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At least 559 records · Page 31

Deformation and fracture behavior of a laser powder bed fusion processed stainless steel: In situ synchrotron x-ray computed microtomography study

Tensile plastic deformation and fracture behavior of a laser powder bed fusion processed 316L stainless steel alloy was investigated in situ using high-resolution synchrotron x-ray computed microtomography (sXCT). Three different cases were studied: (1) specimen A1, near full-density with initial porosity of 0.04%, (2) specimen B1, initial lack-of-fusion (LOF) porosity of about 3% with the major axis of defects aligned nearly perpendicular to the tensile loading direction (LD), and (3) specimen B, similar to B1 but with the major axis of LOF defects aligned nearly parallel to LD. The effects of type, density, and orientation of defects in as-printed samples on plastic deformation and failure modes were studied by analyzing sXCT image sequences and quantitative defect properties. Specifically, the evolutions of porosity, size, aspect ratio, and angle of gas pores and LOF defects were characterized as a function of applied strain. Moreover, interactions between as-printed defects and deformation-induced crack propagation were investigated. The tensile behavior of specimen A1 was comparable to that of a commercial wrought plate. Furthermore, the quantitative in-situ sXCT results showed a void-growth phenomenon in A1 but without noticeable coalescence, resulting in a ductile cup-cone failure. Specimen B1 showed damage-driven brittle failure with limited plasticity due to early and rapid propagation of open voids. On the other hand, specimen B, with a similar amount of LOF defects as B1, showed deceivingly strong and ductile tensile behavior similar to A1 without any major crack propagations due to the favorable orientation relationship between LOF defects and the LD.

36 MATERIALS SCIENCE↗

Toward In Situ Synchrotron Mapping of Crystal Selection Processes during Crystal Growth

In this work, we present an automated and rapid method for non-destructive mapping of crystal grains in a rod-shaped sample. The approach was designed for application to in situ float-zone crystal growth experiments at an x-ray synchrotron source, but could be useful in other applications. The methods have been tested on a TiO 2 boule grown in an optical float zone furnace. The approach applies a statistical filter to polycrystalline diffraction patterns on 2D detectors to rapidly determine the degree of powder-quality 1of the signal. When larger crystals emerge in the growth, their position, size and shape can be tracked using an automated blob-tracking algorithm that follows individual Bragg peaks as a function of position in a grid-scan, even when multiple crystals are contributing spots to diffraction images. This method is found to be robust as the same crystal shape can be independently reconstructed using different sets of Bragg reflections. Image segmentation methods are then used to map out the polycrystalline grains. We also note that other information about crystal quality, such as mosaicity or strain state, may be inferred and mapped from the intensity variation of the Bragg peaks at different locations within the sample.

36 MATERIALS SCIENCE↗

3D Experimental Measurements of Evolution of Force Chains in Natural Silica Sand

The mechanisms of force transmission in granular materials is a classic physics problem that has been addressed since the 19th century, when Heinrich Rudolf Hertz investigated the interaction between two similar objects that were in contact under compression. However, the study of force transmission mechanisms in assemblies of more particles has proven to be a formidable problem due to the complex nature of granular materials. In recent years, synchrotron microcomputed tomography (SMT) and three-dimensional X-ray diffraction microscopy (3DXRD) have been employed to study the mechanics of granular materials experimentally. Combining SMT and 3DXRD offers unique three-dimensional (3D) experimental measurements of the internal structure, kinematics (such as rotation and translation), and lattice strains of individual sand particles. In this paper, in situ SMT and 3DXRD scans were acquired at multiple load steps for a specimen composed of 2,705 natural Ottawa sand particles that were subjected to one-dimensional (1D) confined compression. An algorithm was developed to combine SMT images and 3DXRD lattice strain measurements and used to characterize the constitutive behavior of sand particles. The results were used to identify the crystal structure and the evolution of the stresses and lattice strains of individual sand particles. Another algorithm was developed to characterize the force structures within the specimen. Force structures were identified, and their properties (such as length) and evolution through the experiment were examined. The contact number of particles is a particle-scale property that affects the mechanics of granular materials. The effect of the contact number of the sand particles on the onset and evolution of the force structures was also investigated and discussed.

