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At least 145 records · Page 8

High-speed quantitative X-ray multi-contrast imaging with deep learning based modulated pattern analysis

The advent of X-ray multi-contrast imaging methods, providing absorption, phase, and dark-field images, holds tremendous promise for complementary and non-destructive visualization of inner structures within materials and bio-samples. However, the low efficiency in measuring and analyzing X-ray modulated patterns has hindered their application in high-resolution in situ imaging. In this work, the Enhanced Scanning Pattern-based Imaging Neural Network (ESPINNet) is introduced as a powerful tool for achieving high-speed, high-resolution quantitative imaging. ESPINNet is faster than correlation-based speckle tracking methods such as XSVT and UMPA, and provides a balanced performance in terms of resolution and speed for data collection by using fewer scanning images. In comparison with our previously developed neural network, ESPINNet introduces the capability to generate dark-field images, further enhancing its versatility. By leveraging scanning patterns, ESPINNet significantly improves resolution and measurement precision. Furthermore, its adaptability to various modulation patterns, including those produced by sandpaper, coded masks, or gratings, ensures broad applicability. These features enable real-time 2D and 3D multi-contrast imaging, positioning ESPINNet as a transformative solution for applications in materials science and biomedical research, particularly for high-speed and in situ measurements.

X-ray at-wavelength metrology↗

Dynamic in situ imaging of methane hydrate formation in coal media

Fast 3D X-ray imaging has proved to provide crucial insights into multi-phase dynamic processes in various geomaterials. In particular, many in situ imaging experiments have been made to study gas-hydrate formation in porous sandy samples. Such imaging is challenging for the methane gas-hydrate formation in coal samples because of the coal micro-porosity structure and lower X-ray contrast. Here we present results of the first dynamic in situ micro-computed tomography experiment of methane-hydrate formation in coal samples. Synchrotron phase-contrast tomography techniques allowed to achieve necessary contrast levels to separate all the materials of interest (gas, water, coal, and gas hydrate) in reconstructed images with high spatial and temporal resolution. The imaging results are compared to the ones from a similar tomographic experiment with sand samples. Methane-hydrate formation is accompanied by the water movements caused by cryogenic water suction that happens in sequences of short fast movements with longer equilibrium states in between. Only one type of the hydrate formation was observed in coal (growth as shells on grain boundaries) as opposed to three types in sand (shells, growth into gas pockets, and inside water volumes). In particular, this leads to a slower hydrateformation speed in coal. For the coal sample, we also observed water extraction from grains, and interpreted it as competitive sorption of methane. Lastly, we visualized the dynamic behavior of this water extraction via microchannels inside the coal grains, and performed nano-tomography imaging of these channels for a better understanding of this phenomenon.

58 GEOSCIENCES↗

Serial Moire scanning phase contrast x-ray imaging

Method include emitting x-rays from an x-ray source, directing a first portion of the x-rays through an object grating situated adjacent to an object while the object is scanned relative to the object grating along a scan direction, directing a second portion of the x-rays through the object and subsequently through a detector grating without transmitting through the object grating, wherein the object grating and detector grating are adjacently arranged in a field of view of the x-rays sequentially with respect to each other in the scan direction, and receiving the first portion transmitted through the object and object grating with a first portion of a detector and receiving the second portion transmitted through the object and the detector grating with a second portion of the detector adjacent to the first portion of the detector. Systems are also disclosed, along with related techniques for beam hardening correction.

Miller, Erin A.↗

PhaseT3M: 3D imaging at 1.6 Å resolution via electron cryo-tomography with nonlinear phase retrieval

Electron cryo-tomography (cryo-ET) enables 3D imaging of complex, radiation-sensitive structures with molecular detail. However, image contrast from the interference of scattered electrons is nonlinear with atomic density and multiple scattering further complicates interpretation. These effects degrade resolution, particularly in conventional reconstruction algorithms, which assume linearity. Particle averaging can reduce such issues but is unsuitable for heterogeneous or dynamic samples ubiquitous in biology, chemistry, and materials sciences. Here, we develop a phase retrieval-based cryo-ET method, PhaseT3M. We experimentally demonstrate its application to an approximately 7 nm Co3O4 nanoparticle on an approximately 30 nm carbon substrate, achieving a maximum resolution of 1.6 Å, surpassing conventional limits using standard cryo-TEM equipment. PhaseT3M uses a multislice model for multiple scattering and Bayesian optimization for alignment and computational aberration correction, with a positivity constraint to recover ‘missing wedge’ information. Applied directly to biological particles, it enhances reconstruction quality and reduces artifacts, establishing a standard for routine 3D imaging with phase contrast.

