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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 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Iron and iron-bound phosphate accumulate in surface soils of ice-wedge polygons in arctic tundra

Phosphorus (P) is a limiting or co-limiting nutrient to plants and microorganisms in diverse ecosystems that include the arctic tundra. Certain soil minerals can adsorb or co-precipitate with phosphate, and this mineral-bound P provides a potentially large P reservoir in soils. Iron (Fe) oxyhydroxides have a high capacity to adsorb phosphate; however, the ability of Fe oxyhydroxides to adsorb phosphate and limit P bioavailability in organic tundra soils is not known. In this study, we examined the depth distribution of soil Fe and P species in the active layer (<30 cm) of low-centered and high-centered ice-wedge polygons at the Barrow Environmental Observatory on the Alaska North Slope. Soil reservoirs of Fe and P in bulk horizons and in narrower depth increments were characterized using sequential chemical extractions and synchrotron-based X-ray absorption spectroscopy (XAS). Organic horizons across all polygon features ( e.g. , trough, ridge, and center) were enriched in extractable Fe and P relative to mineral horizons. Soil Fe was dominated by organic-bound Fe and short-range ordered Fe oxyhydroxides, while soil P was primarily associated with oxides and organic matter in organic horizons but apatite and/or calcareous minerals in mineral horizons. Iron oxyhydroxides and Fe-bound inorganic P (P i ) were most enriched at the soil surface and decreased gradually with depth, and Fe-bound P i was >4× greater than water-soluble P i . These results demonstrate that Fe-bound P i is a large and ecologically important reservoir of phosphate. We contend that Fe oxyhydroxides and other minerals may regulate P i solubility under fluctuating redox conditions in organic surface soils on the arctic tundra.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Measurements of source emittance and beam coherence properties of the upgraded Advanced Photon Source

The Advanced Photon Source (APS) has been upgraded with a multi-bend achromat lattice, achieving significantly reduced electron beam emittance and enhanced X-ray coherence. Precise characterization of these properties is essential for optimizing beamline performance and enabling new experiments that take full advantage of the upgraded source. We report on measurements of source size and transverse coherence properties using grating interferometry at two beamlines: the APS 3-ID-B undulator beamline and the 1-BM-B bending magnet beamline. The results confirm the world-record horizontal emittance of the upgraded APS below 30 pm rad and validate the theoretical design parameters. We further investigate the impact of optical aberrations and mechanical vibrations at the 12-ID-C beamline on coherence preservation. These measurements establish a benchmark for future beamline enhancements and demonstrate the effectiveness of grating interferometry for high-precision beam characterization. Our findings provide critical insights into synchrotron beam dynamics, coherence degradation mechanisms, and strategies for optimizing beamline X-ray optics at next-generation light sources.

Advanced Photon Source↗
DOE OSTI2026

Linking Domain Structure Evolution at a Grain Boundary to Piezoelectric Response via Nano‐Diffraction

Electric-field-induced domain structure switching in a 1 𝜇⁢m -thick Pb 0.99 (Zr 0.45 Ti 0.55 ) 0.98 Nb 0.02 O 3 (Nb-doped PZT) bicrystal film was characterized in situ via nano-focused synchrotron diffraction. The epitaxial film was deposited on a (100) SrTiO 3 bicrystal substrate. The changes in domain structure were mapped within a 5 𝜇⁢m × 5 𝜇⁢m area at and around an in-plane tilt-type (23.6°) grain boundary with 50 nm spatial resolution. Rocking curves collected at each point of the mapped area provided the ability to reconstruct spatially-varying three-dimensional (3D) reciprocal space maps around the grain boundary. The 3D reciprocal space maps reveal how different tilted 𝑎 -type domain variants interact with the grain boundary as a function of increasing electric field. Initially, a subset of 𝑎 -type domain variants with their polarization vectors largely orthogonal to the grain boundary were found in greater abundance within 570 nm of the grain boundary, possibly due to X-ray beam-induced local increases in the electrical conductivity, but after the coercive field was exceeded, reconfiguration of the ferroelastic domains was observed. The spatially-varying reciprocal space maps also facilitated evaluation of the strain field across the mapped area, along with 𝑑 33,𝑓 . Significant spatial heterogeneity of strain and 𝑑 33,𝑓 are observed, especially at the coercive field, which was attributed to maintaining deformation compatibility and correlated ferroelastic switching.