3D x-ray diffraction microscopy↗

Universal chemomechanical design rules for solid-ion conductors to prevent dendrite formation in lithium metal batteries

Dendrite formation during electrodeposition while charging lithium metal batteries compromises their safety. Although high-shear-modulus ( G s ) solid-ion conductors (SICs) have been prioritized to resolve the pressure-driven instabilities that lead to dendrite propagation and cell shorting, it is unclear whether these or alternatives are needed to guide uniform lithium electrodeposition, which is intrinsically density-driven. Here, we show that SICs can be designed within a universal chemomechanical paradigm to access either pressure-driven dendrite-blocking or density-driven dendrite-suppressing properties, but not both. This dichotomy reflects the competing influence of the SIC’s mechanical properties and the partial molar volume of Li + $(V_{\mathrm{Li}^+})$ relative to those of the lithium anode ( G Li and V Li ) on plating outcomes. Within this paradigm, we explore SICs in a previously unrecognized dendrite-suppressing regime that are concomitantly ‘soft’, as is typical of polymer electrolytes, but feature an atypically low $(V_{\mathrm{Li}^+})$ that is more reminiscent of ‘hard’ ceramics. Li plating (1 mA cm -2 ; T = 20 °C) mediated by these SICs is uniform, as revealed using synchrotron hard X-ray microtomography. As a result, cell cycle life is extended, even when assembled with thin Li anodes (~30 µm) and either high-voltage NMC-622 cathodes (1.44 mAh cm -2 ) or high-capacity sulfur cathodes (3.02 mAh cm -2 ).

25 ENERGY STORAGE↗

Towards scanning nanostructure X-ray microscopy

This article demonstrates spatial mapping of the local and nanoscale structure of thin film objects using spatially resolved pair distribution function (PDF) analysis of synchrotron X-ray diffraction data. This is exemplified in a lab-on-chip combinatorial array of sample spots containing catalytically interesting nanoparticles deposited from liquid precursors using an ink-jet liquid-handling system. A software implementation is presented of the whole protocol, including an approach for automated data acquisition and analysis using the atomic PDF method. The protocol software can handle semi-automated data reduction, normalization and modeling, with user-defined recipes generating a comprehensive collection of metadata and analysis results. By slicing the collection using included functions, it is possible to build images of different contrast features chosen by the user, giving insights into different aspects of the local structure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗

Advanced monolithic 2D multilayer Laue lens (MLL) optics for hard x-ray nanofocusing and nanotomography

We report on the development of a new generation of monolithic two-dimensional (2D) multilayer Laue lens (MLL) optics suitable for high-resolution hard x-ray nanoimaging. The 2D optics were assembled on microfabricated silicon templates with high orthogonality and lateral alignment precision, which were characterized using white-light interferometry and confirmed by x-ray measurements. The developed monolithic 2D MLL optics were successfully employed for hard x-ray nanofocusing and nanotomography experiments using the ptychography imaging modality, demonstrating sub-10 nm resolution in 2D and sample-limited ∼30 nm in three-dimensional while exhibiting excellent stability during extended measurements. The new 2D MLL templates with high alignment accuracy represent an important step forward in the development of 2D MLL optics toward direct nanoimaging experiments with sub-10 nm spatial resolution.

36 MATERIALS SCIENCE↗

Work function lowering of LaB 6 by monolayer hexagonal boron nitride coating for improved photo- and thermionic-cathodes

We report a lowering of work function for lanthanum hexaboride (LaB 6 ) by monolayer hexagonal boron nitride (hBN) coating. Photoemission electron microcopy (PEEM) and thermionic emission electron microscopy (TEEM) both revealed that the hBN coated region of a LaB 6 (100) single crystal has a lower work function compared to the bare (i.e., non-coated) and graphene coated regions. A broad and uniform brighter image of the hBN coated region in PEEM was quantitatively supported by a 0.4 eV decrease in the work function in photoelectron spectra compared to the bare region. TEEM results were consistent in that the hBN coated region exhibited thermionic emission at 905 °C, whereas the bare and graphene coated regions did not. A larger decrease in the work function for hBN coated LaB 6 (100) compared to graphene coated LaB 6 (100) was qualitatively supported by our density functional theory calculations. Adding an oxide layer in the calculations improved consistency between the calculation and experimental results. We followed up our calculations with synchrotron-radiation x-ray photoelectron spectroscopy and confirmed the presence of an oxide layer on our LaB 6 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Galaxy Clusters Discovered via the Thermal Sunyaev-Zel’dovich Effect in the 500-square-degree SPTpol Survey

