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At least 397 records · Page 22

Digital autofocusing of a coded-aperture Laue diffraction microscope

To provide optimal depth resolution with a coded-aperture Laue diffraction microscope, an accurate position of the coded-aperture and its scanning geometry need to be known. However, finding the geometry by trial and error is a time-consuming and often challenging process because of the large number of parameters involved. In this paper, we propose an optimization approach to automate the focusing process after data is collected. Here we demonstrate the robustness and efficiency of the proposed approach with experimental data taken at a synchrotron facility.

47 OTHER INSTRUMENTATION↗

Spatially resolved X-ray imaging and molecular characterisation of sulfur and iron in organic- and sulfur-rich hydrocarbon source mudstones

Sulfurisation of organic matter (OM) is a prominent preservation mechanism, however iron sulfide precipitation, particularly pyrite (FeS2), can counteract this mechanism. There is a dearth of high-resolution, spatially-resolved spectroscopic (redox) information on sulfur and iron inventories within organic-rich rocks that would improve our understanding of prevailing environmental conditions during deposition. Here, state-of-the-art synchrotron-based X-ray absorption and fluorescence analyses of key organic- and sulfur-rich mudstones demonstrate the potential of these techniques to non-destructively map and produce detailed spectroscopic information. Detailed high-resolution analyses (μm- to mm-scale) reveal the presence of widespread sulfurised OM in the Blackstone Band of the Kimmeridge Clay Formation, in line with a persistence of euxinia over a long temporal span and low reactive iron input, facilitating the preservation of OM through sulfurisation. In contrast, the presence of sulfurised OM was transitional in the Monterey Formation, consistent with fluctuating water column redox conditions, and is less significant in the Whitby Mudstone Formation, likely due to the high reactive iron concentrations outcompeting sulfurised OM formation. Analyses of sulfur species using model compounds further indicate that the Whitby Formation is strongly enriched in inorganic reduced sulfur minerals, while both the Kimmeridge Clay and Monterey Formations are dominated by organic sulfur species. These synchrotron-based observations improve our understanding of environmental conditions during the time of deposition of these mudstones and thus show great promise in the study of organic-rich sediments, especially in allowing their depositional settings to be more accurately reconstructed.

Kimmeridge Clay Formation↗

Kinetics and evolution of solid-state metal dealloying in thin films with multimodal analysis

Thin-film solid-state metal dealloying (thin-film SSMD) is an emerging technique that uses self-organization to design nanostructured thin films. The resulting 3D bicontinuous nanostructures are promising for a wide range of applications, such as catalysis and energy storage. In this work, we prepared thin films by SSMD using Ti-Cu as the parent alloy and Mg as the solvent. Using a multimodal approach, we combined synchrotron X-ray spectroscopy, diffraction, and high-resolution electron-based spectroscopy and imaging to study their morphological, structural, and chemical evolution. The processing-structure relationship was analyzed as a function of parent alloy composition and dealloying temperature and time. Morphological transitions from globular, to lamellar, to bicontinuous structures, in conjunction with a ligament size evolution, were identified as functions of the parent alloy composition. The dealloying rate increased with increasing concentration of interdiffusing elements (dissolving component) in the parent alloy. The parting limit, a dealloying compositional threshold, was systematically analyzed and determined to be 30%–40%. The order of crystalline phase formation is CuMg 2 , Cu 2 Mg, and Ti; the Ti phase first shows self-reorganization during dealloying, separate from the crystallization process. The coarsening in thin-film SSMD was identified and not entirely self-similar; in addition to the increase of ligament size over time, the formation of larger globular ligaments were also observed. This work furthers our fundamental understanding of thin-film SSMD and nanostructured thin-film design, where the thermodynamic and kinetic effects differ from the bulk counterparts. The fact that dealloying and diffusion outpaces the crystallization and new phase formation also offers opportunities to utilize thin-film SSMD in certain alloy systems in which deleterious intermetallic phases need to be suppressed, that may not be possible in the bulk geometry.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Seeing is believing: visualization of antiferromagnetic domains

Abstract Understanding and utilizing novel antiferromagnetic (AFM) materials has been recently one of the central issues in condensed matter physics, as well as in materials science and engineering. The relevant contemporary topics include multiferroicity, topological magnetism and AFM spintronics. The ability to image magnetic domains in AFM materials is of key importance for the success of these exciting fields. While imaging techniques of magnetic domains on the surfaces of ferro-(ferri)magnetic materials with, for example, magneto-optical Kerr microscopy and magnetic force microscopy have been available for a number of decades, AFM domain imaging is a relatively new development. We review various experimental techniques utilizing scanning, optical, and synchrotron X-ray probes to visualize AFM domains and domain walls, and to unveil their physical properties. We also discuss the existing challenges and opportunities in these techniques, especially with further increase of spatial and temporal resolution.

