X-ray Characterization of Materials

National Laboratory: 
Argonne National Laboratory
Characterization Class: 
Microscopy
Description: 

Argonne National Laboratory provides various capabilities for x-ray characterization of materials that includes and array of instrumentation, including:

  • Tomography using 1-ID, 2-BM, or 6-BM beamlines that can be done either with absorption- or phase-contrast imaging by varying the sample-detector distance. Typical volumes measured are 1–3 mm3 with 1–5 µm voxel resolution. The instruments demonstrate sensitivity to inhomogeneities, including voids, cracks, secondary phases, etc.
  • Wide-angle x-ray scattering (WAXS) using 1-ID, 6-ID, 6-BM, or 11-ID beamlines can provide the atomic structure of both crystalline (diffraction) and non-crystalline (pdf) phases to be measured. For each crystalline phase, the strain (from d-spacings), texture (from intensity variation), and size (from d-spacing breadth, if nano-crystalline) can be determined. The high flux of synchrotrons allows sensitivity to dilute phases (e.g., ZrH have been measured with 100 ppm of H in Zr matrix). Beam sizes range from 0.1–300 microns.
  • Combinations/advanced techniques with 1-ID beamline allows for simultaneous small-angle x-ray scattering. (SAXS) (for 1–100-nm-scale sensitivity) with WAXS, single-grain measurements within polycrystalline materials (high-energy diffraction microscopy technique), or tomography plus WAXS.
  • In situ studies can be done with the MTS servo-hydraulic load frame (+-15 kN) that can be combined with furnaces for thermomechanical studies to ~1200°C (1-ID only) or a Linkham furnace to 1500°C (all beamlines). Battery cycling is available on all beamlines. Users often work with staff for customized in situ environments.
Capability Bounds: 

Limits depend on techniques applied and will vary depending on instrument.

Unique Aspects: 

All capabilities rely on using high-energy x-rays (E >40keV), best provided by ANL’s Advanced Photon Source (APS), the premier source in the western hemisphere. These x-rays provide penetration depths similar to neutrons (e.g., at Oak Ridge National Laboratory’s Spallation Neutron Source) but with vastly higher flux and spatial resolution. Their penetration power allows for probing through several mm of material for bulk characterization, as well as through in situ vessels (e.g., glassware for holding molten specimens). Another benefit of high-energy x-ray is they are forward scattered, with Bragg angles (for scattering) typically 10 degrees or less, which affords fast, efficient data collection when combined with area detectors.

Availability: 

APS is a user facility, which requires a separate proposal to obtain access to the facilities. Access is more readily available when working with ANL researchers.

Single Point of Contact: 

Name: Dr. John Hryn
Email: jhryn@anl.gov
Phone: 630-252-5894

Supporting Document(s):