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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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At least 55 records · Page 3

An algorithm for resolving intragranular orientation fields using coupled far-field and near-field high energy $\mathrm{X}$-ray diffraction microscopy

Here, we present a novel algorithm for reconstructing spatial intragranular lattice orientation fields using both far-field and near-field high energy X-ray diffraction microscopy (HEDM) measurements. An established far-field indexing algorithm is modified to include lattice orientation distribution information (grain orientation envelopes) in addition to average grain orientations. The near-field data reduction algorithm utilizes this enriched far-field orientation data as a seed for reconstructing intragranular spatial maps of lattice orientation from the diffraction images. The primary benefit of the new algorithm is a significant decrease in the number of trial calculations that must be performed in the reconstruction process compared to existing methodologies while maintaining scalability. The resulting gains in efficiency facilitate the use of relatively modest computational resources and improve throughput at the point of measurement. We provide two example applications: volumetric orientation field reconstructions for a Ti-Al alloy both before and after the application of 3% uniaxial strain. The results showcase the efficiency of the new method and the ability to resolve subtle changes in microstructure, which are associated with incipient plastic deformation.

36 MATERIALS SCIENCE↗

Polymorphism of garnet solid electrolytes and its implications for grain-level chemo-mechanics

Understanding and mitigating filament formation, short-circuit and solid electrolyte fracture is necessary for advanced all-solid-state batteries. Here, we employ a coupled far-field high-energy diffraction microscopy and tomography approach for assessing the chemo-mechanical behaviour for dense, polycrystalline garnet (Li 7 La 3 Zr 2 O 12 ) solid electrolytes with grain-level resolution. In situ monitoring of grain-level stress responses reveals that the failure mechanism is stochastic and affected by local microstructural heterogeneity. In this work, coupling high-energy X-ray diffraction and far-field high-energy diffraction microscopy measurements reveals the presence of phase heterogeneity that can alter local chemo-mechanics within the bulk solid electrolyte. These local regions are proposed to be regions with the presence of a cubic polymorph of LLZO, potentially arising from local dopant concentration variation. The coupled tomography and FF-HEDM experiments are combined with transport and mechanics modelling to illustrate the degradation of polycrystalline garnet solid electrolytes. The results showcase the pathways for processing high-performing solid-state batteries.

36 MATERIALS SCIENCE↗

Far-field thermal imaging below diffraction limit

Non-uniform self-heating and temperature hotspots are major concerns compromising the performance and reliability of submicron electronic and optoelectronic devices. At deep submicron scales where effects such as contact-related artifacts and diffraction limits accurate measurements of temperature hotspots, non-contact thermal characterization can be extremely valuable. In this work, we use a Bayesian optimization framework with generalized Gaussian Markov random field (GGMRF) prior model to obtain accurate full-field temperature distribution of self-heated metal interconnects from their thermoreflectance thermal images (TRI) with spatial resolution 2.5 times below Rayleigh limit for 530nm illumination. Finite element simulations along with TRI experimental data were used to characterize the point spread function of the optical imaging system. In addition, unlike iterative reconstruction algorithms that use ad hoc regularization parameters in their prior models to obtain the best quality image, we used numerical experiments and finite element modeling to estimate the regularization parameter for solving a real experimental inverse problem.

42 ENGINEERING↗

Influences of granular constraints and surface effects on the heterogeneity of elastic, superelastic, and plastic responses of polycrystalline shape memory alloys

Deformation heterogeneities at the microstructural length-scale developed in polycrystalline shape memory alloys (SMAs) during superelastic loading are studied using both experiments and simulations. In situ X-ray diffraction, specifically the far-field high energy diffraction microscopy (ff-HEDM) technique, was used to non-destructively measure the grain-averaged statistics of position, crystal orientation, elastic strain tensor, and volume for hundreds of austenite grains in a superelastically loaded nickel-titanium (NiTi) SMA. These experimental data were also used to create a synthetic microstructure within a finite element model. The development of intragranular stresses were then simulated during tensile loading of the model using anisotropic elasticity. Driving forces for phase transformation and slip were calculated from these stresses. The grain-average responses of individual austenite crystals examined before and after multiple stress-induced transformation events showed that grains in the specimen interior carry more axial stress than the surface grains as the superelastic response "shakes down". Examination of the heterogeneity within individual grains showed that regions near grain boundaries exhibit larger stress variation compared to the grain interiors. As a result, this intragranular heterogeneity is more strongly driven by the constraints of neighboring grains than the initial stress state and orientation of the individual grains.

