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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Three-dimensional grain mapping of open-cell metallic foam by integrating synthetic data with experimental data from high-energy X-ray diffraction microscopy
Highlights: • High-energy X-ray measurements are made for ligaments of an open-cell aluminum foam. • Grain centroids and orientations are measured using high-energy X-ray diffraction. • 3D grain map is virtually reconstructed by integrating measured and synthetic data. - Abstract: The complex mechanical response of open-cell foams depends strongly on the hierarchy of length scales inherent in them, from engineering-part scale to the ligament scale through the grain scale down to the crystal-lattice scale. A first step toward understanding and predicting the coordinated mechanical response across length scales requires characterizing the open-cell foam structure in three dimensions at relevant scales. Here, we present an initial attempt to digitally represent a physically-realized aluminum alloy foam in terms of both its geometry/topology as well as its underlying crystallographic orientations by integrating several advanced techniques. Specifically, we use a combination of X-ray computed tomography and X-ray diffraction microscopy in conjunction with synthetic grain mapping. Experimental investigation of the foam shows relatively large grain sizes with respect to the ligament length scale, implying that competing mechanics at different length scales (i.e. grain scale vs. ligament scale) will need to be fully incorporated to understand the mechanical behavior of the foam. The integration of non-destructive measurement techniques with synthetic-data generation provides a path toward realistic modeling of bulk samples of open-cell metal foam resolved at the scale of individual grains.
Collaborative development of diffraction-limited beamline optical systems at US DOE light sources
An ongoing collaboration among four US Department of Energy National Laboratories has demonstrated key technology prototypes and software modeling tools required for new high-coherent flux beamline optical systems. New free electron laser (FEL) and diffraction-limited storage ring (DLSR) light sources demand wavefront preservation from source to sample to achieve and maintain optimal performance. Fine wavefront control was achieved using a novel, roomtemperature cooled mirror system called REAL (resistive element adjustable length) that combines cooling with applied, spatially variable auxiliary heating. Single-grating shearing interferometry (also called Talbot interferometry) and Hartmann wavefront sensors were developed and used for optical characterization and alignment on several beamlines, across a range of photon energies. Demonstrations of non-invasive hard x-ray wavefront sensing were performed using a thin diamond single-crystal as a beamsplitter.
(De)lithiation of spinel ferrites Fe3O4, MgFe2O4, and ZnFe2O4: a combined spectroscopic, diffraction and theory study
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Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal.
Abstract not provided.
Resolving indexing ambiguities in X-ray free-electron laser diffraction patterns
Abstract not provided
Confining system integrity assessment by detection of natural gas migration using seismic diffractions [Seismic diffractions for gas leakage detection in the shallow waters of the Gulf of Mexico]
Successful carbon capture and storage (CCS) requires secure CO 2 confinement within a geologic reservoir. If associated with a depleted hydrocarbon reservoir, the sealing capability can be determined by examination of the shallow subsurface for hydrocarbon leaks. Numerous seismic signatures have been reported to be hydrocarbon indicators. The interpretation can be advanced by using seismic diffractions, which could indicate subtle hydrocarbon accumulations not detectable by conventional techniques. In this work, we investigate the potential of seismic diffractions for use in shallow gas detection. We extract diffractions from the ultra-high-resolution 3D P-Cable seismic dataset acquired along the Gulf of Mexico inner continental shelf. Interpretation of this dataset revealed numerous seismic signatures associated with hydrocarbon accumulations (e.g., a prominent gas chimney). We analyze scattering features of the detected hydrocarbon accumulations and confirm the correlation between confidently interpreted gas accumulations and seismic diffractions. Based on that, we suggest using diffractions for confining system integrity assessment. As a result, diffraction analysis allows operating with subtle seismic signals that facilitates exploration of reliable CO 2 storage sites.
