Angle ◽

National Laboratory ◽

Department Of Energy ◽

Macromolecular Crystallography ◽

X Ray ◽

X Ray Scattering ◽

Advanced Light Source ◽

Ray Scattering

The SIBYLS beamline (12.3.1) of the Advanced Light Source at Lawrence Berkeley National Laboratory, supported by the US Department of Energy and the National Institutes of Health, is optimized for both small-angle X-ray scattering (SAXS) and macromolecular crystallography (MX), making it unique among the world's mostly SAXS or MX dedicated beamlines. Since SIBYLS was commissioned, assessments of the limitations and advantages of a combined SAXS and MX beamline have suggested new strategies for integration and optimal data collection methods and have led to additional hardware and software enhancements. Features described include a dual mode monochromator [containing both Si(111) crystals and Mo/B4C multilayer elements], rapid beamline optics conversion between SAXS and MX modes, active beam stabilization, sample-loading robotics, and mail-in and remote data collection. These features allow users to gain valuable insights from both dynamic solution scattering and high-resolution atomic diffraction experiments performed at a single synchrotron beamline. Key practical issues considered for data collection and analysis include radiation damage, structural ensembles, alternative conformers and flexibility. SIBYLS develops and applies efficient combined MX and SAXS methods that deliver high-impact results by providing robust cost-effective routes to connect structures to biology and by performing experiments that aid beamline designs for next generation light sources.

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SWING detection vacuum tunnel

Diamond Light Source Proceedings ◽

10.1017/s2044820111000189 ◽

2011 ◽

Vol 1 (MEDSI-6) ◽

Author(s):

D. Dalle ◽

J. Perez ◽

O. Lyon ◽

P. Feret ◽

C. Menneglier ◽

...

Keyword(s):

Small Angle ◽

Vacuum Chamber ◽

Incident Beam ◽

Angular Range ◽

Scattered Intensity ◽

Long Distance ◽

General Design ◽

X Ray ◽

X Ray Scattering ◽

Ray Scattering

The SWING beamline is dedicated to the study of the small-angle X-ray scattering. In order to have the possibility to detect scattered intensity very close to the incident beam, it is absolutely necessary to install the detector at a long distance from the sample. In addition, it is easy to change the detector's position to access a wider angular range. A long and large vacuum chamber, the ‘tunnel’, has been designed with specific mechanisms inside to control the detector's position with micrometre resolution. Special attention has been given so as to offer a very useful device to the users. The paper will present the general design of the tunnel equipped with ancillary devices such as very narrow and stiff beam stoppers, diode holders and beam attenuators.

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