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At least 19 records

Direct detection system for full-field nanoscale X-ray diffraction-contrast imaging

Recent developments in X-ray science provide methods to probe deeply embedded mesoscale grain structures and spatially resolve them using dark field X-ray microscopy (DFXM). Extending this technique to investigate weak diffraction signals such as magnetic systems, quantum materials and thin films prove challenging due to available detection methods and incident X-ray flux at the sample. We present a direct detection method developed in conjunction with KAImaging which focuses on DFXM studies in the hard X-ray range of 10s of keV and above capable of approaching nanoscale resolution. Additionally, we compare this direct detection scheme with routinely used scintillator-based optical detection and achieve an order of magnitude improvement in exposure times allowing for imaging of weakly diffracting ordered systems.

47 OTHER INSTRUMENTATION↗

The Evolution of the Deformation Substructure in a Ni-Co-Cr Equiatomic Solid Solution Alloy

The equiatomic NiCoCr alloy exhibits an excellent combination of strength and ductility, even greater than the FeNiCrCoMn high entropy alloy, and also displays a simultaneous increase in strength and ductility with decreasing the testing temperature. To systemically investigate the origin of the exceptional properties of NiCoCr alloy, which are related to the evolution of the deformation substructure with strain, interrupted tensile testing was conducted on the equiatomic NiCoCr single-phase solid solution alloy at both cryogenic and room temperatures at five different plastic strain levels of 1.5%, 6.5%, 29%, 50% and 70%. The evolution of deformation substructure was examined using electron backscatter diffraction (EBSD), transmission Kikuchi diffraction (TKD), conventional transmission electron microscopy (CTEM), diffraction contrast imaging using STEM (DCI-STEM) and atomic resolution scanning transmission electron microscopy. While the deformation substructure mainly consisted of planar dislocation slip and the dissociation of dislocations into stacking faults at small strain levels (≤6.5%), at larger strain levels, additional substructures including nanotwins and a new phase with hexagonal close packed (HCP) lamellae also appeared. The volume fraction of the HCP lamellae increases with increasing deformation, especially at cryogenic temperature. First principles calculations at 0 K indicate that the HCP phase is indeed energetically favorable relative to FCC for this composition. The effects of the nanotwin and HCP lamellar structures on hardening rate and ductility at both cryogenic and room temperature are qualitatively discussed.

Twinning↗

Image contrast of diffraction-limited telescopes for circular incoherent sources of uniform radiance

A simple approximate formula is derived for the background intensity beyond the edge of the image of uniform incoherent circular light source relative to the irradiance near the center of the image. The analysis applies to diffraction-limited telescopes with or without central beam obscuration due to a secondary mirror. Scattering off optical surfaces is neglected. The analysis is expected to be most applicable to spaceborne IR telescopes, for which diffraction can be the major source of off-axis response.

Shackleford, W. L.↗

Semi-Automated, Object-Based Tomography of Dislocation Structures

The characterization of the three-dimensional arrangement of dislocations is important for many analyses in materials science. Dislocation tomography in transmission electron microscopy is conventionally accomplished through intensity-based reconstruction algorithms. Although such methods work successfully, a disadvantage is that they require many images to be collected over a large tilt range. Here, we present an alternative, semi-automated object-based approach that reduces the data collection requirements by drawing on the prior knowledge that dislocations are line objects. Our approach consists of three steps: (1) initial extraction of dislocation line objects from the individual frames, (2) alignment and matching of these objects across the frames in the tilt series, and (3) tomographic reconstruction to determine the full three-dimensional configuration of the dislocations. Drawing on innovations in graph theory, we employ a node-line segment representation for the dislocation lines and a novel arc-length mapping scheme to relate the dislocations to each other across the images in the tilt series. We demonstrate the method for a dataset collected from a dislocation network imaged by diffraction-contrast scanning transmission electron microscopy. Based on these results and a detailed uncertainty analysis for the algorithm, we discuss opportunities for optimizing data collection and further automating the method.

47 OTHER INSTRUMENTATION↗

Diffraction and imaging study of imperfections of crystallized lysozyme with coherent X-rays

Phase-contrast X-ray diffraction imaging and high-angular-resolution diffraction combined with phase-contrast radiographic imaging were employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in the symmetric Laue case. The full-width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal was approximately 16.7 arcsec and imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <1 1 0> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Inclusions of impurities or formations of foreign particles in the central growth region are resolved in the images with high sensitivity to defects. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in X-ray diffraction images. The details of the observed defects and the significant change in the revealed microstructures with drying provide insight into the nature of imperfections, nucleation and growth, and the properties of protein crystals.