36 MATERIALS SCIENCE↗

X-ray ptychography on low-dimensional hard-condensed matter materials

Tailoring structural, chemical, and electronic (dis-)order in heterogeneous media is one of the transformative opportunities to enable new functionalities and sciences in energy and quantum materials. This endeavor requires elemental, chemical, and magnetic sensitivities at the nano/atomic scale in two- and three-dimensional space. Soft X-ray radiation and hard X-ray radiation provided by synchrotron facilities have emerged as standard characterization probes owing to their inherent element-specificity and high intensity. One of the most promising methods in view of sensitivity and spatial resolution is coherent diffraction imaging, namely, X-ray ptychography, which is envisioned to take on the dominance of electron imaging techniques offering with atomic resolution in the age of diffraction limited light sources. In this review, we discuss the current research examples of far-field diffraction-based X-ray ptychography on two-dimensional and three-dimensional semiconductors, ferroelectrics, and ferromagnets and their blooming future as a mainstream tool for materials sciences.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Unstable resonator antenna properties in coherent lidar applications - A comparative study

The antenna parameters of a coherent lidar in the far-field diffraction-limited regime, where the lidar transmitter consists of an unstable resonator with a Gaussian reflectivity profile output coupler, are investigated. A figure-of-merit combining lasr transmitter energy extraction efficiency with the far-field attributes of a given cavity configuration has been used to compare the lidar performance and relative merits of such systems as they relate to those of conventional unstable cavities with diffractive output coupling.

Tratt, David M.↗

Focal construct geometry for high intensity energy dispersive x-ray diffraction based on x-ray capillary optics

We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diffraction by fractally serrated apertures

An investigation of light diffracted by irregularly serrated apertures yields a closed-form analytical solution that confirms experimental recording of the diffracted patterns. These serrated apertures are modeled by a fractal function. Examples are given for both sinusoidal and fractal aperture perimeters with varying fractal dimension. Relations between the far-zone diffracted fields and the fractal dimension are examined.

Kim, Y.↗

Near, far, wherever you are: simulations on the dose efficiency of holographic and ptychographic coherent imaging

Different studies in X-ray microscopy have arrived at conflicting conclusions about the dose efficiency of imaging modes involving the recording of intensity distributions in the near (Fresnel regime) or far (Fraunhofer regime) field downstream of a specimen. A numerical study is presented on the dose efficiency of near-field holography, near-field ptychography and far-field ptychography, where ptychography involves multiple overlapping finite-sized illumination positions. Unlike what has been reported for coherent diffraction imaging, which involves recording a single far-field diffraction pattern, it is found that all three methods offer similar image quality when using the same fluence on the specimen, with far-field ptychography offering slightly better spatial resolution and a lower mean error. These results support the concept that (if the experiment and image reconstruction are done properly) the sample can be near or far; wherever you are, photon fluence on the specimen sets one limit to spatial resolution.

42 ENGINEERING↗

Super-resolution model for overlapping peak detection and improved spatial resolution in high-energy diffraction microscopy

Reconstruction quality in Far-field High-Energy Diffraction Microscopy (FF-HEDM) is limited by the spatial resolution of area detectors and the frequent occurrence of overlapping diffraction spots. To address these challenges, we developed a super-resolution (SR) framework using convolutional neural networks (CNNs) to recreate 2D diffraction peaks at up to ×8 resolution from raw detector data. A specialized simulation tool was created to generate synthetic training datasets with varying degrees of peak overlap. Integrated into the Microstructural Imaging using Diffraction Analysis Software (MIDAS), the SR model improves the spatial accuracy and precision of 3D grain reconstruction by an order of magnitude. This approach provides a robust solution for investigation of complex micromechanical states and material classes where the analysis is limited by the presence of overlapping peaks. Furthermore, the methodology developed here can potentially be extended to other techniques that require sub-pixel accuracy for high-fidelity data analysis.

High-energy diffraction microscopy↗

Dihedral corner reflector backscatter using higher order reflections and diffractions

The uniform theory of diffraction (UTD) plus an imposed edge diffraction extension is used to predict the backscatter cross sections of dihedral corner reflectors which have right, obtuse, and acute included angles. The UTD allows individual backscattering mechanisms of the dihedral corner reflectors to be identified and provides good agreement with experimental cross-section measurements in the azimuthal plane. Multiply reflected and diffracted fields of up to third-order are included in the analysis for both horizontal and vertical polarizations. The coefficients of the uniform theory of diffraction revert to those of the geometrical theory of diffraction (GTD) in far-field cross-section analyses, but finite cross sections can be obtained everywhere by considering mutual cancellation of diffractions from parallel edges. Analytic calculations are performed using UTD coefficients; hence the accuracy required in angular measurements is more critical as the distance increases. The common far-field approximation that all rays to the observation point are parallel is too gross an approxiation for the angular parameters in the UTD coefficients in the far field.