Biophysics↗

Current advances on Talbot–Lau x-ray imaging diagnostics for high energy density experiments (invited)

Talbot–Lau x-ray interferometry is a refraction-based diagnostic that can map electron density gradients through phase-contrast methods. The Talbot–Lau x-ray deflectometry (TXD) diagnostics have been deployed in several high energy density experiments. To improve diagnostic performance, a monochromatic TXD was implemented on the Multi-Tera Watt (MTW) laser using 8 keV multilayer mirrors (Δθ/θ = 4.5%-5.6%). Copper foil and wire targets were irradiated at 10 14 –10 15 W/cm 2 . Laser pulse length (~10 to 80 ps) and backlighter target configurations were explored in the context of Moiré fringe contrast and spatial resolution. Foil and wire targets delivered increased contrast <30%. The best spatial resolution (<6 μm) was measured for foils irradiated 80° from the surface. Further TXD diagnostic capability enhancement was achieved through the development of advanced data postprocessing tools. The Talbot Interferometry Analysis (TIA) code enabled x-ray refraction measurements from the MTW monochromatic TXD. Additionally, phase, attenuation, and dark-field maps of an ablating x-pinch load were retrieved through TXD. The images show a dense wire core of ~60 μm diameter surrounded by low-density material of ~40 μm thickness with an outer diameter ratio of ~2.3. Attenuation at 8 keV was measured at ~20% for the dense core and ~10% for the low-density material. Instrumental and experimental limitations for monochromatic TXD diagnostics are presented. Enhanced postprocessing capabilities enabled by TIA are demonstrated in the context of high-intensity laser and pulsed power experimental data analysis. Significant advances in TXD diagnostic capabilities are presented. Furthermore, these results inform future diagnostic technique upgrades that will improve the accuracy of plasma characterization through TXD.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Comparison of Shadowgraphy and X-Ray Phase Contrast Methods for Characterizing a DT Ice Layer in an Inertial Confinement Fusion Target

Shadowgraphy and x-ray phase contrast (XPC) imaging are two techniques that are used for characterizing the deuterium-tritium ice layer in Inertial Confinement Fusion targets. Each technique has limitations that affect how accurately they can characterize small crystalline defects and measure the ice-thickness non-uniformities that may be only a few micrometers in height. The concern is that shadowgraphy may be overly sensitive to the shape and depth of defects in the surface and insufficiently sensitive to the shape of longer-wavelength roughness, while x-ray phase contrast may be too insensitive to defects in the ice surface. Multiple ice layers with different thicknesses (40 to 63 μm), thickness uniformities (peak-valley variations that range from <2- to 12 μm), and crystal defects were analyzed using shadowgraphy and x-ray phase contrast techniques. The results from each method agree when the ice layer is uniformly thick and the crystal lacks defects. That agreement worsens as the number of defects in the surface of the ice layer increases and the roughness that is determined from a shadowgram image of the target’s limb is greater than can be justified by the number of defects that are seen in the target’s front and rear surfaces. The XPC technique is considerably less sensitive to surface defects, in part due to the poorer dynamic range and image resolution compared to shadowgraphy. Localized regions of the ice layer that are thicker or thinner than the average thickness of the layer are reported by shadowgraphy to be smaller in height and footprint (by up to 30%) than by XPC. As a result, the two techniques report different ice layer thicknesses that can vary by up to 10%. Shadowgraphy results from two caustics that trace different paths through the target, and, in theory, image the same ice-vapor surface (but reflect from either the vapor or ice side of the interface) did not consistently characterize the size or shape of ice features to be the same magnitude. Here, the XPC technique provides the best assessment of low-mode (l < 7) roughness in the ice layer. Shadowgraphy results using the strongest caustic is best for detecting the presence of grooves in the ice, though not for quantifying the size of them. If multiple grooves are present it is best to discard and reform the ice layer.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Complexions at the iron-magnetite interface

