Ultrafast X-Ray Diffraction Visualization of B1-B2 Phase Transition in KCl under Shock Compression.

The classical B1(NaCl)↔B2(CsCl) transitions have been considered as a model for general structural phase transformations, and resolving corresponding phase transition mechanisms under high strain rate shock compression is critical to a fundamental understanding of phase transition dynamics. Here, we use subnanosecond synchrotron x-ray diffraction to visualize the lattice response of single-crystal KCl to planar shock compression. Complete B1-B2 orientation relations are revealed for KCl under shock compression along ⟨100⟩_{B1} and ⟨110⟩_{B1}; the orientation relations and transition mechanisms are anisotropic and can be described with the standard and modified Watanabe-Tokonami-Morimoto model, respectively, both involving interlayer sliding and intralayer ion rearrangement. The current study also establishes a paradigm for investigating solid-solid phase transitions under dynamic extremes with ultrafast synchrotron x-ray diffraction.

Capture Deformation Twinning in Mg during Shock Compression with Ultrafast Synchrotron X-Ray Diffraction.

Deformation twinning plays a vital role in accommodating plastic deformation of hexagonal-close-packed (hcp) metals, but its mechanisms are still unsettled under high strain rate shock compression. Here we investigate deformation twinning in shock-compressed Mg as a typical hcp metal with in situ, ultrafast synchrotron x-ray diffraction. Extension twinning occurs upon shock compression along ⟨112[over ¯]0⟩ and ⟨101[over ¯]0⟩, but only upon release for loading along ⟨0001⟩. Such deformation mechanisms are a result of the polarity of deformation twinning, which depends on directionality and relative magnitude of resolved shear stress and may be common for Mg and its alloys in a wide range of strain rates.

Simultaneous, single-pulse, synchrotron x-ray imaging and diffraction under gas gun loading.

We develop a mini gas gun system for simultaneous, single-pulse, x-ray diffraction and imaging under high strain-rate loading at the beamline 32-ID of the Advanced Photon Source. In order to increase the reciprocal space covered by a small-area detector, a conventional target chamber is split into two chambers: a narrowed measurement chamber and a relief chamber. The gas gun impact is synchronized with synchrotron x-ray pulses and high-speed cameras. Depending on a camera's capability, multiframe imaging and diffraction can be achieved. The proof-of-principle experiments are performed on single-crystal sapphire. The diffraction spots and images during impact are analyzed to quantify lattice deformation and fracture; fracture is dominated by splitting cracks followed by wing cracks, and diffraction peaks are broadened likely due to mosaic spread. Our results demonstrate the potential of such multiscale measurements for studying high strain-rate phenomena at dynamic extremes.

Dynamic crystal rotation resolved by high-speed synchrotron X-ray Laue diffraction.

Dynamic compression experiments are performed on single-crystal Si under split Hopkinson pressure bar loading, together with simultaneous high-speed (250-350 ns resolution) synchrotron X-ray Laue diffraction and phase-contrast imaging. A methodology is presented which determines crystal rotation parameters, i.e. instantaneous rotation axes and angles, from two unindexed Laue diffraction spots. Two-dimensional translation is obtained from dynamic imaging by a single camera. High-speed motion of crystals, including translation and rotation, can be tracked in real time via simultaneous imaging and diffraction.

Simultaneous X-ray diffraction and phase-contrast imaging for investigating material deformation mechanisms during high-rate loading.

Using a high-speed camera and an intensified charge-coupled device (ICCD), a simultaneous X-ray imaging and diffraction technique has been developed for studying dynamic material behaviors during high-rate tensile loading. A Kolsky tension bar has been used to pull samples at 1000 s(-1) and 5000 s(-1) strain-rates for super-elastic equiatomic NiTi and 1100-O series aluminium, respectively. By altering the ICCD gating time, temporal resolutions of 100 ps and 3.37 µs have been achieved in capturing the diffraction patterns of interest, thus equating to single-pulse and 22-pulse X-ray exposure. Furthermore, the sample through-thickness deformation process has been simultaneously imaged via phase-contrast imaging. It is also shown that adequate signal-to-noise ratios are achieved for the detected white-beam diffraction patterns, thereby allowing sufficient information to perform quantitative data analysis diffraction via in-house software (WBXRD_GUI). Of current interest is the ability to evaluate crystal d-spacing, texture evolution and material phase transitions, all of which will be established from experiments performed at the aforementioned elevated strain-rates.

