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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

High-throughput, in situ imaging of multi-layer powder-blown directed energy deposition with angled nozzle

Laser metal additive manufacturing (AM) has become an increasingly popular technology due to its flexibility in geometry and materials. As one of the commercialized additive processes, powder-blown directed energy deposition (DED) has been used in multiple industries such as aerospace, automotive, medical device, etc. However, a lack of fundamental understanding remains for this process, and many opportunities for alloy development and implementation can be identified. A high-throughput, in situ DED system capable of multi-layer builds that can address these issues is presented here. In this work, implications of layer heights and energy density are investigated through an extensive process parameter sweep, showcasing the power of a high-throughput setup while also discussing multi-layer interactions.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Twinning-mediated anomalous alignment of rutile films revealed by synchrotron X-ray nanodiffraction

Nanotwin structures in materials engender fascinating exotic properties. However, twinning usually alter the crystal orientation, resulting in random orientation and limited performances. Here, we report a well-aligned rutile TiO 2 nanotwin film with superior preferential orientation than its isostructural substrate. By means of the synchrotron X-ray Laue nanodiffraction technique, the crystal orientation, twin boundaries, and deviatoric stresses of the film were quantitatively imaged at unprecedented spatial resolution to unravel the underlying mechanism of this anomalous alignment. Massive {101}-type rutile nanotwins were observed, and a crystallographic relationship of the heteroepitaxy was proposed. The rapid twinning and twin-controlled heteroepitaxy are responsible for the texture improvement. This work would open up opportunities for rational design of better twin-based functional materials, and implies the powerful capabilities of X-ray nanodiffraction technique for multidisciplinary applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

IRIXS Spectrograph: an ultra high-resolution spectrometer for tender RIXS

The IRIXS Spectrograph represents a new design of an ultra-high-resolution resonant inelastic X-ray scattering (RIXS) spectrometer that operates at the Ru L 3 -edge (2840 eV). First proposed in the field of hard X-rays by Shvyd'ko [(2015), Phys. Rev. A, 91, 053817], the X-ray spectrograph uses a combination of laterally graded multilayer mirrors and collimating/dispersing Ge(111) crystals optics in a novel spectral imaging approach to overcome the energy resolution limitation of a traditional Rowland-type spectrometer [Gretarsson et al. (2020), J. Synchrotron Rad. 27, 538–544]. In combination with a dispersionless nested four-bounce high-resolution monochromator design that utilizes Si(111) and Al 2 O 3 (110) crystals, an overall energy resolution better than 35 meV full width at half-maximum has been achieved at the Ru L 3 -edge, in excellent agreement with ray-tracing simulations.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2025

Chemical speciation correlated with microstructural heterogeneity of interdicted uranium materials

Two uranium powders seized by law enforcement in Victoria, Australia, have been characterized by established nuclear forensic methods in a previously published study. Here, in this work, the results of further characterization by a scanning transmission x-ray microscope (STXM) operating in the soft x-ray regime are reported. STXM images are used to estimate the elemental distribution in micrometer-scale particles of each powder, and oxygen K-edge absorption spectra are used to determine the chemical state of uranium. The results of the current study are consistent with the previous analysis; the first powder is found to be a potassium-uranium hydrate, while the second powder is determined to be a mixture of uranium oxides primarily consisting of UO 3 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2020

Magnetic Field Optimization of an In-Vacuum Undulator at NSLS-II Transactions on Applied Superconductivity

A 3.0 m long In-Vacuum Undulator (IVU) is employed at the National Synchrotron Light Source II (NSLS-II) for the Hard X-ray Nanoprobe (HXN) beamline providing structural and X-ray fluorescence imaging with world-leading spatial resolution. On July 1 st 2018 a gearbox shaft in the gap drive train assembly sheared due to corrosion fatigue caused by stress due to mechanical misalignment. Furthermore, the device was extracted from the storage ring and measured. The magnetic field measurements detected a degradation of the magnetic performance as well as a localized demagnetization of the magnetic modules of the first 3 upstream periods. We describe here the mechanical repairs and the magnetic phase shimming optimization implemented to restore the spectral performance of the device.