Griesser, Timothy↗

A Planar Biaxial Experiment Platform for In Situ High-Energy Diffraction Studies

In this work, an experimental platform for multiscale studies of materials subjected to plane stress loads is presented. Specifically, a planar biaxial mechanical load frame with four independent hydraulic actuators capable of applying arbitrary loading paths and ratios of tension and compression was designed and built for in situ diffraction experimentation. The load frame is integrated for use at the Argonne National Laboratory Advanced Photon Source (APS) synchrotron, Sector 1, 1-ID-E endstation and the Los Alamos Neutron Science Center (LANSCE) spallation neutron source, Spectrometer for Materials Research at Temperature and Stress (SMARTS) instrument. Cruciform specimen geometries were designed to experience loading ratios in the gauges commensurate with those applied at the grips, and to minimize interference with diffracted X-rays and neutrons. The finite element models used to design the cruciform specimen geometries were experimentally validated using stereo digital image correlation measurements. This complete planar biaxial in situ diffraction platform provides a new capability for studying multiaxial micromechanics of crystalline materials (e.g., elastic, slip, twinning, phase transformation) and their dependencies on grain size, location, texture, and neighborhood characteristics. The coupling with far-field high energy diffraction microscopy (ff-HEDM) for grain-by-grain measurements provides an additional benefit; provided crystal elastic constants of a material are known, it enables the direct measurement of local and average stress tensors in the gauge sections of cruciform specimens, resolving a long outstanding challenge of planar biaxial mechanical testing.

36 MATERIALS SCIENCE↗

Intermittent plasticity in individual grains: A study using high energy x-ray diffraction

Abstract Long-standing evidence suggests that plasticity in metals may proceed in an intermittent fashion. While the documentation of intermittency in plastically deforming materials has been achieved in several experimental settings, efforts to draw connections from dislocation motion and structure development to stress relaxation have been limited, especially in the bulk of deforming polycrystals. This work uses high energy x-ray diffraction measurements to build these links by characterizing plastic deformation events inside individual deforming grains in both the titanium alloy, Ti-7Al, and the magnesium alloy, AZ31. This analysis is performed by combining macroscopic stress relaxation data, complete grain stress states found using far-field high energy diffraction microscopy, and rapid x-ray diffraction spot measurements made using a Mixed-Mode Pixel Array Detector. Changes in the dislocation content within the deforming grains are monitored using the evolution of the full 3-D shapes of the diffraction spot intensity distributions in reciprocal space. The results for the Ti-7Al alloy show the presence of large stress fluctuations in contrast to AZ31, which shows a lesser degree of intermittent plastic flow.

36 MATERIALS SCIENCE↗

Infrared Astronomical Satellite (IRAS) analysis, appendix B

Analytical results derived during the development of the PADE program are presented. Near field on-axis diffraction from a circular aperture is analyzed by integrating Kirchhoff's formula, the boundary wave formulation, and the Rayleigh-Sommerfeld theory. Far field on-axis diffraction from obliquely illuminated apertures is described using the angular spectrum approach. Transmission functions and diffracted fields for rectangular, circular, and rotated square apertures are presented.

Source record↗

3D In-situ Stop Action Study of Recrystallization in Additively Manufactured 316L Stainless Steel: Reconstruction Optimization and Observations

A volume of an additively manufactured 316L stainless steel sample has been tracked during its recrystallization using near-and far-field High Energy Diffraction Microscopy (HEDM) and absorption tomography at Advanced Photon Source beamline 1-ID. A nearfield compatible in situ furnace allows monitoring of Bragg diffraction signals as they evolve out of a weak and diffuse background while the sample temperature is approximate to 1250 degrees C. The sample is rapidly cooled to room temperature after observation of significant signal evolution and ti similar to 0.035 mm(3) is mapped by the near-field method. Four cycles of heat treatment follow the structure from a state of small, isolated grains through impingement of domains to near completion of recyrstallization. Here, the experiment and reconstructions are described, and recrystallized fractions, twin domains, and distributions of grain boundary types are discussed.

Liu, He↗