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At least 55 records · Page 3

Multimodal, Multidimensional, and Multiscale X-ray Imaging at the National Synchrotron Light Source II

Over the last couple of decades, the synchrotron radiation research community has witnessed tremendous advancement in the field of x-ray imaging and microscopy. Continuing enhancement of the light sources’ brightness, advances in x-ray focusing optics, incorporation of precision instruments, and development of innovative imaging techniques are some of the leading contributors for the rapid progress. New imaging and microscopy beamlines, such as the ones at the National Synchrotron Light Source II (NSLS-II), a Department of Energy (DOE) Office of Science user facility located at DOE’s Brookhaven National Laboratory, are capable of performing more sophisticated and complicated measurements than ever before, either on their own or used together as a suite of tools. These sophisticated and complex measurements exhibit attributes for multimodal, multidimensional, and multiscale imaging. Recent popularity of these methods is strongly driven by the current trends in materials characterizations, where researchers desire to map out hierarchical materials structure over a large range of length scales, to understand structure-property correlation, to quantify materials structures in 3D, and/or to perform operando or in situ experiments. It is important to emphasize that “materials” under investigation are not only synthesized materials but also the natural materials. In this article, we describe multimodal, multidimensional and multiscale x-ray imaging capabilities of the NSLS-II beamlines and how these methods are used to tackle complex scientific problems.

47 OTHER INSTRUMENTATION↗

Revealing transient powder-gas interaction in laser powder bed fusion process through multi-physics modeling and high-speed synchrotron x-ray imaging

Laser powder bed fusion (LPBF) is an emerging metal additive manufacturing process. The gas-driven powder motions in laser powder bed fusion have significant influence on the build quality. However, the transient powder-gas interaction has not been well understood due to the challenges in quantitative experiment measurements. In this work, the powder-gas interaction for a single pulse laser illuminating on the powder bed is studied. We establish a multi-physics model to simulate the complex liquid/gas flow as well as the gas-driven powder motions, which is substantiated by high-speed synchrotron x-ray imaging. We identify and quantify four characteristic modes of powder-gas interaction in LPBF. The motion of a powder is controlled by one or multiple interaction modes collectively. As revealed by simulations and confirmed by experiments, powders can merge into the molten pool from its rim, be ejected at different divergence angles (powder spattering), or dive into the molten pool to cause significant molten pool fluctuation. Overall, our results provide insights toward the driving forces controlling the dynamic powder behavior, which pave the way for reducing structure defects during the build process.

36 MATERIALS SCIENCE↗

Pressure Drop with Moving Contact Lines and Dynamic Contact Angles in a Hydrophobic Round Minichannel: Visualization via Synchrotron X-ray Imaging and Verification of Experimental Correlations

In hydrophobic mini- and microchannels, slug flow with moving contact lines is typically generated under various two-phase flow conditions. There is a significant pressure drop in this flow pattern with moving contact lines, which is closely related to the dynamic contact angles. Researchers have investigated dynamic contact angles experimentally for decades, but due to the limitations of visualization techniques, these experiments have typically been conducted in low Weber number regions (We < 10 –3 ). In this study, we clearly visualized the dynamic contact angles of a liquid slug in high Weber number regions (10 –3 < We <1) via synchrotron X-ray imaging with high temporal (~1000 fps) and spatial (~ 2 μm/pixel) resolutions. We precisely measured the pressure drop with moving contact lines in a hydrophobic minichannel (inner diameter = 1.018 mm). On the basis of our experimental data, we verified previous correlations for dynamic contact angles and explored the relationship between pressure drop with moving contact lines and dynamic contact angles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Polarized Image of a Synchrotron-emitting Ring of Gas Orbiting a Black Hole

Synchrotron radiation from hot gas near a black hole results in a polarized image. The image polarization is determined by effects including the orientation of the magnetic field in the emitting region, relativistic motion of the gas, strong gravitational lensing by the black hole, and parallel transport in the curved spacetime. We explore these effects using a simple model of an axisymmetric, equatorial accretion disk around a Schwarzschild black hole. By using an approximate expression for the null geodesics derived by Beloborodov and conservation of the Walker–Penrose constant, we provide analytic estimates for the image polarization. We test this model using currently favored general relativistic magnetohydrodynamic simulations of M87*, using ring parameters given by the simulations. For a subset of these with modest Faraday effects, we show that the ring model broadly reproduces the polarimetric image morphology. Our model also predicts the polarization evolution for compact flaring regions, such as those observed from Sgr A* with GRAVITY. With suitably chosen parameters, our simple model can reproduce the EVPA pattern and relative polarized intensity in Event Horizon Telescope images of M87*. Under the physically motivated assumption that the magnetic field trails the fluid velocity, this comparison is consistent with the clockwise rotation inferred from total intensity images.