43 PARTICLE ACCELERATORS↗
DOE OSTI2026

Evaluation of an event-driven 3FI ASIC for spectroscopic X-ray detection with synchrotron radiation

The novel design and evaluation on the NSLS-II beamline of the 3FI application-specific integrated circuit (ASIC) bump-bonded to a simple, planar, 2D segmented silicon sensor are presented. The ASIC was developed for full-field fluorescence spectral X-ray imaging (3FI). It is a small-scale prototype that features a square array of 32 × 32 pixels, and the size of the pixels is 100 µm × 100 µm. The ASIC was implemented in a 65 nm CMOS integrated circuit fabrication process. Each pixel incorporates a charge-sensitive amplifier, a shaping filter, a discriminator, a peak detector and a sample-and-hold circuit, allowing detection of events and storage of signal amplitudes. The system operates in a frameless event-driven readout mode, outputting analog values for threshold-triggered events, allowing high-speed multi-element X-ray fluorescence data acquisition. The 3FI ASIC achieves per-channel spectrometric performance at a power consumption of only 200 µW per pixel, with nearly all dissipation confined to the analog front-end. An energy resolution is measured at the level of 308 eV full width at half-maximum (FWHM) at 8.04 keV (Cu Kα), and 138 eV FWHM at 3.69 keV (Ca Kα). This per-pixel capability makes the prototype suitable for in situ trace element microanalysis in biological and environmental studies. Moreover, the frameless architecture of the detector is designed to address limitations of conventional X-ray fluorescence microscopy, which typically requires mechanical scanning, by enabling continuous high-throughput data acquisition in future full-field implementations.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Ultimate brightness of a medium-energy synchrotron light source at operational beam intensity

Synchrotron light sources are key instruments of modern science, providing unique opportunities for groundbreaking studies in diverse scientific disciplines and driving innovation in numerous scientific and technological fields. Fourth-generation light sources provide unprecedented capabilities in imaging, spectroscopy and diffraction techniques. Ultimate brightness is the key to advancing to a smaller scale, faster response, and higher data measurement and processing rate. The brightness is primarily determined by the electron beam emittance and energy spread at operational intensity. A common feature of fourth-generation synchrotrons is the short length of the electron bunches combined with a very small transverse beam size. Consequently, the high particle density leads to strong collective effects that significantly increase the emittance and limit the achievable brightness at operational beam intensity. In this article, we summarize our studies of the emittance and brightness scaled with the beam energy and intensity, taking into account the effects of intrabeam scattering, beam-impedance interaction and bunch lengthening provided by higher-harmonic RF systems to identify optimal combinations of machine and beam parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Synchrotron-based X-ray fluorescence microscopy mapping the ionome of a toxic freshwater cyanobacterium

Harmful algal blooms (HABs) pose a major environmental concern across the globe. In abundance, cyanobacteria, or so-called green-blue algae can produce extremely dangerous cyanotoxins that harm humans and animals. This study focused on the mapping and distribution of intracellular macro-and micronutrients of the widespread freshwater cyanobacteria Microcystis aeruginosa (M. aeruginosa). Towards a better understanding of trace metal uptake and homeostasis throughout the cell cycle, we quantitatively mapped the spatial distribution of the elements P, K, Fe, Ca, Zn, Mn, and Cu across the ultrastructure of frozen-hydrated single cells using state-of-theart X-ray nanofluorescence imaging at the Advanced Photon Source (APS) at Argonne National Laboratory. Further, bulk cellular nutrient and trace metal content correlated well with the total intracellular elemental content in individual cells obtained by quantitative synchrotron X-ray fluorescence measurements. Multi-dimensional mappings showed P and K atoms colocalized as discrete semicircular hotspots that were analyzed with respect to their stoichiometry. Elevated Cu and Ca concentrations were detected along division plane of cells. P and K were found to have similar spatial elemental distribution with about 65% and 69% of the total cellular P and K, respectively, located at the hotspots. The P and K colocalization were refined further using nanotomography, showing a K envelope surrounding the P core. Inorganic P and organic P compounds were specified using solution-state 31 P nuclear magnetic resonance (NMR) spectroscopy from M. aeruginosa. Of the total extracted P determined by 31 P NMR spectroscopy, 47% were found to be nucleotides while only 11% were polyphosphates. Multimodal X-ray imaging provides a better understanding of intracellular biochemical processes in cyanobacteria, helping us monitor and combat an emerging environmental threat.

31P NMR spectroscopy↗
DOE OSTI2024

Deep learning approaches for instantaneous laser absorptance prediction in additive manufacturing

Abstract The quantification of absorbed light is essential for understanding laser-material interactions and melt pool dynamics in order to minimize defects in additively manufactured metal components. The geometry of a vapor depression formed during laser melting is closely related to laser energy absorption. This relationship has been observed by the state-of-the-art in situ high-speed synchrotron X-ray visualization and integrating sphere radiometry. These two techniques create a temporally resolved dataset consisting of vapor depression images and corresponding laser absorptance. In this work, we propose two different approaches to predict instantaneous laser absorptance. The end-to-end approach uses deep convolutional neural networks to learn implicit features of X-ray images automatically and predict the laser energy absorptance. The two-stage approach uses a semantic segmentation model to engineer geometric features and predict absorptance using classical regression models. While having distinct advantages, both approaches achieved a consistently low mean absolute error of less than 3.3%.