Three-dimensional optical trapping and orientation of microparticles for coherent X-ray diffraction imaging
Optical trapping has been implemented in many areas of physics and biology as a noncontact sample manipulation technique to study the structure and dynamics of nano-andmesoscale objects. It provides a unique approach for manipulating microscopic objects without inducing undesired changes in structure. Combining optical trapping with hard X-ray microscopy techniques, such as coherent diffraction imaging and crystallography, provides a nonperturbing environment where electronic and structural dynamics of an individual particle in solution can be followed in situ. It was previously shown that optical trapping allows the manipulation of micrometer-sized objects for Xray fluorescence imaging. However, questions remain over the ability of optical trapping to position objects for X-ray diffraction measurements, which have stringent requirements for angular stability. Our work demonstrates that dynamic holographic optical tweezers are capable of manipulating single micrometer-scale anisotropic particles in a microfluidic environment with the precision and stability required for X-ray Bragg diffraction experiments-thus functioning as an "optical goniometer." The methodology can be extended to a variety of X-ray experiments and the Bragg coherent diffractive imaging of individual particles in solution, as demonstrated here, will be markedly enhanced with the advent of brighter, coherent X-ray sources.
Deep-Learning Electron Diffractive Imaging
Here, we report the development of deep-learning coherent electron diffractive imaging at subangstrom resolution using convolutional neural networks (CNNs) trained with only simulated data. We experimentally demonstrate this method by applying the trained CNNs to recover the phase images from electron diffraction patterns of twisted hexagonal boron nitride, monolayer graphene, and a gold nanoparticle with comparable quality to those reconstructed by a conventional ptychographic algorithm. Fourier ring correlation between the CNN and ptychographic images indicates the achievement of a resolution in the range of 0.70 and 0.55 Å. We further develop CNNs to recover the probe function from the experimental data. The ability to replace iterative algorithms with CNNs and perform real-time atomic imaging from coherent diffraction patterns is expected to find applications in the physical and biological sciences.
Takagi–Taupin dynamical X-ray diffraction simulations of asymmetric X-ray diffraction from crystals: the effects of surface undulations
Dynamical X-ray diffraction simulations from crystals with surface undulations are reported. The Takagi–Taupin equations are applied and used to derive results in good agreement with experimental data reported in a separate paper [Macrander, Pereira, Huang, Kasman, Qian, Wojcik & Assoufid (2020). J. Appl. Cryst. 53, 789–792]. The development of Uragami [J. Phys. Soc. Jpn, (1969), 27, 147–154] is followed. Although previous work by Olekhnovich & Olekhnovich [Acta. Cryst. (1980), A36, 22–27] treated a crystal in the shape of a round cylinder, there do not seem to be any reports of previous dynamical X-ray diffraction treatments specifically for surface undulations. The significance of the present work is that it bridges the diffraction treatment of more classical dynamical diffraction theory, which assumes a flat surface, and the simple kinematic diffraction theory. Finally, the kinematic theory has, to date, been the primary means of simulating X-ray diffraction from surfaces.
Energy dispersive X-ray diffraction (EDXRD) for operando materials characterization within batteries
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Microgravity crystallization of perdeuterated tryptophan synthase for neutron diffraction
Abstract Biologically active vitamin B 6 -derivative pyridoxal 5′-phosphate (PLP) is an essential cofactor in amino acid metabolic pathways. PLP-dependent enzymes catalyze a multitude of chemical reactions but, how reaction diversity of PLP-dependent enzymes is achieved is still not well understood. Such comprehension requires atomic-level structural studies of PLP-dependent enzymes. Neutron diffraction affords the ability to directly observe hydrogen positions and therefore assign protonation states to the PLP cofactor and key active site residues. The low fluxes of neutron beamlines require large crystals (≥0.5 mm 3 ). Tryptophan synthase (TS), a Fold Type II PLP-dependent enzyme, crystallizes in unit gravity with inclusions and high mosaicity, resulting in poor diffraction. Microgravity offers the opportunity to grow large, well-ordered crystals by reducing gravity-driven convection currents that impede crystal growth. We developed the Toledo Crystallization Box (TCB), a membrane-barrier capillary-dialysis device, to grow neutron diffraction-quality crystals of perdeuterated TS in microgravity. Here, we present the design of the TCB and its implementation on Center for Advancement of Science in Space (CASIS) supported International Space Station (ISS) Missions Protein Crystal Growth (PCG)-8 and PCG-15. The TCB demonstrated the ability to improve X-ray diffraction and mosaicity on PCG-8. In comparison to ground control crystals of the same size, microgravity-grown crystals from PCG-15 produced higher quality neutron diffraction data. Neutron diffraction data to a resolution of 2.1 Å has been collected using microgravity-grown perdeuterated TS crystals from PCG-15.