36 MATERIALS SCIENCE↗

Fragmentation dynamics of CS 2 dications and trications following S 2p ionization

Here, we present the results from a detailed study of the fragmentation dynamics of CS$_2^{2+}$ and CS$_2^{3+}$, formed in intense femtosecond soft x-ray pulses above the sulfur 2p edge, primarily through single core photoionization from the S 2p site, and subsequent Auger–Meitner decay(s). By combining three-dimensional velocity map imaging with covariance analysis, we determine the relative momenta of the ions produced in each two- and three-body fragmentation channel, at significantly higher ion count rates than conventional coincidence measurements. We shed new light on the wide range of fragmentation channels observed from the CS 2 dication and trication, including channels that involve ionization-induced bond formation and fragmentations producing undetected neutral cofragments. In the latter case, a “native frames” approach is used to isolate contributions from concerted and sequential fragmentations and extract dynamical information about each step of a concerted fragmentation process. While dications often fragment sequentially, the trication is dominated by concerted fragmentation. The main trication fragmentation channel into S + + C + + S + can be well-approximated by classical Coulombic simulations of the ground-state geometry distribution, reflecting both the nature of the trication potential energy surface and the rapid multiple ionization prior to substantial structural dynamics. This study demonstrates ways in which fundamental insights into the fragmentation dynamics of polycations following x-ray ionization may be extracted, which will be beneficial to future studies that employ time-resolved x-ray Coulomb explosion imaging to study ultrafast photochemistry.

Allum, Felix [Deutsches Elektronen-Synchrotron (DE↗

The development and use of metal-based probes for X-ray fluorescence microscopy

Abstract X-ray fluorescence microscopy (XFM) has become a widely used technique for imaging the concentration and distribution of metal ions in cells and tissues. Recent advances in synchrotron sources, optics, and detectors have improved the spatial resolution of the technique to <10 nm with attogram detection sensitivity. However, to make XFM most beneficial for bioimaging—especially at the nanoscale—the metal ion distribution must be visualized within the subcellular context of the cell. Over the years, a number of approaches have been taken to develop X-ray-sensitive tags that permit the visualization of specific organelles or proteins using XFM. In this review, we examine the types of X-ray fluorophore used, including nanomaterials and metal ions, and the approaches used to incorporate the metal into their target binding site via antibodies, genetically encoded metal-binding peptides, affinity labeling, or cell-specific peptides. We evaluate their advantages and disadvantages, review the scientific findings, and discuss the needs for future development.

36 MATERIALS SCIENCE↗

Fluid/Fluid Interfacial Areas Measured for Different Non-Wetting/Wetting Fluid Pairs in Natural Porous Media

This study examined the impact of fluid type and grain diameter on the interfacial area between different pairs of non-wetting and wetting fluids in natural porous media. Synchrotron X-ray microtomography was used to obtain high-resolution, three-dimensional images of multi-phase porous media systems. Multiple porous media, comprising a range of physical and geochemical properties, were used in this study. The four pairs of non-wetting/wetting fluids used were dense OIL/water, light OIL/water, air/dense OIL, and air/water. Images were obtained over a broad range of wetting phase saturation and for both wetting phase drainage and imbibition conditions. The results showed that for each fluid pair, the total (capillary + film) interfacial area increased with decreasing wetting fluid saturation. Interfacial areas were similar among all fluid pairs for a given porous medium. They were also similar for drainage and imbibition conditions. The maximum specific interfacial area (A m ) was shown to correlate well with inverse median grain diameter. The physical properties of the porous medium appear to have a greater influence on the magnitude of specific total interfacial area for a given saturation than fluid properties or wetting phase history.