We present a catalog of 689 galaxy cluster candidates detected at significance ξ > 4 via their thermal Sunyaev-Zel’dovich (SZ) effect signature in 95 and 150 GHz data from the 500-square-degree SPTpol survey. We use optical and infrared data from the Dark Energy Camera and the Wide-field Infrared Survey Explorer (WISE) and Spitzer satellites, to confirm 544 of these candidates as clusters with ~ 94% purity. The sample has an approximately redshift-independent mass threshold at redshift z > 0.25. The confirmed sample spans 1.5 × 10 14 < M 500 c < 9 × 10 14 M ⊙ /h 70 and 0.03 < z ≲ 1.6 in mass and redshift, respectively, with a median mass of 2.5×10 14 M ⊙ /h 70 and median redshift z = 0.7; 21% of the confirmed clusters are at z > 1. We use external radio data from the Sydney University Molonglo Sky Survey (SUMSS) to estimate contamination to the SZ signal from synchrotron sources. The contamination reduces the recovered ξ by a median value of 0.032, or ~ 0.8% of the ξ = 4 threshold value, and ~ 7% of candidates have a predicted contamination greater than Δξ = 1. With the exception of a small number of systems (< 1%), an analysis of clusters detected in single-frequency 95 and 150 GHz data shows no significant contamination of the SZ signal by emission from dusty or synchrotron sources. This cluster sample, representing the deepest SZ-selected cluster sample to date, will be a key component in upcoming astrophysical and cosmological analyses of clusters. In addition to the cluster catalog, we also release the millimeter-wave maps and associated data products used to produce this sample. These maps have depths of 5.3 (11.7) µK CMB -arcmin at 150 (95) GHz and an effective angular resolution of 1. '2 (1. '7). The SPTpol products are available at https:// pole.uchicago.edu/public/data/sptpol_500d_clusters/index.html, and the NASA LAMBDA website. An interactive sky server with the SPTpol maps and Dark Energy Survey data release 2 images is also available at NCSA https://skyviewer.ncsa.illinois.edu.

79 ASTRONOMY AND ASTROPHYSICS↗

PyXAS – an open-source package for 2D X-ray near-edge spectroscopy analysis

In the synchrotron X-ray community, X-ray absorption near-edge spectroscopy (XANES) is a widely used technique to probe the local coordination environment and the oxidation states of specific elements within a sample. Although this technique is usually applied to bulk samples, the advent of new synchrotron sources has enabled spatially resolved versions of this technique (2D XANES). This development has been extremely powerful for the study of heterogeneous systems, which is the case for nearly all real applications. However, associated with the development of 2D XANES comes the challenge of analyzing very large volumes of data. As an example, a single 2D XANES measurement at a synchrotron can easily produce ~106 spatially resolved XANES spectra. Conventional manual analysis of an individual XANES spectrum is no longer feasible. Here, a software package is described that has been developed for high-throughput 2D XANES analysis. A detailed description of the software as well as example applications are provided.

25 ENERGY STORAGE↗

Collimated phase measuring deflectometry II: Re-design of the optical layout for high-curvature surfaces

Collimated phase measuring deflectometry (CPMD) is an optical metrology technique developed to improve upon traditional phase measuring deflectometry (PMD). CPMD utilizes telecentric imaging and collimated structured light illumination to eliminate the height-slope ambiguity present in traditional PMD measurements. After the publication of the first CPMD paper, efforts began to optimize the optical layout of the CPMD system. The first proposed change, and the one detailed in this work, was to move the Fourier transform (FT) lens closer to the surface under test (SUT). Moving the FT lens closer to the SUT meant that for a given FT lens diameter, a larger range of surface slopes on the SUT could be measured. This change to the optical layout was not trivial and introduced at least two concerns that had to be addressed: telecentricity in the imaging path and possible ghost reflections from the re-located FT lens. Here, in this work, we examine how these concerns were addressed and present results showing that the revised optical layout is capable of measurement results at least as good as the original CPMD optical layout. We also demonstrate the increased slope measuring range of the revised optical layout.