Muramidase/chemistry↗

Analyzer-based X-ray phase contrast imaging using the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut crystal

An analyzer-based X-ray phase contrast imaging experiment employing the forward-diffracted o-beam in a few-millimetre-thick Bragg-case asymmetrically cut analyzer crystal has been implemented and tested in a geometry similar to that used in conventional radiography. The high angular stability requirements were overcome using specially designed crystals and a closed-loop feedback intensity system, monitoring the intensity of the diffracted h-beam. Analyzer-based images (ABis) taken at different angular positions on the forward-diffracted o-beam rocking curve show different contrasts, as expected. However, the ABis did not show sharp borders. This was closely investigated by X-ray topography and Δ d / d mapping and was attributed to the stresses caused by the analyzer crystal's own weight in the bulk. Further investigation of the crystal design using finite element analysis coupled with dynamical theory of X-ray diffraction is envisaged.

Honnicke, Marcelo Goncalves (ORCID:000000033276432↗

Ultrafast radiographic imaging and tracking: An overview of instruments, methods, data, and applications

Ultrafast radiographic imaging and tracking (U-RadIT) use state-of-the-art ionizing particle and light sources to experimentally study sub-nanosecond transients or dynamic processes in physics, chemistry, biology, geology, materials science and other fields. These processes are fundamental to modern technologies and applications, such as nuclear fusion energy, advanced manufacturing, communication, and green transportation, which often involve one mole or more atoms and elementary particles, and thus are challenging to compute by using the first principles of quantum physics or other forward models. One of the central problems in U-RadIT is to optimize information yield through, e.g. high-luminosity X-ray and particle sources, efficient imaging and tracking detectors, novel methods to collect data, and large-bandwidth online and offline data processing, regulated by the underlying physics, statistics, and computing power. We review and highlight recent progress in: (a.) Detectors such as high-speed complementary metal-oxide semiconductor (CMOS) cameras, hybrid pixelated array detectors integrated with Timepix4 and other application-specific integrated circuits (ASICs), and digital photon detectors; (b.) U-RadIT modalities such as dynamic phase contrast imaging, dynamic diffractive imaging, and four-dimensional (4D) particle tracking; (c.) U-RadIT data and algorithms such as neural networks and machine learning, and (d.) Applications in ultrafast dynamic material science using XFELs, synchrotrons and laser-driven sources. Hardware-centric approaches to U-RadIT optimization are constrained by detector material properties, low signal-to-noise ratio, high cost and long development cycles of critical hardware components such as ASICs. Interpretation of experimental data, including comparisons with forward models, is frequently hindered by sparse measurements, model and measurement uncertainties, and noise. Alternatively, U-RadIT make increasing use of data science and machine learning algorithms, including experimental implementations of compressed sensing. Machine learning and artificial intelligence approaches, refined by physics and materials information, may also contribute significantly to data interpretation, uncertainty quantification and U-RadIT optimization.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Microstructure-Property Relationships in Epitaxial Cu(In, Ga)Se2 Solar-Cell Absorbers

Epitaxially grown Cu(In,Ga)Se 2 (CIGS) absorber layers were analyzed by various techniques in scanning electron microscopy in order to reveal microstructure-property relationships in these thin films. Owing to their epitaxial nature, these CIGS absorber layers do not contain any grain boundaries, but only anti-phase domains (APDs) and dislocations. By combining electron channeling-contrast imaging, electron backscatter diffraction, and cathodoluminescence (CL), in some cases on identical specimen positions of polished cross-sections of CIGS/Mo/glass stacks, it was possible to correlate the presence and orientations of APDs and dislocations with the lateral distributions of the CL intensity and emission-peak energy. We studied CIGS layers with three different [Ga]/([Ga]+[In]) ratios as well as with and without NaF/KF treatments. Considerable differences between the CIGS layer properties in the microstructure-property relationships were found, depending on the growth parameters. Dislocations in the epitaxial CIGS layers do not tend to exhibit strong CL intensity decreases, which contrasts with the situation in numerous other semiconductor materials.