NAPL↗

Characterisation of a laser plasma betatron source for high resolution x-ray imaging

Abstract We report on the characterisation of an x-ray source, generated by a laser-driven plasma wakefield accelerator. The spectrum of the optimised source was consistent with an on-axis synchrotron spectrum with a critical energy of 13.8 − 1.9 + 2.2 keV and the number of photons per pulse generated above 1 keV was calculated to be 6 − 0.9 + 1.2 × 10 9 . The x-ray beam was used to image a resolution grid placed 37 cm from the source, which gave a measured spatial resolution of 4 µ m × 5 µ m. The inferred emission region had a radius and length of 0.5 ± 0.2 µ m and 3.2 ± 0.9 mm respectively. It was also observed that laser damage to the exit aperture of the gas cell led to a reduction in the accelerated electron beam charge and a corresponding reduction in x-ray flux due to the change in the plasma density profile.

plasma acceleration↗

Integrated atomic force microscopy and x-ray irradiation for in situ characterization of radiation-induced processes

Understanding radiation-induced chemical and physical transformations at material interfaces is important across diverse fields, but experimental approaches are often limited to either ex situ observations or in situ electron microscopy or synchrotron-based methods in which cases the radiation type and dose are inextricably tied to the imaging basis itself. In this work we overcome this limitation by demonstrating integration of an X-ray source with an atomic force microscope to directly monitor radiolytically-driven interfacial chemistry at the nanoscale. We illustrate the value of in situ observations by examining effects of radiolysis on material adhesion forces in aqueous solution, as well as examining the production of alkali nitrates at the interface between an alkali halide crystal surface and air. For the examined salt-air interface, direct visualization under flexible experimental conditions greatly extends prior observations by enabling the transformation process to be followed comprehensively from source-to-sink with mass balance quantitation. Overall, our novel rad-AFM opens doors into understanding the dynamics of radiolytically-driven mass transfer and surface alteration at the nanoscale in real-time.

47 OTHER INSTRUMENTATION↗

Multilayer and grazing incidence X-ray/EUV optics for astronomy and projection lithography; Proceedings of the Meeting, San Diego, CA, July 19-22, 1992

The present volume on multilayer and grazing incidence X-ray/EUV optics for astronomy and projection lithography discusses AXAF grazing incidence mirrors, the theory and high throughput optics of grazing incidence optics, multilayer mirror fabrication and characterization, and multilayer optics for X-ray projection lithography. Attention is given to the VETA-I X-ray detection system, a motion detection system for AXAF X-ray ground testing, image analysis of the AXAF VETA-I X-ray mirror, and optical constants from mirror reflectivities measured at synchrotrons. Topics discussed include the application of aberration theory to calculate encircled energy of Wolter I-II telescopes, W/C multilayers deposited on plastic films, nonspecular X-ray scattering from Si/Mo multilayers, and multilayer thin-film design as FUV polarizers. Also discussed are thin-film filter lifetesting results in the EUV, chromospheric and coronal observations with multilayer optics, present and future requirements of soft X-ray projection lithography, and the imaging Schwarzschild multilayer X-ray microscope.

Hoover, Richard B.↗

Dimorphic Mechanisms of Fragility in Diabetes Mellitus: the Role of Reduced Collagen Fibril Deformation

ABSTRACT Diabetes mellitus (DM) is an emerging metabolic disease, and the management of diabetic bone disease poses a serious challenge worldwide. Understanding the underlying mechanisms leading to high fracture risk in DM is hence of particular interest and urgently needed to allow for diagnosis and treatment optimization. In a case–control postmortem study, the whole 12th thoracic vertebra and cortical bone from the mid-diaphysis of the femur from male individuals with type 1 diabetes mellitus (T1DM) (n = 6; 61.3 ± 14.6 years), type 2 diabetes mellitus (T2DM) (n = 11; 74.3 ± 7.9 years), and nondiabetic controls (n = 18; 69.3 ± 11.5) were analyzed with clinical and ex situ imaging techniques to explore various bone quality indices. Cortical collagen fibril deformation was measured in a synchrotron setup to assess changes at the nanoscale during tensile testing until failure. In addition, matrix composition was analyzed including determination of cross-linking and non-crosslinking advanced glycation end-products like pentosidine and carboxymethyl-lysine. In T1DM, lower fibril deformation was accompanied by lower mineralization and more mature crystalline apatite. In T2DM, lower fibril deformation concurred with a lower elastic modulus and tendency to higher accumulation of non-crosslinking advanced glycation end-products. The observed lower collagen fibril deformation in diabetic bone may be linked to altered patterns mineral characteristics in T1DM and higher advanced glycation end-product accumulation in T2DM. © 2022 The Authors. Journal of Bone and Mineral Research published by Wiley Periodicals LLC on behalf of American Society for Bone and Mineral Research (ASBMR).