79 ASTRONOMY AND ASTROPHYSICS↗

Fe Oxidation and Species Distribution at the Rock–Fluid Interface of Marcellus Shale Reacted with Hydraulic Fracturing Fluid

Hydraulic fracturing of shale reservoirs resulted in significant opportunity for increased oil and gas production in the United States. Rock-fluid interactions can cause mineral dissolution and precipitation reactions that lead to permeability changes in the shale matrix, which ultimately may affect transport pathways and hydrocarbon production. Understanding the distribution of secondary precipitates, such as barite and Fe(III) (hydro)oxides, and cation leaching at the rock-fluid interface is an important step to further investigate how these geochemical processes can change permeability and transport pathways. In this study, thin sections of the fracture-matrix interface were made from reacted Marcellus shale cores. The thin sections were characterized using synchrotron X-ray fluorescence imaging and synchrotron X-ray absorption spectroscopy. Fe species with different oxidation states were identified in the maps, together with barite and Ca distribution. The results show that ferrihydrite, as newly formed Fe(III)-bearing precipitates, aligned well with the border of the Ca (e.g., calcite) leaching region in the reaction front. Some Fe-containing clay also dissolved, but the dissolution region for the clay was not as deep as the calcite. Further, the reaction front is about three times deeper in the direction parallel to the shale bedding than that perpendicular to the bedding. The Ca leaching region can be an index for reaction front detection for Marcellus shale. Reactive transport modeling was conducted and the predicted Ca leaching boarder align well with ferrihydrite precipitation, consistent with the experimental observation. The carbonate mineral dissolution can be crucial to promote fluid access into the shale matrix. Together with our previous study on the shale reactive surface, this follow-up study showed similar Ca leaching region and Fe(III) precipitates distribution in the reaction front regardless of barite precipitation on the surface, indicating that the barite coatings on the surface may not pose a significant impact on reactive transport at the shale-fluid interface.

04 OIL SHALES AND TAR SANDS↗

A new μ -high energy resolution fluorescence detection microprobe imaging spectrometer at the Stanford Synchrotron Radiation Lightsource beamline 6-2

In this report we describe a new synchrotron X-ray Fluorescence (XRF) imaging instrument with an integrated High Energy Fluorescence Detection X-ray Absorption Spectroscopy (HERFD-XAS) spectrometer at the Stanford Synchrotron Radiation Lightsource at beamline 6-2. The X-ray beam size on the sample can be defined via a range of pinhole apertures or focusing optics. XRF imaging is performed using a continuous rapid scan system with sample stages covering a travel range of 250 × 200 mm 2 , allowing for multiple samples and/or large samples to be mounted. The HERFD spectrometer is a Johann-type with seven spherically bent 100 mm diameter crystals arranged on intersecting Rowland circles of 1 m diameter with a total solid angle of about 0.44% of 4π sr. A wide range of emission lines can be studied with the available Bragg angle range of ~64.5°–82.6°. With this instrument, elements in a sample can be rapidly mapped via XRF and then selected features targeted for HERFD-XAS analysis. Furthermore, utilizing the higher spectral resolution of HERFD for XRF imaging provides better separation of interfering emission lines, and it can be used to select a much narrower emission bandwidth, resulting in increased image contrast for imaging specific element species, i.e., sparse excitation energy XAS imaging. This combination of features and characteristics provides a highly adaptable and valuable tool in the study of a wide range of materials.

47 OTHER INSTRUMENTATION↗

High-resolution in-beam video rate imaging with the ClearXCam for synchrotron beamlines

The ClearXCam detector is a new video rate imaging in-beam monitor based on a diamond sensor. Imaging with 2304 effective pixels is achieved by sequentially biasing one of 48 metal stripes on one side of a diamond sensor, while reading out the current from 48 stripes on the other side of the sensor. This system was characterized for real-time X-ray beam diagnostics at synchrotron beam­line 17-BM at the National Synchrotron Light Source II. Significant results include: detection of in-beam structure via the imaging mode, beam focusing in one minute with real-time imaging feedback during a focusing event, linearity over five orders of magnitude, validation of a fast mode operating at 100 Hz, and sub-micron beam-positioning resolution. The system is now available commercially.