anti-phase domains↗

Effects of diffraction and static wavefront errors on high-contrast imaging from the Thirty Meter Telescope

High-contrast imaging, particularly direct detection of extrasolar planets, is a major science driver for the next generation of extremely large telescopes such as the segmented Thirty Meter Telescope. This goal requires more than merely diffraction-limited imaging, but also attention to residual scattered light from wavefront errors and diffraction effects at the contrast level of 10-8-10-9. Using a wave-optics simulation of adaptive optics and a diffraction suppression system we investigate diffraction from the segmentation geometry, intersegment gaps, obscuration by the secondary mirror and its supports. We find that the large obscurations pose a greater challenge than the much smaller segment gaps. In addition the impact of wavefront errors from the primary mirror, including segment alignment and figure errors, are analyzed. Segment-to-segment reflectivity variations and residual segment figure error will be the dominant error contributors from the primary mirror. Strategies to mitigate these errors are discussed.

segmented mirrors↗

Phase Sensitive X-Ray Diffraction Imaging Study of Protein Crystals

The study of defects and growth of protein crystals is of importance in providing a fundamental understanding of this important category of systems and the rationale for crystallization of better ordered crystals for structural determination and drug design. Yet, as a result of the extremely weak scattering power of x-rays in protein and other biological macromolecular crystals, the extinction lengths for those crystals are extremely large and, roughly speaking, of the order of millimeters on average compared to the scale of micrometers for most small molecular crystals. This has significant implication for x-ray diffraction and imaging study of protein crystals, and presents an interesting challenge to currently available x-ray analytical techniques. We proposed that coherence-based phase sensitive x-ray diffraction imaging could provide a way to augment defect contrast in x-ray diffraction images of weakly diffracting biological macromolecular crystals. I shall examine the principles and ideas behind this approach and compare it to other available x-ray topography and diffraction methods. I shall then present some recent experimental results in two model protein systems-cubic apofemtin and tetragonal lysozyme crystals to demonstrate the capability of the coherence-based imaging method in mapping point defects, dislocations, and the degree of perfection of biological macromolecular crystals with extreme sensitivity. While further work is under way, it is intended to show that the observed new features have yielded important information on protein crystal perfection and nucleation and growth mechanism otherwise unobtainable.

Hu, Z. W.↗

Multimodal microscopy of extended defects in β-Ga 2 O 3 (010) EFG crystals

Beta-phase gallium oxide (β-Ga 2 O 3 ) has attracted attention in recent years as a potentially low cost, large area substrate and active layer material for high power, high temperature power electronics and sensing devices. However, growth of β-Ga 2 O 3 crystals is complicated by easily activated (100) and (001) cleavage planes, the presence of low angle grain boundaries (LAGBs) and twins, and the potential formation of polycrystalline grains. In this study, β-Ga 2 O 3 crystals were grown by the edge-defined film-fed growth technique with an (010) principal face. Two crystals with apparently randomly formed high angle grain boundaries (HAGBs) were selected and analyzed by electron backscatter diffraction, electron channeling contrast imaging, and cathodoluminescence to investigate the nature of the LAGBs and the source of the HAGB formation. It was discovered that planar LAGBs lying parallel to the (010) plane exist in the region immediately preceding the start of an HAGB. Increased misorientation across the LAGB was observed, approaching the initiation of a new grain. We present multimodal microscopy characterization, correlating misorientation and variation in optoelectronic properties with LAGBs and the associated dislocations.

14 SOLAR ENERGY↗

TPSAS-NF1676L-31770-DND

HREBSD (high resolution electron backscatter diffraction) is a scanning electron microscope based diffraction technique that measures stress, elastic strain and dislocation density in crystalline materials with a spatial resolution on the order of tens of nanometers. This information represents a glut of quantitative data that may be directly incorporated in microscale crystal plasticity models. However, concerns over the accuracy of HREBSD make integration of microscopy data with material models problematic. This presentation addresses a number of issue concerning the accuracy of HREBSD, including pattern center error, cross-correlation error and random noise. Additionally, a computational framework is presented that allows for rapid, non-deterministic calibration of material models. Finally, several tests cases are presented where HREBSD is cross-validated with other diffraction techniques: X-ray diffraction, electron channeling contrast imaging and transmission electron microscopy. The accuracy of HREBSD, when incorporating these new techniques, is sufficient to measure local stress to below 10 MPa and to detect individual dislocations.

