The Advanced Photon Source
a U.S. Department of Energy Office of Science User Facility

Techniques

1-ID techniques leverage the high-brilliance of synchrotron x-rays in the 42<E<120 keV range to non-destructively probe bulk materials. Often the techniques listed below can be combined on a single specimen, to obtain multi-modal data that span a wide range of length scales. These techniques can also be conducted in situ using external stimuli including temperature and mechanical loading.

Panoramic view of 1-ID-E
Schematic view of 1-ID-E

At 1-ID, Wide Angle X-ray Scattering (WAXS) technique employs a transmission geometry and large area detector(s) to measure grain-averaged quantities such as phase fraction, internal strain, dislocation density and crystallographic texture in each phase of a polycrystalline material. Such materials encompass the vast majority of structural materials, ranging from aircraft wings to engine crankshafts to bones and teeth. The high-flux of synchrotron x-rays combined with modern area detectors allows for weak phases to be detected, such as Zr-H phases in Zr alloys with H concentrations on the 100 parts-per-million level, and rapid data collection with less than 1 s/detector frame common. 

At the low Bragg angles associated with these high-energies (2θ(typ) < 15 degrees), the area detector captures diffraction information from a 2D plane of sample orientations which are nearly perpendicular to the incident beam. The incident x-ray beam size can be decreased to approximately 2 (V) x 10 (H) microns using slits and/or focusing elements, allowing gradients transverse to the incident beam to be probed by translating the sample relative to the fixed beam. In the longitudinal direction, diffraction is typically averaged over the entire sample thickness traversed by the x-ray beam; however diffracted beam apertures may be used to produce longitudinal resolutions down to ~100 microns.

By taking diffraction patterns as a function of a rotation, about an axis perpendicular to the incident beam (ω), multi-dimensional quantities may be measured including the orientation distribution function (macro-texture) and full strain tensor. In addition, this rotation provides 3D spatially-resolved WAXS reconstructions via the high-energy diffraction microscopy (HEDM) and scattering tomography (ST) techniques.

Examples

Small Angle X-ray Scattering (SAXS)  is a pinhole-based technique which uses an area detector and ~6m sample-detector distance to determine the distribution of nanoparticle or void sizes as well as periodicity of long-range orders in hierarchical materials. SAXS is often combined with WAXS and the two signals can be captured concurrently using strategically located detectors as illustrated in the panoramic view of the 1-ID-E hutch.

Examples

In the HEDM technique, individual grains within a polycrystalline aggregate can be mapped by taking diffraction patterns as a function of rotation angle. HEDM requires that diffraction spots from individual grains can be identified, meaning that there is an upper limit to the number of grains which can be measured in a given diffraction volume. In non-deformed samples as many as several thousands of grains may be indexed, while this number decreases with crystallite disorder (e.g. plastic deformation). There are 2 flavors of HEDM: near-field and far-field.  In near-field HEDM the detector is placed several mm from the sample and sample-orientation is mapped with high (micron level) spatial resolution.  In far-field HEDM the detector is about 1m from the sample and grain-level quantities are mapped with high q-resolution.  Taken together, these techniques produce maps of crystallographic parameters in the illuminated volume including lattice parameters, orientations, positions and volumes and grain shape. Currently only a few synchrotron facilities are available worldwide which can generate this type of diffraction data. The closest non-x-ray analogue is electron backscatter diffraction, available much more widely, which provides 2D (surface) information with higher spatial resolution but poorer resolution of crystallographic parameters.

Examples

The Scattering Tomography technique is based on collecting position-resolved 'powder-like' WAXS data at a number of angular orientations of the specimen, with positional intervals generally matching the beam-size and number chosen to cover the entire specimen cross-section.Through subsequent reconstruction of this data, the cross-section is partitioned, or voxellated, such that powder diffraction data can be attributed to each voxel.Three-dimensional imaging can be performed by an orthogonal specimen translation and repeating the process. This method is used for 3D volume reconstructions in lieu of HEDM when grain sizes are too small to be individually resolved with HEDM (roughly this limit is in the 1-5 micron range), and thus valuable for studying inhomogeneities in nano-grained materials including bio-materials and many energy-storage materials.

High-energy monochromator characteristics

Available beam sizes

  • Spot sizes delivered by slits
    • ~20 um x ~20 um minimum
    • 2 mm (horizontal) x 1 mm (vertical) maximum

WAXS detector

  • GE amorphous-Si area detector (200 micron x 200 micron; 2048 x 2048 array; integrating detector with 2e14 max counts)
  • Single panel or 4 panel (hydra) arrangement

SAXS detector

  • Pixirad2 CdTe detector (56 micron x 56 micron; 476 x 1024 array; counting detector with 2e15 max counts)

Tomography detector

  • APS in-house built detector (more information available upon request)

NF-HEDM detector

  • APS in-house built detector (more information available upon request)

Detector distances

  • Sample to WAXS (single panel) distance (min / max): ~500 mm / ~3000 mm 
  • Sample to WAXS (hydra configuration) distance (min / max): ~1500 mm / ~4000 mm
  • Sample to tomography detector distance (min / max): ~50 mm / ~140 mm
  • Sample to NF-HEDM detector distance (min / max): ~5 mm / ~13 mm
  • Sample to SAXS detector distance: ~6200 mm
  • Sample to VFF-HEDM detector distance (min / max): ~4200 mm / ~6200 mm