59 BASIC BIOLOGICAL SCIENCES↗

Tonian Carbonates Record Phosphate-Rich Shallow Seas

The early-middle Neoproterozoic is thought to have witnessed significant perturbations to marine P cycling, in turn facilitating the rise of eukaryote-dominated primary production. However, with few robust constraints on aqueous P concentrations, current understanding of Neoproterozoic P cycling is generally model-dependent. To provide new geochemical constraints, we combined microanalytical data sets with solid-state Nuclear Magnetic Resonance, synchrotron-based X-ray Absorption Near Edge Structure spectroscopy, and micro-X-ray Fluorescence imaging to characterize the speciation and distribution of P in Tonian shallow-water carbonate rocks. These data reflect shallow water phosphate concentrations 10–100× higher than modern systems, supporting the hypothesis that tectonically-driven influxes in P periodically initiated kinetically-controlled CaCO 3 deposition, in turn destabilizing marine carbonate chemistry, climate, and nutrient inventories. Alongside these observations, a new compilation and statistical analysis of mudstone geochemistry data indicates that, in parallel, C org and P burial increased across later Tonian continental margins until becoming decoupled at the close of the Tonian, implicating widespread N-limitation triggered by increasing atmospheric O 2 .

58 GEOSCIENCES↗

Center for the development of commercial crystal growth in space

The second year of operation of the Center for Commercial Crystal Growth in Space is described. This center is a consortium of businesses, universities and national laboratories. The primary goal of the Center's research is the development of commercial crystal growth in space. A secondary goal is to develop scientific understanding and technology which will improve commercial crystal growth on earth. In order to achieve these goals the Center's research is organized into teams by growth technique; melt growth, solution growth, and vapor growth. The melt growth team is working on solidification and characterization of bulk crystals of gallium arsenide and cadmium telluride. They used high resolution X-ray topography performed at the National Synchrotron Light Source at Brookhaven National Laboratory. Streak-like features were found in the diffraction images of semi-insulating undoped LEC GaAs. These were shown to be (110) antiphase boundaries, which have not been reported before but appear to be pervasive and responsible for features seen via less-sensitive characterization methods. The results on CdTe were not as definitive, but indicate that antiphase boundaries may also be responsible for the double peaks often seen in X-ray rocking curves of this material. A liquid encapsulated melt zone system for GaAs has been assembled and techniques for casting feed rods developed. It was found that scratching the inside of the quartz ampoules with silicon carbide abrasive minimized sticking of the GaAs to the quartz. Twelve floating zone experiments were done.

Wilcox, William R.↗

Characterization of Three Carbon- and Nitrogen-Rich Particles from Comet 81P/WILD

Comets may sample the early solar system s complement of volatile-forming elements - including C and N - more fully and reliably than do the terrestrial planets or asteroids. Until recently, all elemental analyses of unambiguously cometary material were carried out remotely. The return of the Stardust mission makes it possible to analyze documented material from P81/Wild 2 in the laboratory Wild 2 particles fragmented when they stopped in the aerogel collectors. We have studied three fragments thought to be rich in C and N by using several techniques: FTIR to characterize organic matter; synchrotron-induced x-ray fluorescence (SXRF) to determine Fe and certain element/Fe ratios; SEM to image sample morphology and to detect semiquantitatively Mg, Al, Si, Ca, and Fe; and nuclear reaction analysis (NRA) to measure C, N, O, and Si.