Chemistry↗
DOE OSTI2026

Hard X-ray imaging with sub-10 nm resolution by scanning bonded 2D multilayer Laue lenses

Multilayer Laue lenses (MLLs) offer significant advantages over traditional diffractive focusing optics, such as zone plates (ZPs), in terms of efficiency and durability when focusing hard X-rays to 10 nm and below. Typically, a pair of 1D MLLs is aligned independently to achieve point focusing. This approach only permits scanning microscopy by moving the sample stage, which presents a limitation when it comes to scanning large or bulky objects at high speed. In this study, we present an experimental demonstration of scanning monolithically bonded 2D MLLs while keeping the sample stationary, effectively addressing the limitation of the sample’s size and weight. We characterized the system’s positional and angular stabilities during scanning, which are critical parameters to the nanofocusing performance of MLLs. In addition, we provided the X-ray measurement results and corresponding image resolution analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Bulk modulus measurement at mHz frequencies and high-pressure using synchrotron x-ray radiation

We report an experimental protocol for measuring the frequency dependence of the bulk modulus carried out in a synchrotron x-ray facility based multi-anvil high-pressure apparatus. An oscillating pressure perturbation characterized by x-ray diffraction produces a volume strain measured by imaging. Together, these yield the bulk modulus of the sample. In this work, we report data at 3 mHz as an example of the possibility of providing these data for the frequency range of 1 mHz–100 mHz.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Dynamic in-situ imaging of methane hydrate formation and self-preservation in porous media

Here we present the results of dynamic in-situ 3D X-ray imaging of methane hydrates microstructure during methane hydrate formation and dissociation in sand samples. Short scanning times and high resolution provided by synchrotron X-rays allowed for better understanding of water movement and different types of gas-hydrate formation. Complementing previous observations, we conclude that the process of gas-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 (when the water is immobile). Based on the 3D microstructure we identified two distinct types of gas-hydrate formation: (i) into the gas pockets and (ii) inside water volumes. For both mechanisms we do not see problems in gas or water supply to support the gas-hydrate formation. The rate of dissociation in the self-preservation mode (pressure drop at negative temperatures) appears to be different for these two types of gas hydrates. This means that the history of the gas-hydrate formation may influence its behaviour at the dissociation stage (e.g. gas-hydrate production).

58 GEOSCIENCES↗
DOE OSTI2020

Multiprincipal Component P2-Na 0.6 (Ti 0.2 Mn 0.2 Co 0.2 Ni 0.2 Ru 0.2 )O 2 as a High-Rate Cathode for Sodium-Ion Batteries

Mixing transition metal cations in nearly equiatomic proportions in layered oxide cathode materials is a new strategy for improving the performances of Na-ion batteries. The mixing of cations not only offers entropic stabilization of the crystal structure but also benefits the diffusion of Na ions with tuned diffusion activation energy barriers. In light of this strategy, a high-rate Na 0.6 (Ti 0.2 Mn 0.2 Co 0.2 Ni 0.2 Ru 0.2 )O 2 cathode was designed, synthesized, and investigated, combining graph-based deep learning calculations and complementary experimental characterizations. This new cathode material delivers high discharge capacities of 164 mA g –1 at 0.1 C and 68 mAh g –1 at a very high rate of 86 C, demonstrating an outstanding high rate capability. Ex situ and operando synchrotron X-ray diffraction were used to reveal the detailed structural evolution of the cathode upon cycling. Using the climbing-image nudged elastic-band calculation and Ab initio molecular dynamics simulations, we show that the optimal transition metal composition enables a percolating network of low barrier pathways for fast, macroscopic Na diffusion, resulting in the observed high rate performance.

25 ENERGY STORAGE↗
DOE OSTI2022

Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)

Dark and clear silicate glasses formed during an iron age vitrification event ≈ 1500 years ago at the Broborg hillfort near Uppsala, Sweden have been analyzed using a scanning electron microscope equipped with a micro-X-ray fluorescence (μXRF) spectrometer. Correlated µXRF and electron beam-induced energy dispersive spectrometry (EDS) X-ray maps were collected via stage-scanning at constant velocity. This coupled procedure represents a new approach for the cultural heritage community to conduct analytical studies of archaeometric specimens composed of metal, ceramic, or mixed inorganic/organic materials, where major and trace element compositions are registered in space for areas up to the centimeter-length scale at micrometer-scale resolution. Overview images were used to select areas for EDS beam scan maps correlated with multispectral cathodoluminescence (CL) imaging and co-located quantitative EDS and μXRF point analysis. Fe, Ca, Mg, Ti, P, Mn, Zr, Zn, and Y are enriched in the dark glass, while Si, Al, K, Na, Ba, Sr, Rb, and Ga are enriched in the clear glass. Unmelted material is comprised predominately of quartz (SiO 2 ) along with trace apatite (Ca 5 (PO 4 ) 3 [Cl,OH]) and zircon (ZrSiO 4 ). Multivariate statistical analysis was used to measure the area fractions of high variance components while lower variance components represented phase mixtures. Differences between calculated melt viscosities for the glass compositions are consistent with field and laboratory observations. Coupled large area EDS and μXRF imaging shows significant promise for informed selection of higher spatial resolution and higher sensitivity follow-up studies, e.g., those performed using synchrotron analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Developing in-situ capabilities for synchrotron light source relevant to PNNL mission research areas