36 MATERIALS SCIENCE↗

Quantitative and qualitative bone imaging: A review of synchrotron radiation microtomography analysis in bone research

All levels of the unique hierarchical structure of bone, consisting of collagen and hydroxyapatite crystals at the nanoscale to osteon/lamellae structures at the microscale, contribute to its characteristic toughness and material properties. Elements of bone's density and size contribute to bone quantity (or bone mass), whereas elements of bone's material composition, material properties, internal structure, and organization describe bone quality. Furthermore, bone quantity and quality can be degraded by factors such as aging, disease, treatments, and irradiation, compromising its ability to resist fracture and sustain loading. Accessing the morphology and architecture of bone at the microscale to quantify microstructural features and assess the degree of mineralization and path of crack propagation in bone provides crucial information on how these factors are influencing bone quantity and quality. Synchrotron radiation micro-computed tomography (SRμCT) was first used to assess bone structure at the end of the 1990's. One of the main advantages of the technique is that it enables accurate three-dimensional (3D), non-destructive quantification of structure while traditional histomorphometry on histological sections is inherantly destructive to the sample and two-dimensional (2D). Additionally, SRμCT uses monochromatic, high-flux X-ray beams to provide high-resolution and high-contrast imaging of bone samples. This allows the quantification of small microstructural features (e.g. osteocyte lacunae, canals, trabeculae, microcracks) and direct gray value compositional mapping (e.g. mineral quantification, cement lines) with greater speed and fidelity than lab-based micro-computed tomography. In this article, we review how SRμCT has been applied to bone research to elucidate the mechanisms by which bone aging, disease, and other factors affect bone fragility and resistance to fracture.

60 APPLIED LIFE SCIENCES↗

In situ synchrotron X-ray imaging and mechanical properties characterization of additively manufactured high-entropy alloy composites

Laser beam directed energy deposition has become an increasingly popular advanced manufacturing technique for materials discovery as a result of the in situ alloying capability. In this study, we leverage an additive manufacturing enabled high throughput materials discovery approach to explore the composition space of a graded W x (CoCrFeMnNi) 100–x sample spanning 0 ≤ x ≤ 21 at%. In addition to microstructural and mechanical characterization, synchrotron high speed x-ray computer aided tomography was conducted on a W 20 (CoCrFeMnNi) 80 composition to visualize melting dynamics, powder-laser interactions, and remelting effects of previously consolidated material. Results reveal the formation of the Fe 7 W 6 intermetallic phase at W concentrations> 6 at%, despite the high configurational entropy. Unincorporated W particles also occurred at W concentrations> 10 at% accompanied by a dissolution band of Fe 7 W 6 at the W/matrix interface and hardness values greater than 400 HV. In this work, the primary strengthening mechanism is attributed to the reinforcement of the Fe 7 W 6 and W phases as a metal matrix composite. The in situ high speed x-ray imaging during remelting showed that an additional laser pass did not promote further mixing of the Fe 7 W 6 or W phases suggesting that, despite the dissolution of the W into the Fe 7 W 6 phase being thermodynamically favored, it is kinetically limited by the thickness/diffusivity of the intermetallic phase, and the rapid solidification of the laser-based process.

36 MATERIALS SCIENCE↗

Real-time damage characterization for GFRCs using high-speed synchrotron X-ray phase contrast imaging

Here, we report the application of high-speed synchrotron X-ray phase contrast imaging (PCI) in real-time damage characterization for glass fiber reinforced composites (GFRCs) subjected to dynamic loading. Dynamic single-edge notched bending (DSENB) experiments on pre-notched S-2 GFRCs were performed on a modified Kolsky compression bar. During loading, the synchrotron X-ray beam penetrated through the composite specimen from the side to detect damage evolution inside the material. Entire dynamic events were recorded by a high-speed camera as image sequences.0° and 90° unidirectional and cross-ply composites were investigated. An optical imaging technique was also employed to capture similar dynamic events in comparison with the radiographic imaging. It is demonstrated that high-speed X-ray PCI had sufficient phase contrast to characterize a crack initiation at a 20-μm spatial resolution within 920 ns and track the crack geometry during propagation, thereby providing reliable data to quantify the dynamic damage resistance of GFRCs. Furthermore, being capable of recognizing microscopic damage-related features at a sub-10-μm resolution, high-speed X-ray PCI provided fundamental material failure mechanisms to reveal the essential of macroscale structural failure of composites. It can also track the damage evolution inside and between individual plies of laminated composites. However, current high-speed X-ray PCI technique only supports in-situ observation and the high timing and spatial resolutions are limited within a field of view of ~2.5 mm in square, preventing its application in the three-dimensional and larger-area damage detection for GFRC structures.