Gallien, J.-P.↗

Time-Resolved Geometric Feature Tracking Elucidates Laser-Induced Keyhole Dynamics

In this report, during laser melting of metals, localized metal evaporation resulting in the formation of a keyhole shaped cavity can occur if processing conditions are chosen with high power density. An unstable keyhole can have deleterious effects in certain applications (e.g., laser powder bed fusion) as it increases the likelihood of producing defects such as porosity. In this work, we propose a pipeline that enables complete segmentation and extraction of various geometric features in keyholing conditions. In situ synchrotron high-speed X-ray visualization at the Advanced Photon Source provides large datasets of experimental images with a high spatio-temporal resolution across a range of laser parameters for Ti-6Al- 4 V. Computer vision image processing techniques were used to extract time-resolved quantitative geometric features (e.g., depth, width, front wall angle) throughout keyhole evolution which were subsequently analyzed to understand the relationship between the variation of local keyhole geometry and processing conditions. This analysis is the first to employ a data-driven approach to further our understanding of the keyholing process regime.

36 MATERIALS SCIENCE↗

Using Image Pro Plus Software to Develop Particle Mapping on Genesis Solar Wind Collector Surfaces

The continued success of the Genesis mission science team in analyzing solar wind collector array samples is partially based on close collaboration of the JSC curation team with science team members who develop cleaning techniques and those who assess elemental cleanliness at the levels of detection. The goal of this collaboration is to develop a reservoir of solar wind collectors of known cleanliness to be available to investigators. The heart and driving force behind this effort is Genesis mission PI Don Burnett. While JSC contributes characterization, safe clean storage, and benign collector cleaning with ultrapure water (UPW) and UV ozone, Burnett has coordinated more exotic and rigorous cleaning which is contributed by science team members. He also coordinates cleanliness assessment requiring expertise and instruments not available in curation, such as XPS, TRXRF [1,2] and synchrotron TRXRF. JSC participates by optically documenting the particle distributions as cleaning steps progress. Thus, optical document supplements SEM imaging and analysis, and elemental assessment by TRXRF.

Rodriquez, Melissa C.↗

Simulations of coherent scattering experiments at storage ring synchrotron radiation sources in the hard x-ray range

Detailed simulations of experiments carried out at modern light sources are directly related to the most efficient and productive use of these facilities for research in multiple branches of science and technology. The “Synchrotron Radiation Workshop” computer code with its Python interface, and Sirepo web-browser-based graphical user interface, currently supports physical optics simulations of coherent X-ray scattering and imaging experiments on user-defined virtual samples. We present examples of simulations of coherent scattering experiments that are typically performed at the Coherent Hard X-ray beamline at Brookhaven National Laboratory’s (BNL) National Synchrotron Light Source II. We also present several comparisons of the simulations with the results of actual coherent X-ray scattering experiments with nano-fabricated test samples produced at BNL’s Center for Functional Nanomaterials.

36 MATERIALS SCIENCE↗

Convolutional Neural Network for Segmenting Micro-X-ray Computed Tomography Images of Wood Cellular Structures

To further enhance the performance of wood products, improved tools are needed to study in situ cellular scale phenomena like mechanical deformations and moisture swelling. Micro-X-ray computed tomography (μXCT) using brilliant synchrotron light sources now has the spatial and temporal resolution for real-time visualization of phenomena in three-dimensional cellular structures. However, the tradeoff for speed includes the loss of intensity contrast between different types of materials within the imaged structure, such as cell wall and air in wood. This loss of contrast prevents traditional histogram-based segmentation methods from being used effectively. A new convolutional neural network (CNN) approach was therefore developed to segment fast μXCT images of wood into cell wall and air volumes. The fast μXCT and segmentation were demonstrated in the study of moisture swelling in loblolly pine (Pinus taeda) earlywood and latewood cellular structures conditioned at 0%, 33%, 75%, and 95% relative humidity (RH). The CNN segmentation results had a mean intersection over union (IoU) metric accuracy of 96%. Initial analysis of the swelling in the latewood revealed cell walls swelled about 25% when conditioned from 0% to 95% RH. Additionally, the widths of ray cell lumina in the transverse plane of latewood could be observed to increase at higher RH. The segmentation method presented here will facilitate future quantitative analyses in in situ μXCT studies of wood and other similar cellular materials.

Arzola-Villegas, Xavier (ORCID:0000000305369766)↗