Typical calibration samples used

Techniques Sample size Coverage Spatial resolution Angular / strain resolution  Remarks
SAXS / WAXS several mm; thickness governed by X-ray energy WAXS - d from 20 Angstrom to 1 Angstrom with an area detector placed 1 m away from the sample; sample to detector distance can be changed
SAXS - q from 0.01 A-1 to 0.1 A-1; detector position fixed to 6 m from the sample
20 um resolution with regular slits (X / Y), averaging along Z
1 um resolution with focusing optics (X / Y), averaging along Z
100 um - 200 um resolution along Z with conical slits
0.01o / 1e-4 Conical slits available for polycrystalline materials with cubic crystal symmetry; simultaneous measurement along multiple scattering vectors using monochromatic X-rays and area detector; custom matlab codes for analysis.
Diffraction / scattered beam tomography several mm; thickness governed by X-ray energy; scanning parameters dictates spatial resolution WAXS - d from 20 Angstrom to 1 Angstrom with an area detector placed 1 m away from the sample; sample to detector distance can be changed
SAXS - q from 0.01 A-1 to 0.1 A-1; detector position fixed to 6 m from the sample
~20 um spatial resolution; highly dependent on scanning parameters 0.01o / 1e-4 Custom matlab codes for analysis.
Tomography several mm; thickness governed by X-ray energy 2 mm x 2 mm field of view; absorption or phase contrast tomogrpahy available ~1-2 um spatial resolution - several reconstruction codes available
near field-high energy diffraction microscopy (non-destructive EBSD) 1 mm x 1 mm cross-section recommended; can do larger samples if needed d from 20 Angstrom to 1 Angstrom with an area detector placed ~5 mm away from the sample; obtain grain map in polycrystalline materials ~1-2 um spatial resolution 0.1o / relatively insensitive to strain reconstruction codes include MIDAS and IceNine
far field-high energy diffraction microscopy  1 mm x 1 mm cross-section recommended; can do larger samples if needed d from 20 Angstrom to 1 Angstrom with an area detector placed 1 m away from the sample; sample to detector distance can be changed; obtain grain center of mass, crystallographic orientation, and strain in polycrystalline materials ~10 um spatial resolution 0.01o / 1e-4 reconstruction codes include MIDAS and HEXRD
very far field-high energy diffraction microscopy  1 mm x 1 mm cross-section recommended; can do larger samples if needed high resolution reciprocal space mapping an area detector placed ~5 m away from the sample - ~0.001o Can be used for (currently very limited) coherence measurements.

 The 1-ID mail-in program is available for many experimental techniques supported by the beamline.

  • SAXS and/or WAXS
  • Tomography
  • FF-HEDM
  • NF-HEDM

The samples are typically mounted on a 3D printed wheel that can hold up to 48 samples (SAXS / WAXS) or 20 samples (Tomography / FF-HEDM).

Since NF-HEDM is highly time consuming, the samples are not mounted on a wheel. 

Interested users should contact the MPE staff to make appropriate arrangements.

We also recommend users to contact 11-BM's powder diffraction mail-in program depending on the measurement needs.

Experimental Setup
Sample wheel at 1-ID-E Sample wheel at 1-ID-E
For each sample on the sample wheel, the sample manipulation system can move the sample in X-Y-Z to acquire a 2D or a 3D map. 
Sample wheel geometry

Illustrations of the primary sample wheels used for 1-ID mail-in program are below. While we strongly recommend that these wheel designs are used for mounting mail-in samples to leverage the streamlined measurement procedure, other sample mounting schemes can be devised if absolutely necessary. 

A kinematic mount is attached to the square recess so that the wheel can be replaced easily. 

These wheel can be printed by the APS and shipped to users or the STL file can be provided to print at user's home institution.

Sample wheel for tomography and FF-HEDM

Samples are mounted on the flat faces around the wheel.

Small sample wheel

Sample wheel for SAXS / WAXS

Samples are mounted in the sample slots. They can take various forms - puck to capillaries.

Large sample wheel

Examples

Accurate measurement of lattice parameter in human metacarpals

Multiple human metacarpals extracted from several archaeological sites were measured using SAXS / WAXS to understand the change in bone structure due to burial sites.

Understanding the process-dependent precipitate characteristics in aluminum alloys

The precipitates in model 7000 series aluminum alloys were characterized using SAXS / WAXS to understand the process-dependent precipitate formation.

Understanding the effect of protein mutation on bone matrix composition and property

SAXS / WAXS was used to measure the changes induced by G171V mutation in the low density lipoprotein receptor-related protein 5 (LRP5) in mouse bones.

The APS Upgrade project (APS-U) will be an exciting endeavor that will boost the coherence and brilliance of the x-ray beam by replacing the existing APS storage ring and associated photon delivery infrastructure. To take advantage of the new highly coherent and brilliant beam, 1-ID will also undergo various enhancements so that we can continue to deliver world-class in situ experimental capabilities after APS-U.

One of the new experimental techniques that is anticipated to come on-line is Bragg Coherent Diffraction Imaging (BCDI). The BCDI technique has been demonstrated at lower energy x-rays and utilized to measure the intra-granular structural changes in single, often isolated, particles.

In preparation for APS-U, 1-ID has been collaborating with ANL-Material Science Division's Synchrotron Studies of Materials group (https://www.anl.gov/msd/synchrotron-studies-of-materials) to develop the experimental and analysis infrastructure for BCDI at high-energy x-rays and combining it with HEDM to broaden the length scales that our techniques can cover.

 

02.09.2021