Transient x-ray diffraction with simultaneous imaging under high strain-rate loading.

Real time, in situ, multiframe, diffraction, and imaging measurements on bulk samples under high and ultrahigh strain-rate loading are highly desirable for micro- and mesoscale sciences. We present an experimental demonstration of multiframe transient x-ray diffraction (TXD) along with simultaneous imaging under high strain-rate loading at the Advanced Photon Source beamline 32ID. The feasibility study utilizes high strain-rate Hopkinson bar loading on a Mg alloy. The exposure time in TXD is 2-3 µs, and the frame interval is 26.7-62.5 µs. Various dynamic deformation mechanisms are revealed by TXD, including lattice expansion or compression, crystal plasticity, grain or lattice rotation, and likely grain refinement, as well as considerable anisotropy in deformation. Dynamic strain fields are mapped via x-ray digital image correlation, and are consistent with the diffraction measurements and loading histories.

Note: Dynamic strain field mapping with synchrotron X-ray digital image correlation.

We present a dynamic strain field mapping method based on synchrotron X-ray digital image correlation (XDIC). Synchrotron X-ray sources are advantageous for imaging with exceptional spatial and temporal resolutions, and X-ray speckles can be produced either from surface roughness or internal inhomogeneities. Combining speckled X-ray imaging with DIC allows one to map strain fields with high resolutions. Based on experiments on void growth in Al and deformation of a granular material during Kolsky bar/gas gun loading at the Advanced Photon Source beamline 32ID, we demonstrate the feasibility of dynamic XDIC. XDIC is particularly useful for dynamic, in-volume, measurements on opaque materials under high strain-rate, large, deformation.

High speed synchrotron x-ray phase contrast imaging of dynamic material response to split Hopkinson bar loading.

The successful process of amalgamating both the time-resolved imaging capabilities present at the Advanced Photon Source beamline 32ID-B and the proficiency of high-rate loading offered by the split Hopkinson or Kolsky compression/tension bar apparatus is discussed and verification of system effectiveness is expressed via dynamic experiments on various material systems. Single particle sand interaction along with glass cracking during dynamic compression, and fiber-epoxy interfacial failure, ligament-bone debonding, and single-crystal silicon fragmentation due to dynamic tension, were imaged with 0.5 µs temporal resolution and µm-level spatial resolution. Synchrotron x-ray phase contrast imaging of said material systems being loaded with the Kolsky bar apparatus demonstratively depicts the effectiveness of the novel union between these two powerful techniques, thereby allowing for in situ analysis of the interior of the material system during high-rate loading for a variety of applications.

Impact system for ultrafast synchrotron experiments.

The impact system for ultrafast synchrotron experiments, or IMPULSE, is a 12.6-mm bore light-gas gun (<1 km/s projectile velocity) designed specifically for performing dynamic compression experiments using the advanced imaging and X-ray diffraction methods available at synchrotron sources. The gun system, capable of reaching projectile velocities up to 1 km/s, was designed to be portable for quick insertion/removal in the experimental hutch at Sector 32 ID-B of the Advanced Photon Source (Argonne, IL) while allowing the target chamber to rotate for sample alignment with the beam. A key challenge in using the gun system to acquire dynamic data on the nanosecond time scale was synchronization (or bracketing) of the impact event with the incident X-ray pulses (80 ps width). A description of the basic gun system used in previous work is provided along with details of an improved launch initiation system designed to significantly reduce the total system time from launch initiation to impact. Experiments were performed to directly measure the gun system time and to determine the gun performance curve for projectile velocities ranging from 0.3 to 0.9 km/s. All results show an average system time of 21.6 ± 4.5 ms, making it possible to better synchronize the gun system and detectors to the X-ray beam.