Synthesizing distinct phases and controlling crystalline defects are key concepts in materials design. These approaches are often decoupled, with the former grounded in equilibrium thermodynamics and the latter in nonequilibrium kinetics. By unifying them through defect phase diagrams, we can apply phase equilibrium models to thermodynamically evaluate defects—including dislocations, grain boundaries, and phase boundaries—establishing a theoretical framework linking material imperfections to properties. Using scanning transmission electron microscopy (STEM) with differential phase contrast (DPC) imaging, we achieve the simultaneous imaging of heavy Fe and light O atoms, precisely mapping the atomic structure and chemical composition at the iron-magnetite (Fe/Fe 3 O 4 ) interface. We identify a well-ordered two-layer interface-stabilized phase state (referred to as complexion) at the Fe[001]/Fe 3 O 4 [001] interface. Using density-functional theory (DFT), we explain the observed complexion and map out various interface-stabilized phases as a function of the O chemical potential. The formation of complexions increases interface adhesion by 20% and alters charge transfer between adjacent materials, impacting transport properties. Our findings highlight the potential of tunable defect-stabilized phase states as a degree of freedom in materials design, enabling optimized corrosion protection, catalysis, and redox-driven phase transitions, with applications in materials sustainability, efficient energy conversion, and green steel production.

36 MATERIALS SCIENCE↗

Time-resolved spray characterization via unified optical flow and binarization technique

This work leverages an unsupervised machine learning and advanced image processing techniques to characterize the breakup of fuel sprays in a small-scale combustor under reacting conditions, providing valuable insights into near-nozzle flow phenomenology. The proposed methodology integrates an improved optical flow model on a convolutional neural network to extract flow vectors with a binarization technique to assess droplets’ size and shape across the region of interest. The velocimetry approach demonstrates superior performance compared to a state-of-the-art optical flow model when applied to high-speed X-ray phase contrast spray images, achieving more accurate and reliable flow predictions. Moreover, breakup processes are quantified by breakup length and sphericity in accordance with velocity estimations, allowing a more complete characterization of the flow. This study establishes a robust methodology for analyzing spray morphology and primary breakup in compact combustors, contributing valuable means of understanding and optimizing fuel spray behavior in advanced combustion systems.

42 ENGINEERING↗

Spatial Mapping of Electrostatic Fields in 2D Heterostructures

In situ electron microscopy is an effective tool for understanding the mechanisms driving novel phenomena in 2D structures. However, due to practical challenges, it is difficult to address these technologically relevant 2D heterostructures with electron microscopy. Here, we use the differential phase contrast (DPC) imaging technique to build a methodology for probing local electrostatic fields during electrical operation with nanoscale spatial resolution in such materials. We find that, by combining a traditional DPC setup with a high-pass filter, we can largely eliminate electric fluctuations emanating from short-range atomic potentials. Using a method based on this filtering algorithm, a priori electric field expectations can be directly compared with experimentally derived values to readily identify inhomogeneities and potentially problematic regions. Furthermore, we use this platform to analyze the electric field and charge density distribution across layers of hBN and MoS 2 .

79 ASTRONOMY AND ASTROPHYSICS↗

The incommensurate modulation of tetragonal tungsten bronze quantified by high resolution 4D STEM

Many members of the tetragonal tungsten bronze (TTB) family of oxides display an incommensurate periodic lattice distortion, the nature of which has been the subject of some controversy. Here we present a study of this structural modulation in the relaxor ferroelectric Ba 5 SmSn 3 Nb 7 O 30 (BSSN) by quantitative scanning transmission electron microscopy (STEM). Additionally, we characterize the modulation in BSSN by employing a fast, pixelated direct electron detector to perform high resolution phase contrast STEM imaging of the crystalline lattice. By quantitatively analyzing the images, we visualize the atomic structural correlations present in the material on both the cation and anion sublattices. This analysis reveals the incommensurate structure to have an octahedral tilting pattern and cooperative A2 site cation displacements, analogous to an Ama2 commensurate cell. Finally, we show that the modulation is composed of a structural motif with a period of 3 x $d_{1\bar{1}0}$ and modified by discommensurations, likely arise from frustrated octahedral tilting in the odd-valued periodicity.