The main objective of the proposed research is to engage synchrotron light source capabilities to address the critical mission areas at PNNL. We have carried out Multi-model chemical analysis and imaging to unravel the role of surface chemistry during realistic heterogeneous interfacial processes - through a close collaboration that will help BES and BER research projects. In particular, we performed the following activities to understand role of surface chemistry on metal and oxide reactivity and metal ion transfer across oxide surface and aqueous solutions: 1) Perform light source experiments utilizing samples generated at PNNL; 2) Develop early career PNNL scientists utilizing light sources; 3) Build collaborations with ALS scientists in developing new in-situ capabilities; 4) Complete AMBER capabilities in collaboration with ALS scientists and make those available to the scientific community including PNNL scientists.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Hyperspectral X-ray Imaging with TES Detectors for Nanoscale Chemical Speciation Mapping

We are developing an imaging capability (“Hyperspectral X-ray Imaging”) for mapping chemical information (molecular formula, phase, oxidation state, hydration) that is based on ultra-high-resolution X-ray emission spectroscopy with large transition-edge sensor microcalorimeter arrays in the scanning electron microscope. By combining microcalorimeter arrays with hundreds of pixels, high-bandwidth microwave frequency-division multiplexing, and fast digital electronics for near real-time data processing, our goal is to enable measurements using laboratory-scale instrumentation rather than synchrotron beamlines. Our application focus here is on mapping the chemical form of uranium compounds on the nanoscale. Furthermore, we will present our approach to developing the Hyperspectral X-ray Imaging capability, progress toward a 128-pixel microwave multiplexed X-ray fluorescence instrument at LANL, and the path to high-throughput nanoscale chemical mapping.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Synchrotron X-ray-induced Synthesis of Copper Hydroxide Nitrate Nanoplates on Cu Thin Films in an Ambient Atmosphere

Synchrotron X-rays are widely used for material characterizations. However, they can also ionize atoms and molecules to damage and manipulate probed materials. We report here an X-ray-induced growth of copper hydroxide nitrate, Cu 2 (OH) 3 NO 3 , on copper thin films in the ambient atmosphere without solvents and thermal treatment. In situ synchrotron X-ray diffraction measurements showed that the time-dependent growth process of the Cu 2 (OH) 3 NO 3 is accompanied by the consumption of Cu metal and can be described by a sigmoidal model. The growth rate was reduced after the initial fast growth period. Scanning electron microscopy (SEM) images show that the isolated islands of Cu 2 (OH) 3 NO 3 nanoplates formed in the beginning, which grew together with new nanoplates formed under continued X-ray irradiation. The result demonstrated that high-flux synchrotron X-rays may provide an unconventional approach to synthesizing and manipulating materials, which will inspire future investigation both experimentally and theoretically.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Operando X-ray imaging reveals size-dependent evolution of cobalt oxide thermochemical material during thermal redox cycles

Multivalent metal oxides are promising thermochemical materials (TCMs) for energy storage and conversion owing to their high energy density, air compatibility, and high-temperature stability. Co 3 O 4 serves as a model system for examining particle-size- and structure-dependent redox behavior. While particle size and porosity are known to affect performance, their interplay and the kinetics of pore formation during cycling remain unclear. Here we show the chemical and 3D morphological evolution of Co 3 O 4 micro- and nanoparticles during redox cycles at 800–900 °C using thermal analysis, in-situ synchrotron transmission X-ray microscopy (TXM), and scanning electron microscopy. Thermal analysis shows that nanoparticles re-oxidize more rapidly than microparticles at 800 °C. In-situ nanotomography and chemical imaging reveals that nanoparticles undergo redox conversion without forming internal pores, whereas microparticles develop isolated porosity during reduction. These pores persist through re-oxidation, correlating to a lower conversion rate in subsequent cycles. Our results demonstrate distinct degradation kinetics in Co 3 O 4 micro- and nanoparticles, underscoring the critical role of particle size and porosity in redox performance and informing strategies to enhance the long-term efficiency of metal oxide TCMs.

25 ENERGY STORAGE↗