Implications of gnomonic distortion on electron backscatter diffraction and transmission Kikuchi diffraction
The effect of gnomonic distortion on orientation indexing of electron backscatter diffraction patterns is explored through simulation of electron diffraction patterns for sample-to-detector geometries associated with transmission Kikuchi diffraction (TKD) and electron backscatter diffraction (EBSD). Simulated data were analysed by computing a similarity index for both Hough transformed data and simulated patterns to determine the sensitivity of each method for detecting subtle differences in the effect of gnomonic distortions on electron diffraction patterns. These results indicate that the increased gnomonic distortions in electron diffraction patterns for a TKD geometry enhance the sensitivity for detecting subtle differences in interband angles. Additionally, the utilisation of a Hough transform-based indexing approach further enhances the sensitivity.
Dynamic diffraction artefacts in Bragg coherent diffractive imaging
This article reports a theoretical study on the reconstruction artefacts in Bragg coherent diffractive imaging caused by dynamical diffraction effects. It is shown that, unlike the absorption and refraction effects that can be corrected after reconstruction, dynamical diffraction effects have profound impacts on both the amplitude and the phase of the reconstructed complex object, causing strong artefacts. At the dynamical diffraction limit, the reconstructed shape is no longer correct, as a result of the strong extinction effect. Simulations for hemispherical particles of different sizes show the type, magnitude and extent of the dynamical diffraction artefacts, as well as the conditions under which they are negligible.
X-ray back-diffraction: can we further increase the energy resolution by tuning the energy slightly below that of exact backscattering?
X-ray beams at energies tuned slightly below that of exact backscattering (extreme conditions, where X-ray back-diffraction is almost extinguished - called residual XBD) are better focused if the experiment is carried out at lower energies in order to avoid multiple-beam diffraction effects. Following previous work by the authors [Honnicke, Conley, Cusatis, Kakuno, Zhou, Bouet, Marques & Vicentin (2014). J. Appl. Cryst.47, 1658-1665], herein efforts are directed towards characterizing the residual XBD beam of an ultra-thin Si 220 crystal (UTSiXTAL) at similar to 3.2 keV. To achieve the residual XBD condition the UTSiXTAL was cooled from 310 to 273 K. The results indicate that under this extreme condition the energy resolution can be further improved. Issues with the energy resolution measurements due to incoming beam divergence and the ultra-thin crystal flatness are discussed.
Extending the limits of powder diffraction analysis: diffraction parameter space, occupancy defects, and atomic form factors
Although the determination of site occupancies is often a major goal in Rietveld refinement studies, the accurate refinement of site occupancies is exceptionally challenging due to the many correlations and systematic errors that have a hidden impact on the final refined occupancy parameters. Through the comparison of results independently obtained from neutron and synchrotron powder diffraction, improved approaches capable of detecting occupancy defects with an exceptional sensitivity of 0.1% (absolute) in the class of layered NMC Li-ion battery cathode materials have been developed. A new method of visualizing the diffraction parameter space associated with crystallographic site scattering power through the use of f* diagrams is described and this method is broadly applicable to ternary compounds. The f* diagrams allow the global minimum fit to be easily identified and also permit a robust determination of the number and type of occupancy defects within a structure. Through a comparison of neutron and X-ray diffraction results, a systematic error in the synchrotron results was identified using f* diagrams for a series of NMC compounds. Using neutron diffraction data as a reference, this error was shown to specifically result from problems associated with the neutral oxygen X-ray atomic form factor and could be eliminated by using the ionic O 2- form factor for this anion while retaining the neutral form factors for cationic species. The f* diagram method offers a new opportunity to experimentally assess the quality of atomic form factors through powder diffraction studies on chemically related multi-component compounds.
Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction
In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residual strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. Furthe, we found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.
Refinements for Bragg coherent X-ray diffraction imaging: electron backscatter diffraction alignment and strain field computation
Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe–Ni and Co–Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe–Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI samples and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.