47 OTHER INSTRUMENTATION↗

High-energy X-ray imaging with a Germanium MM-PAD hybrid pixel detector

Germanium is a high-Z sensor material with excellent energy resolution and attractive properties for high-energy photon detection. Despite its advantages, the need for cryogenic operation and challenges in the fabrication of pixelated high-purity germanium have hindered the development of segmented detectors. We report on the fabrication and performance of a germanium imaging detector with 150 μm pixel pitch hybridized to the MM-PAD ASIC. The detector was capable of high-resolution radiographic imaging and has a fast temporal response. Additionally, we describe the detector's upper operating temperature limits using both the MM-PAD and MARS ASICs, achieving stable operation up to 130 K and 190 K, respectively.

36 MATERIALS SCIENCE↗

Synthesis and Properties of Bulk Mg 3 WN 4 in a Wurtzite-Derived Structure

Experimental synthesis of theoretically predicted materials with controlled elemental coordination environments can lead to the realization of useful properties, such as facile ion transport or ferroelectric switching. Among such materials are ternary nitrides in the Mg−W−N composition space, where several stable and metastable compounds have been predicted and synthesized recently in bulk and film forms. Here, we report for the first time on the bulk synthesis of Mg 3 WN 4 in a wurtzite-derived crystal structure via a solid-state metathesis reaction. In situ synchrotron powder X-ray diffraction shows how the ion exchange proceeds from Li 6 WN 4 + MgCl 2 precursors to Mg 3 WN 4 + LiCl products, with the reaction starting slowly near 380 °C and completing by 600 °C, including the presence of a competing disordered rocksalt-derived phase (Mg,W)N above 440 °C. The follow-up ex situ powder synthesis at 400 °C for 0.5 h with 10% excess MgCl 2 reveals the cation-ordered nature of the wurtzite-derived Mg 3 WN 4 structure with polar symmetry confirmed by second-harmonic generation measurements. Optical absorption spectra, chemical composition analysis, and electron microscopy imaging suggest that bulk Mg 3 WN 4 obtained via metathesis reaction is prone to defect formation. Overall, this study shows that selective ex situ synthesis of the phase-pure ternary nitrides, informed by in situ measurements, is possible by carefully controlling the thermal budget of the reaction and paves the way toward property characterization of the Mg 3 WN 4 wurtzite-derived material.

36 MATERIALS SCIENCE↗

Considerations about future hard x-ray area detectors

X-ray sources continue to advance in both intensity and temporal domains, thereby opening new ways to analyze the structure and properties of matter, provided that the resultant x-ray images can be efficiently and quantitatively recorded. In this perspective we focus on specific limitations of pixel area x-ray detectors. Although pixel area x-ray detectors have also advanced in recent years, many experiments are still detector limited. Specifically, there is need for detectors that can acquire successive images at GHz rates; detectors that can accurately measure both single photon and millions of photons per pixel in the same image at frame rates of hundreds of kHz; and detectors that efficiently capture images of very hard x-rays (20 keV to several hundred keV). The data volumes and data rates of state-of-the-art detection exceeds most practical data storage options and readout bandwidths, thereby necessitating on-line processing of data prior to, or in lieu of full frame readouts.

36 MATERIALS SCIENCE↗

Passive Freeze-Out of the Richtmyer-Meshkov Instability

The Richtmyer-Meshkov instability (RMI) poses a major challenge in inertial confinement fusion (ICF) due to its role in mixing and performance degradation. We report the first experimental observation of passive freeze-out of RMI in a low-pressure surrogate regime, an instability stagnation effect induced without modifying the driving pressure pulse or the target surface geometry. Using additively manufactured subsurface voids in a sinusoidal target, we convert a single shock into a sequence of weaker shocks that suppress instability growth upstream of the surface by over 70%. High-speed x-ray imaging and hydrodynamic simulations suggest that this suppression arises primarily from temporal shaping, with lesser contributions from spatial curvature and shock weakening. Our results demonstrate a driver-independent pathway for controlling shock-driven hydrodynamic instabilities relevant to ICF and other high energy density systems.