Timothy J Ruggles↗

X-Ray Diffraction and Imaging Study of Imperfections of Crystallized Lysozyme with Coherent X-Rays

Phase-sensitive x-ray diffraction imaging and high angular-resolution diffraction combined with phase contrast radiographic imaging are employed to characterize defects and perfection of a uniformly grown tetragonal lysozyme crystal in symmetric Laue case. The fill width at half-maximum (FWHM) of a 4 4 0 rocking curve measured from the original crystal is approximately 16.7 arcseconds, and defects, which include point defects, line defects, and microscopic domains, have been clearly observed in the diffraction images of the crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front, and they have been found to originate mostly at a central growth area and occasionally at outer growth regions. Individual point defects trapped at a crystal nucleus are resolved in the images of high sensitivity to defects. Slow dehydration has led to the broadening of the 4 4 0 rocking curve by a factor of approximately 2.4. A significant change of the defect structure and configuration with drying has been revealed, which suggests the dehydration induced migration and evolution of dislocations and lattice rearrangements to reduce overall strain energy. The sufficient details of the observed defects shed light upon perfection, nucleation and growth, and properties of protein crystals.

Hu, Zheng-Wei↗

Compatibility of a Diffractive Pupil and Coronagraphic Imaging

Detection and characterization of exo-earths require direct-imaging techniques that can deliver contrast ratios of 10(exp 10) at 100 milliarc-seconds or smaller angular separation. At the same time, astrometric data is required to measure planet masses and can help detect planets and constrain their orbital parameters. To minimize costs, a single space mission can be designed using a high efficiency coronograph to perform direct imaging and a diffractive pupil to calibrate wide-field distortions to enable high precision astrometric measurements. This paper reports the testing of a diffractive pupil on the high-contrast test bed at the NASA Ames Research Center to assess the compatibility of using a diffractive pupil with coronographic imaging systems. No diffractive contamination was found within our detectability limit of 2x10(exp -7) contrast outside a region of 12lambda/D and 2.5x10(exp -6) within a region spanning from 2 to 12lambda/D. Morphology of the image features suggests that no contamination exists even beyond the detectability limit specified or at smaller working angles. In the case that diffractive contamination is found beyond these stated levels, active wavefront control would be able to mitigate its intensity to 10(exp -7) or better contrast.

Bendek, Eduardo↗

Dynamical diffraction imaging (topography) with X-ray synchrotron radiation

By contrast to electron microscopy, which yields information on the location of features in small regions of materials, X-ray diffraction imaging can portray minute deviations from perfect crystalline order over larger areas. Synchrotron radiation-based X-ray optics technology uses a highly parallel incident beam to eliminate ambiguities in the interpretation of image details; scattering phenomena previously unobserved are now readily detected. Synchrotron diffraction imaging renders high-resolution, real-time, in situ observations of materials under pertinent environmental conditions possible.

Kuriyama, M.↗

Transmission Electron Microscopy of Single Wall Carbon Nanotube/Polymer Nanocomposites: A First-Principles Study

The physics of HRTEM image formation and electron diffraction of SWCNT in a polymer matrix were investigated theoretically on the basis of the multislice method, and the optics of a FEG Super TWIN Philips CM 200 TEM operated at 80 kV. The effect of nanocomposite thickness on both image contrast and typical electron diffraction reflections of nanofillers were explored. The implications of the results on the experimental applicability to study dispersion, chirality and diameter of nanofillers are discussed.

Sola, Francisco↗

Diffraction and Imaging Study of Imperfections of Protein Crystals with Coherent X-rays

High angular-resolution x-ray diffraction and phase contrast x-ray imaging were combined to study defects and perfection of protein crystals. Imperfections including line defects, inclusions and other microdefects were observed in the diffraction images of a uniformly grown lysozyme crystal. The observed line defects carry distinct dislocation features running approximately along the <110> growth front and have been found to originate mostly in a central growth area and occasionally in outer growth regions. Slow dehydration led to the broadening of a fairly symmetric 4 4 0 rocking curve by a factor of approximately 2.6, which was primarily attributed to the dehydration-induced microscopic effects that are clearly shown in diffraction images. X-ray imaging and diffraction characterization of the quality of apoferritin crystals will also be discussed in the presentation.

Hu, Z. W.↗