42 ENGINEERING↗

Synchrotron X-ray based particle image velocimetry to measure multiphase streamflow and densitometry

Synchrotron-based radiation techniques are increasingly used in the field of flow condition measurements. As a complicated multiphase flow, cavitation has been investigated in a wide variety of industrial fields, to prevent damages on spillways at large dams or intensify the bacteria eradication rate during water treatments. To control the detrimental effects of cavitating flows, the dynamics of and mechanisms affecting cavitation development shall be visualized and identified in real-time. Due to the large reflection and scattering effects of multiphase flow, standard visible-light imaging technologies cannot penetrate vapor bubbles and provide extremely limited information. In this study, the synchrotron source emitted high-flux X-ray pulses are used to capture flow motion and visualize internal structures with sufficiently high spatial and temporal resolutions. The image processing procedures on raw x-ray images are developed using 2D Fourier transform (FT) and wavelet transform (WT) to implement the contrast enhancement and de-noising. Through the edge detection algorithm, tracking either seeded particles or phase interfaces inside the opaque multiphase flow can be achieved to perform the particle image velocimetry. Further, with decomposing particle-only and particle-eliminated subplots from the X-ray phase-contrast image, the time-resolved velocity and void fraction fields are obtained simultaneously, paving a way for further flow condition analysis such as densitometry.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Root size and soil physicochemical properties drive microscale spatial patterns of Fe and As retention in the rice rhizosphere

Background and Aims: Radial oxygen loss from rice roots in flooded soils oxidizes and precipitates dissolved Fe(II), Mn(II), and As(III) into mixed Fe(III), Mn(III/IV), and As(V) as root plaque and in the rhizosphere soil. It is unknown how different soils and root sizes impact the spatial extent of Fe and As retention outside the root. Methods: We imaged cross-sections of 90 roots from 6 different soils using synchrotron μXRF imaging followed by k-means clustering and elliptical averaging to distinguish bulk soil, rhizosphere, plaque, and roots based on As and Fe patterns. Results: We found preferential As retention in the plaque and rhizospheres of most roots except small (< 0.45 mm) roots in silty soils with low P or high As. In contrast, clayey soils had similar As-Fe correlations across plaque, rhizosphere, and bulk soil. Large (> 0.45 mm) roots often had no oxidized rhizosphere region. We obtained an extensive dataset of 256 As and 155 Mn synchrotron μXANES measurements, which revealed that rhizosphere and plaque As was mainly inorganic As(V) and As(III), and Mn oxidation state varied between soils but not between belowground locations. Conclusion: Small roots in coarse-textured soils were less likely to have As retention in the plaque or rhizosphere compared to large roots and fine-textured soils. Furthermore, the unique and extensive data in this study provides new insight into soil and root size impacts on As retention in the rhizosphere. It is essential to investigate a representative number of samples to draw conclusions from XRF imaging.

36 MATERIALS SCIENCE↗

High throughput automated characterization of enamel microstructure using synchrotron tomography and optical flow imaging

The remarkable damage-tolerance of enamel has been attributed to its hierarchical microstructure and the organized bands of decussated rods. A thorough characterization of the microscale rod evolution within the enamel is needed to elucidate this complex structure. While prior efforts in this area have made use of single particle tracking to track a single rod evolution to various degrees of success, such a process can be both computationally and labor intensive, limited to the evolution path of a single rod, and is therefore prone to error from potentially tracking outliers. Particle image velocimetry (PIV) is a well-established algorithm to derive field information from image sequences for processes that are time-dependent, such as fluid flows and structural deformation. In this work, we demonstrate the use of PIV in extracting the full-field microstructural distribution of rods within the enamel. Further, enamel samples from a wild African lion were analyzed using high-energy synchrotron X-ray micro-tomography. Results from the PIV analysis provide sufficient full-field information to reconstruct the growth of individual rods that can potentially enable rapid analysis of complex microstructures from high resolution synchrotron datasets. Such information can serve as a template for designing damage-tolerant bioinspired structures for advanced manufacturing.

36 MATERIALS SCIENCE↗

The use of synchrotron X-ray fluorescent imaging to study distribution and content of elements in chemically fixed single cells: a case study using mouse pancreatic beta-cells

Synchrotron X-ray fluorescence microscopy (SXRF) presents a valuable opportunity to study the metallome of single cells because it simultaneously provides high-resolution subcellular distribution and quantitative cellular content of multiple elements. Different sample preparation techniques have been used to preserve cells for observations with SXRF, with a goal to maintain fidelity of the cellular metallome. In this case study, mouse pancreatic beta-cells have been preserved with optimized chemical fixation. We show that cell-to-cell variability is normal in the metallome of beta-cells due to heterogeneity and should be considered when interpreting SXRF data. Additionally, we determined the impact of several immunofluorescence (IF) protocols on metal distribution and quantification in chemically fixed beta-cells and found that the metallome of beta-cells was not well preserved for quantitative analysis. However, zinc and iron qualitative analysis could be performed after IF with certain limitations. To help minimize metal loss using samples that require IF, we describe a novel IF protocol that can be used with chemically fixed cells after the completion of SXRF.

59 BASIC BIOLOGICAL SCIENCES↗