Materials science↗

Towards a new generation long trace profiler LTP-2020: optical design of pencil beam interferometry sensor

Improvements in the quality of synchrotron beamline x-ray optics required for next-generation light sources (e.g. the ALS Upgrade project) drive the need to improve the performance of the metrology instrumentation used to measure these components. The Long Trace Profiler (LTP) that is in use at many synchrotron metrology laboratories around the world has some known issues that affect the accuracy of its measurements. The main error source is optical path difference (OPD) phase error introduced into the probe beam by inhomogeneities in the glass components used in the optical head. We have developed a new optical head design, LTP-2020, that replaces the cube polarizing beamsplitter (PBS) with a thin wedge plate polarizing beamsplitter (WPBS) and replaces the cemented doublet lens with an aspheric singlet. Both of these components significantly reduce the glass volume traversed by the laser probe beam. Careful attention to ghost ray interference produced by back reflection from optical surfaces is necessary to minimize distortion in the primary image that translates into systematic error in the slope angle measurement. We make extensive use of a commercial raytracing program to model the back reflections and adjust component parameters as necessary to minimize distortion. Deliberate misalignment of components is necessary to make the system perform correctly. Stringent requirements are placed on the 45◦ incidence coatings on the WPBS and on the normal incidence coatings on the lens and camera window elements. We encourage our colleagues who wish to upgrade their current LTP systems to join us in the procurement of these custom optical components.

Takacs, Peter Z.↗

Magnetic field driven emergent phenomena: Insights from magneto-optics and nanoscopy

This review explores magnetic field-driven emergent phenomena across various material systems, emphasizing the pivotal roles of magneto-optical and nanoscopy techniques. We examine fundamental aspects of Landau electrodynamics in both 2D and 3D systems, including quantum Hall and topological magnetoelectric effects in graphene and topological insulators. Particularly attention is given to magnetic excitations and magnetopolaritons, such as surface magnon polaritons, magnetoplasmons, and magnetoexcitons in novel quantum materials, including quantum magnets and hybrid heterostructures. Advanced imaging techniques, such as scattering-type scanning near-field optical microscopy (SNOM) and microwave impedance microscopy, are showcased for their capability to resolve these phenomena with microscopic and nanoscopic resolution. These insights are complemented by discussions of advanced experimental approaches, including cryogenic environments, ultrafast pump-probe techniques, and the integration of magnetic fields into near-field optical methodologies. We further investigate the potential of these imaging techniques for unraveling complex magnetic orders, quantum phases, and correlated electronic behaviors. Finally, we offer perspectives on future research directions and highlight emerging opportunities in the evolving field of optical magneto-nanoscopy.

36 MATERIALS SCIENCE↗

Using multimodal X-ray computed tomography to advance 3D petrography: A non-destructive investigation of olivine inside a carbonaceous chondrite

Rocks form in three dimensions through time and studying them provides information from inside dynamic systems we cannot otherwise observe. Yet how we typically access the interior of the rocks themselves to gain that information may limit our understanding and influence how we reconstruct the processes that formed them. Here, we demonstrate combined non-destructive 3D X-ray imaging techniques that produce quantitative densitometric and crystallographic maps of entire individual grains inside a rock. Olivine grains throughout a sample of the carbonaceous chondrite Northwest Africa (NWA) 11346 were each characterized by size, shape, composition, zoning intensity, and crystallographic orientation. The addition of 3D crystallographic mapping to calibrated 3D densitometric analysis—used to calculate chemical composition—demonstrates a fully non-destructive petrographic method and provides unique insight. For instance, in our case, using crystallographic data to delineate individual grains and then measuring the 3D size, shape, and composition of each distinguishes variably reset relict grains from those later crystallized after a melting event. Intersection in a 2D slice could not have led to this interpretation because the integration of three-dimensional size, rounding, composition, location, and crystallographic orientation measured from each grain forms the key patterns. Multimodal laboratory X-ray imaging has strong potential to advance 3D petrography.

36 MATERIALS SCIENCE↗