Advanced Photon Source at Argonne National Laboratory   APS USAXS instrument
USAXS instrument at the Advanced Photon Source,
X-ray science division, beamline 9ID-C

Advanced Photon Source

A U.S. Department of Energy, Office of Science,
Office of Basic Energy Sciences national synchrotron x-ray research facility

 
 
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Schedule
Staff web pages:
      Jan Ilavsky, inst. scientist
Documentation

      Glassy Carbon int. stnd.
      Example USAXS data
      Getting beam time
      Instrument Geometries
      USAXS imaging
      Overview
      Posters
      Sample Holders
      Select publications
      User publications
      Shipping Instructions
Live USAXS data
Software by Jan Ilavsky:
      Indra (reduction)
      Irena (analysis)
      Nika (2D data reduction)
      Cromer-Liberman AtFF
      Clementine (kinetic rate analysis)
      other macros
Useful WWW links


APS 9ID USAXS/SAXS/WAXS
Ultra-Small-Angle X-ray Scattering Facility

e-mail: usaxs@aps.anl.gov, instrument scientist: Jan Ilavsky, 630-252-0866, ilavsky@aps.anl.gov and Ivan Kuzmenko, 630-252-0327, kuzmenko@aps.anl.gov

The heart of the Ultra-Small-Angle X-ray Scattering (USAXS) facility located at 9ID beamline, station C, at Argonne National Laboratory is an advanced-design Bonse-Hart camera (USAXS) with integrated fixed length pinhole SAXS (500mm) and WAXS (320mm) cameras.

The USAXS/SAXS/WAXS instrument provides World-unique capabilties:
Standard configuration (Si 220 crystals)
Energy range ..........10 - 24 keV
Q range .................. 0.0001 to 6 [1/A] (max depending on energy used)
Intensity range ........ up to 12 decades (depending on sample)
Q resolution ............ ~ 0.00008 [1/A] in the USAXS range (up to ~0.1 [1/A])
WAXS ...................... d spacing range approximately 6A to 0.8 A, min depending on energy

Per request (with justification) special configuration (Si 440 crystals)
Energy ....................14 - 24 keV
Q range .................. 0.00003 to 6 [1/A] (max depending on energy used)
Intensity range ........ up to 12 decades (depending on sample)
Q resolution ............ ~ 0.00003 [1/A] in the USAXS range (up to ~0.1 [1/A])
WAXS ...................... d spacing range approximately 6A to 0.8 A, min depending on energy
example of data is at the end of this page.

NOTE: 440 special configuration needs to be requested ahead of scheduling since it requires significant setup and alignment time. Keep in mind, that it is by nature of higher Q resolution less sensitive than 220 geometry and therefore not suitable for weakly scattering samples.

Want to see how USAXS operates? 3 min (166Mb) movie with data collection is here: USAXS_operations.mp4

For details and to refer to the use of the USAXS instrument, please use following publication:
Ultra-small-angle X-ray scattering at the Advanced Photon Source. J. Ilavsky, P.R. Jemian, A.J. Allen, F. Zhang, L.E. Levine and G.G. Long. Journal of Applied Crystallography, 2009, 42 (3), p 469-479.
Abstract: 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 108 to 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 A-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.

For more publications see here.

APS highlights from USAXS work: 2013, 2007, 2016(1), 2016(2)

USAXS users awards: Student award 2015, NIST Silver medal 2016,

Large pinhole SAXS camera with 0.6m, 2m, and 4m lengths and energy range 10 - 30 keV is located at beamline 15ID ChemMatCARS.

   
1D USAXS Schematic
USAXS

2-D USAXS & USAXS-XPCS Schematic 2D USAXS

Channel-Cut
collimating channel-cut crystal

Schematics of USAXS instrument. For illustration only, NOT for publications. For latest updated drawing please contact beamline scientist.

 

Schematics of USAXS-SAXS-WAXS

Schematics of the USAXS - SAXS - WAXS instrument with all three geometries. Data are collected sequentially using the three devices. Changover time between detectors is about 30 seconds.

Annealing movie

An in-situ USAXS-SAXS-WAXS study of precipitate dissolution and size evolution in a model gamma-gammaPrime ternary Ni-based alloy (collaboration with Dr. G. Muralidharan, ORNL). A 0.1 mm thick sample was heated from RT to 1100C at 4.5C/min while undergoing repeated USAXS-SAXS-WAXS (24 keV) at 5 minute intervals. Research sponsored by the U.S. Department of Energy, Assistant Secretary for Energy Efficiency and Renewable Energy, Office of Vehicle Technologies, as part of the Propulsion Materials Program.

In situ data collected at 226C over 16 hours using USAXS, SAXS, and WAXS on Al alloy. Courtessy of A. Allen, L. Levine, and F. Zhang, NIST.

USAXS/pinSAXS/WAXS data : In situ data collected at 226°C over about 16 hours represent microstructure evolution of AA2024 aluminum alloy (Allen, Levine, and Zhang, NIST). USAXS data enable quantification of second phase formation (size and volume), WAXS enables phase identification.

SiO2 scattering

Scattering of 1 micron SiO2 spheres in aqueous solution.

High explosives Microstructure change

USAXS/pinSAXS/WAXS in situ data : Data collected by LLNL (Tervor Willey et.al.) on high-explosives. The material is composite of two high-explosives and plastic binder. The WAXS clearly shows phase changes while USAXS/pinSAXS data show microstructure change as function of heating.

 

USAXS spheres


Scattering of 1 micron Polystyrene spheres in solution.

 

 


        

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This page last modified: 2016-11-22 2:22 PM