Differential phase contrast↗

A Three-Dimensional Reconstruction Algorithm for Scanning Transmission Electron Microscopy Data from a Single Sample Orientation

Abstract Increasing interest in three-dimensional nanostructures adds impetus to electron microscopy techniques capable of imaging at or below the nanoscale in three dimensions. We present a reconstruction algorithm that takes as input a focal series of four-dimensional scanning transmission electron microscopy (4D-STEM) data. We apply the approach to a lead iridate, PbIrO, and yttrium-stabilized zirconia, YZrO, heterostructure from data acquired with the specimen in a single plan-view orientation, with the epitaxial layers stacked along the beam direction. We demonstrate that Pb–Ir atomic columns are visible in the uppermost layers of the reconstructed volume. We compare this approach to the alternative techniques of depth sectioning using differential phase contrast scanning transmission electron microscopy (DPC-STEM) and multislice ptychographic reconstruction.

47 OTHER INSTRUMENTATION↗

Single-distance nano-holotomography with coded apertures

High-resolution phase-contrast 3D imaging using nano-holotomography typically requires collecting multiple tomograms at varying sample-to-detector distances, usually 3 to 4. This multi-distance approach limits temporal resolution, making it impractical for operando studies. Moreover, shifting the sample complicates reconstruction, requiring precise alignment, registration, and interpolation to correct for shift-dependent magnification on the detector. In response, we propose and validate through simulations a novel, to the best of our knowledge, single-distance approach that leverages coded apertures to structure beam illumination while the sample rotates. Finally, this approach relies on a joint reconstruction scheme, which integrates phase retrieval with 3D tomography, ensuring data consistency and achieving artifact-free reconstructions from a single distance, unlocking dynamic experiments.

Nikitin, Viktor [Argonne National Laboratory (ANL)↗

Robust Atomic-Resolution Imaging of Lithium in Battery Materials by Center-of-Mass Scanning Transmission Electron Microscopy

The performance of energy storage materials is often governed by their structure at the atomic scale. Conventional electron microscopy can provide detailed information about materials at these length scales, but direct imaging of light elements such as lithium presents a challenge. While several recent techniques allow lithium columns to be distinguished, these typically either involve complex contrast mechanisms that make image interpretation difficult or require significant expertise to perform. In this work, we demonstrate how center-of-mass scanning transmission electron microscopy (CoM-STEM) provides an enhanced ability for simultaneous imaging of lithium and heavier element columns in lithium ion conductors. Through a combination of experiments and multislice electron scattering calculations, we show that CoM-STEM is straightforward to perform and produces directly interpretable contrast for thin samples, while being more robust to variations in experimental parameters than previously demonstrated techniques. As a result, CoM-STEM is positioned to become a reliable and facile method for directly probing all elements within energy storage materials at the atomic scale.

25 ENERGY STORAGE↗

Experimental investigation of fuel temperature effects on transient needle motion and injection velocity of solenoid type diesel injector

Real driving emission (RDE) test conducted in sub-zero temperature conditions has been acting as a severe emission regulation over the existing test methods for diesel engines. In order to cope with this tightened regulation, many studies have been conducted to interpret the factors causing the deteriorated diesel engine combustion in cold operation conditions. The deteriorated fuel injection performance has been regarded as one of the key contributing factors but the governing mechanisms are not thoroughly understood so far. This study aims to provide a comprehensive understanding of the effects of fuel temperature including sub-zero conditions on fuel injection performance by measuring the transient needle motion and injection velocity of a diesel injector using synchrotron X-ray imaging techniques. Here, the factors causing the deteriorated injector performance and their contributions are discussed thoroughly based on the results. The results showed that the injection duration was shortened as the fuel temperature decreased as a result of decreased needle opening speed and increased needle closing speed. The increase of fuel viscosity and bulk modulus was discussed as the main factors associated with these results. The total injection mass was reduced by lowering the fuel temperature not only by the shortened injection duration but also by the decreased injection velocity. These factors exerted near equivalent contribution to the reduced injection mass at low fuel temperatures.