Gas gun shock experiments with single-pulse x-ray phase contrast imaging and diffraction at the Advanced Photon Source.

The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for in situ, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal (<100 ps) and spatial (∼2 µm) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.

X-ray-induced water vaporization.

We present quantitative evidence for x-ray-induced water vaporization: water is vaporized at a rate of 5.5 pL/s with the 1-Å-wavelength x-ray irradiation of ~0.1 photons per Å(2); moreover, water vapor is reversibly condensed during pauses in irradiation. This result fundamentally suggests that photoionization induces vaporization. This phenomenon is attributed to surface-tension reduction by ionization and would be universally important in radiological and electrohydrodynamic situations.

Multiple microscopy modalities applied to a sea urchin tooth fragment.

Two synchrotron X-ray microscopy methods, phase-contrast microradiography (the propagation method) and absorption microCT (high-resolution computed tomography or microtomography), and laser-scanning confocal microscopy (visible wavelength) were used to study a fragment of the keel of a tooth of the sea urchin Lytechinus variegatus. Stripes observed in the phase-contrast images of the fragment were also seen in confocal micrographs. MicroCT showed that the stripes were due to two parallel planar arrays of low-absorption channels within the bulk of the keel. In the phase microradiographs, maximum contrast stripes appear when a channel image from one row coincides with a channel image from the second row; otherwise, contrast is minimal. Long channels do not appear to have been observed previously in keels of sea urchin teeth.

Cryogenically cooled bent double-Laue monochromator for high-energy undulator X-rays (50-200 keV).

A liquid-nitrogen-cooled monochromator for high-energy X-rays consisting of two bent Si(111) Laue crystals adjusted to sequential Rowland conditions has been in operation for over two years at the SRI-CAT sector 1 undulator beamline of the Advanced Photon Source (APS). It delivers over ten times more flux than a flat-crystal monochromator does at high energies, without any increase in energy width (DeltaE/E approximately 10(-3)). Cryogenic cooling permits optimal flux, avoiding a sacrifice from the often employed alternative technique of filtration - a technique less effective at sources like the 7 GeV APS, where considerable heat loads can be deposited by high-energy photons, especially at closed undulator gaps. The fixed-offset geometry provides a fully tunable in-line monochromatic beam. In addition to presenting the optics performance, unique crystal design and stable bending mechanism for a cryogenically cooled crystal under high heat load, the bending radii adjustment procedures are described.

Performance limits of indirectly cryogenically cooled silicon monochromators--experimental results at the APS.

The results of high-heat-load tests of indirectly cryogenically cooled silicon monochromators are presented. The measurements show that, provided that the total power absorbed by the crystal is less than approximately 150 W, indirect cryogenically cooled silicon monochromators will perform well, with thermal-induced slope errors of less than 2 arcsec. At the Advanced Photon Source, this corresponds to the undulator closed-gap (11 mm) condition at 100 mA with white-beam slit sizes slightly larger than the full width at half-maximum of the radiation central cones. The dependence of the slope errors on the thermomechanical properties of silicon are discussed and clearly demonstrated.

X-ray interferometry of surfaces with Fresnel mirrors.

With a small double-mirror setup, we used grazing-x-ray interferometry to study nanometric steps. These one-dimensional steps were microfabricated upon the surface of one of the two mirrors; the other mirror provided the reference wave. Two geometries were studied. In the longitudinal case in which the x rays are parallel to the step edges, it is straightforward to determine the step size. In the transverse case, one deals with Fourier holography, and a reconstruction process for a phase object had been demonstrated for the case of a single step.

X-Ray Interferometry at ESRF Using Two Coherent Beams from Fresnel Mirrors.

Using two small flat mirrors under grazing incidence, we have produced interference patterns from partially coherent x-ray beams at the European Synchrotron Radiation Facility. By piezoelectrically orienting one mirror around the horizontal plane, both the vertical and horizontal transverse coherence distances of the radiation have been measured. The experimental setup can be used to characterize the coherence properties along x-ray synchrotron beamlines.