Development of combined microstructure and structure characterization facility for <i>in situ</i> and <i>operando</i> studies at the Advanced Photon Source

Ilavský, Ján; Zhang, Fan; Andrews, Ross N.; Kuzmenko, Ivan; Jemian, Pete R.; Levine, Lyle E.; Allen, Andrew P.

doi:10.1107/s160057671800643x

Cited by 151 publications

(132 citation statements)

References 63 publications

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“…USAXS data were acquired using the USAXS instrument at the Advanced Photon Source, Argonne National Laboratory. 48 We measured a representative population of pristine RDX crystals and recovered crystals that had been shocked to maximum pressures of 10 GPa, 16 GPa, and 28 GPa. USAXS measures the scattering intensities produced due to differences (contrast) in electron density.…”

Section: Analysis Of Crystals Recovered After Shockmentioning

confidence: 99%

Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX)

et al. 2020

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We demonstrate a strongly thresholded response in cyclotrimethylene trinitramine (RDX) when it is cylindrically shocked using a novel waveguide geometry. Using ultrafast single-shot multi-frame imaging, we demonstrate that <100-μm diameter single crystals of RDX embedded in a polymer host deform along preferential planes for >100 ns after the shock first arrives in the crystal. We use in-situ imaging and time-resolved photoemission to demonstrate that short-lived chemistry is linked to high-energy deformation planes. Using scanning electron microscopy and ultrasmall-angle X-ray scattering, we demonstrate that the shock-induced dynamics leave behind sintered crystals, with pore shapes and sizes that change significantly with shock energy. A threshold pressure of ~ 12 GPa at the center of convergence separated the single-mode planar crystal deformations from the chemistry-coupled multi-plane dynamics at higher pressures. Our observations indicate preferential deformation mechanics in our cylindrically shocked system, despite the applied stress along many different crystallographic planes. AUTHOR INFORMATIONCorresponding Author: Leora E. Dresselhaus-Cooper, dresselhausc1@llnl.gov † Present address: Author ContributionsThe project was directed by KAN. Shock experiments were carried out by LEDC. Samples were prepared by LEDC and DJM. USAXS experiments were performed with LEDC, FZ, JI and DJM. The orientation of the crystal in Fig. 6 was measured by LEDC, CT, SYGW and YSC.Analysis of the results were carried out by LEDC and KAN. The manuscript was written by LEDC, with supporting contributions from all authors.

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Section: Analysis Of Crystals Recovered After Shockmentioning

confidence: 99%

Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX)

et al. 2020

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“…We measured the transmission of the fundamental and harmonic radiations for our scheme using the ultra-small-angle X-ray scattering (USAXS) instrument at APS sector 9-ID (Ilavsky et al ., 2009, 2018). This beamline makes use of an APS undulator A source and a Si(111) double-crystal monochromator.…”

Section: Experimental Verification: Harmonic Transmissionmentioning

confidence: 99%

High-efficiency coherence-preserving harmonic rejection with crystal optics

Zhang

Allen

Levine

et al. 2018

J Synchrotron Radiat

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This work reports a harmonic-rejection scheme based on the combination of Si(111) monochromator and Si(220) harmonic-rejection crystal optics. This approach is of importance to a wide range of X-ray applications in all three major branches of modern X-ray science (scattering, spectroscopy, imaging) based at major facilities, and especially relevant to the capabilities offered by the new diffraction-limited storage rings. It was demonstrated both theoretically and experimentally that, when used with a synchrotron undulator source over a broad range of X-ray energies of interest, the harmonic-rejection crystals transmit the incident harmonic X-rays on the order of 10−6. Considering the flux ratio of fundamental and harmonic X-rays in the incident beam, this scheme achieves a total flux ratio of harmonic radiation to fundamental radiation on the order of 10−10. The spatial coherence of the undulator beam is preserved in the transmitted fundamental radiation while the harmonic radiation is suppressed, making this scheme suitable not only for current third-generation synchrotron sources but also for the new diffraction-limited storage rings where coherence preservation is an even higher priority. Compared with conventional harmonic-rejection mirrors, where coherence is poorly preserved and harmonic rejection is less effective, this scheme has the added advantage of lower cost and footprint. This approach has been successfully utilized at the ultra-small-angle X-ray scattering instrument at the Advanced Photon Source for scattering, imaging and coherent X-ray photon correlation spectroscopy experiments. With minor modification, the harmonic rejection can be improved by a further five orders of magnitude, enabling even more performance capabilities.

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“…In this paper, the evolution of calcium carbonate phases from calcium hydroxide and the corresponding changes in the roughness of the pore-solid interface are investigated using in-operando synchrotron ultrasmall, small, and wide angle X-ray scattering (USAXS/SAXS/WAXS) measurements [6,8,10,11,[28][29][30][31][32]. Wide angle X-ray scattering measurements provide unambiguous insights into the structural changes, while ultrasmall and small angle X-ray scattering measurements reveal the changes in the textures of the pore-solid interface during the carbon mineralization of calcium hydroxide to produce calcium carbonate.…”

Section: Introductionmentioning

confidence: 99%

Phase Evolution and Textural Changes during the Direct Conversion and Storage of CO2 to Produce Calcium Carbonate from Calcium Hydroxide

Liu

Gadikota

2018

Geosciences

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The increasing use of energy resources recovered from subsurface environments and the resulting carbon imbalance in the environment has motivated the need to develop thermodynamically downhill pathways to convert and store CO 2 as water-insoluble calcium or magnesium carbonates. While previous studies extensively explored aqueous routes to produce calcium and magnesium carbonates from CO 2 , there is limited scientific understanding of the phase evolution and textural changes during the direct gas-solid conversion routes to produce calcium carbonate from calcium hydroxide, which is one of the abundant constituents of alkaline industrial residues. With increasing interest in developing integrated pathways for capturing, converting, and storing CO 2 from dilute flue gases, understanding the composition of product phases as they evolve is essential for evaluating the efficacy of a given processing route. Therefore, in this study, we investigate the phase evolution and the corresponding textural changes as calcium hydroxide is converted to calcium carbonate under the continuous flow of CO 2 at an ambient pressure of 1 atm with continuous heating from 30 • C to 500 • C using in-operando wide angle X-ray scattering (WAXS), small angle X-ray scattering (SAXS), and ultrasmall angle X-ray scattering (USAXS) measurements.

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Development of combined microstructure and structure characterization facility for in situ and operando studies at the Advanced Photon Source

Cited by 151 publications

References 63 publications

Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX)

Pressure-Thresholded Response in Cylindrically Shocked Cyclotrimethylene Trinitramine (RDX)

High-efficiency coherence-preserving harmonic rejection with crystal optics

Phase Evolution and Textural Changes during the Direct Conversion and Storage of CO2 to Produce Calcium Carbonate from Calcium Hydroxide

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