42 ENGINEERING↗

Radiation and heat transport in divergent shock–bubble interactions

Shock–bubble interactions (SBIs) are important across a wide range of physical systems. In inertial confinement fusion, interactions between laser-driven shocks and micro-voids in both ablators and foam targets generate instabilities that are a major obstacle in achieving ignition. Experiments imaging the collapse of such voids at high energy densities (HED) are constrained by spatial and temporal resolution, making simulations a vital tool in understanding these systems. In this study, we benchmark several radiation and thermal transport models in the xRAGE hydrodynamic code against experimental images of a collapsing mesoscale void during the passage of a 300 GPa shock. We also quantitatively examine the role of transport physics in the evolution of the SBI. This allows us to understand the dynamics of the interaction at timescales shorter than experimental imaging framerates. We find that all radiation models examined reproduce empirical shock velocities within experimental error. Radiation transport is found to reduce shock pressures by providing an additional energy pathway in the ablation region, but this effect is small (∼1% of total shock pressure). Employing a flux-limited Spitzer model for heat conduction, we find that flux limiters between 0.03 and 0.10 produce agreement with experimental velocities, suggesting that the system is well-within the Spitzer regime. Higher heat conduction is found to lower temperatures in the ablated plasma and to prevent secondary shocks at the ablation front, resulting in weaker primary shocks. Finally, we confirm that the SBI-driven instabilities observed in the HED regime are baroclinically driven, as in the low energy case.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Characterizing the microstructures of mammalian enamel by synchrotron phase contrast microCT

The enamel of mammalian teeth is a highly mineralized tissue that must endure a lifetime of cyclic contact and is inspiring the development of next-generation engineering materials. Attempts to implement enamel-inspired structures in synthetic materials have had limited success, largely due to the absence of a detailed understanding of its microstructure. Here, the present work used synchrotron phase-contrast microCT imaging to evaluate the three-dimensional microstructure of enamel from four mammals including Lion, Gray Wolf, Snow Leopard, and Black Bear. Quantitative results of image analysis revealed that the decussation pattern of enamel consists of discrete diazone (D) and parazone (P) bands of rods organized with stacking arrangement of D+/P/D-/P in all mammals evaluated; the D+ and D- refer to distinct diazone bands with juxtaposed rod orientations from the reference plane. Furthermore, the rod orientations in the bands can be described in terms of two principal angles, defined here as the pitch and yaw. While the pitch angle increases from the outer enamel to a maximum (up to ≈ 40°) near the dentin enamel junction, minimal spatial variations are observed in yaw across the enamel thickness. There are clear differences in the decussation parameters of enamel across species that are interpreted here with respect to the structural demands placed on their teeth. The rod pitch and band width of enamel are identified as important design parameters and appear to be correlated with the bite force quotient of the four mammals evaluated.

36 MATERIALS SCIENCE↗

Development of simplified model for injection rate prediction of diesel injectors during transient and steady operation

Determining the injection rate of the diesel injector during the transient short injection operations is a critical matter to enhance the combustion process by improving air/fuel mixture formation. In this regard, numerous injection models have been suggested in the literature to predict the injection rate accurately. However, such algorithms have not precisely predicted the rate of injection (ROI) in transient short injection events. In addition, most of those models require many input parameters to characterize hydraulic and mechanical subsystems in the injector, which can make them inconvenient to tune for different injector specifications, in other words not suitable for universal usage. Therefore, our study aims to develop a simple injection model that can predict injection rate precisely in the short and long injection durations considering relatively fewer input parameters. The model traces the pressure variation inside the sac based on the bulk modulus theory to predict nozzle exit velocity, thus the injection rate of the injector. In the algorithm, the bulk modulus of fuel (E) and discharge coefficients of the nozzle hole and needle seat (C d,H and C d,N ) have been considered to vary rather than set constant during the injection process since such flow parameters would have a critical impact on the flow development at the transient stage, thus affecting the injection rate of diesel injectors. Here with this modelling strategy, the accuracy of the new model on ROI prediction was confirmed with acceptable model error for both short and long injection durations by validating against experimental results. To understand the effect of the new model scheme on ROI prediction, ROI results with the new model have been discussed by comparing it with the ROI results predicted with constant flow parameters.

42 ENGINEERING↗