36 MATERIALS SCIENCE↗
DOE OSTI2021

How Austenitic Is a Martensitic Steel Produced by Laser Powder Bed Fusion? A Cautionary Tale

Accurate phase fraction analysis is an essential element of the microstructural characterization of alloys and often serves as a basis to quantify effects such as heat treatment or mechanical deformation. Additive manufacturing (AM) of metals, due to the intrinsic nonequilibrium solidification and spatial variability, creates additional challenges for the proper quantification of phase fraction. Such challenges are exacerbated when the alloy itself is prone to deformation-induced phase transformation. Using commonly available in-house X-ray diffraction (XRD) and electron backscatter diffraction (EBSD) and less commonly used synchrotron-based high-energy X-ray diffraction, we characterized nitrogen-atomized 17-4 precipitation-hardening martensitic stainless steel, a class of AM alloy that has received broad attention within the AM research community. On the same build, our measurements recovered the entire range of reported values on the austenite phase fractions of as-built AM 17-4 in literature, from ≈100% martensite to ≈100% austenite. Aided by Calphad simulation, our experimental findings established that our as-built AM 17-4 is almost fully austenitic and that in-house XRD and EBSD measurements are subject to significant uncertainties created by the specimen’s surface finish. Hence, measurements made using these techniques must be understood in their correct context. Our results carry significant implications, not only to AM 17-4 but also to AM alloys that are susceptible to deformation-induced structure transformation and suggest that characterizations with less accessible but bulk sensitive techniques such as synchrotron-based high energy X-ray diffraction or neutron diffraction may be required for proper understanding of these materials.

17-4 steel↗
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 OSTI2023

Ultrahigh‐Flux X‐ray Detection by a Solution‐Grown Perovskite CsPbBr 3 Single‐Crystal Semiconductor Detector

Abstract Solution‐processed perovskites are promising for hard X‐ray and gamma‐ray detection, but there are limited reports on their performance under extremely intense X‐rays. Here, a solution‐grown all‐inorganic perovskite CsPbBr 3 single‐crystal semiconductor detector capable of operating at ultrahigh X‐ray flux of 10 10 photons s −1 mm −2 is reported. High‐quality solution‐grown CsPbBr 3 single crystals are fabricated into detectors with a Schottky diode structure of eutectic gallium indium/CsPbBr 3 /Au. A high reverse‐bias voltage of 1000 V (435 V mm − 1 ) can be applied with a small and stable dark current of ≈60–70 nA (≈9–10 nA mm − 2 ), which enables a high sensitivity larger than 10 000 µC Gy air −1 cm − 2 and a simultaneous low detection limit of 22 nGy air s − 1 . The CsPbBr 3 semiconductor detector shows an excellent photocurrent linearity and reproducibility under 58.61 keV synchrotron X‐rays with flux from 10 6 to 10 10 photons s − 1 mm − 2 . Defect characterization by thermally stimulated current spectroscopy shows a similar low defect density of a synchrotron X‐ray and a lab X‐ray irradiated device. Solid‐state nuclear magnetic resonance spectroscopy suggests that the excellent performance of the solution‐grown CsPbBr 3 single crystal may be associated with its good short‐range order, comparable to the spectrometer‐grade melt‐grown CsPbBr 3 .

Pan, Lei↗
DOE OSTI2020

Characterization of Rare-earth Doped Thermal Barrier Coatings for Phosphor Thermometry

Thermal Barrier Coatings have been extensively used to protect and insulate the metallic components in turbine engines from extreme environments to achieve higher turbine inlet temperatures, resulting in an increase in combined engine cycle efficiency, lowering NOx emissions and fuel consumption. Additionally, as the major failure mechanisms determining lifetime are thermally activated during engine operation, uncertainty in temperature measurements affects lifetime prediction. Early detection of Thermal Barrier Coatings spallation symptoms, associated with local delamination induced temperature changes, can reduce forced engine outages. Further improvements are envisioned with the development of more reliable measurement techniques. For this purpose, Phosphor Thermometry has been considered a promising method for precision monitoring of turbine blade coatings that contain embedded phosphor dopants. In this work, a modified four-flux Kubelka-Munk model for luminescent rare-earth doped Thermal Barrier Coating configurations supported the design and the fabrication of viable sensing coatings for potential industrial implementation. Phosphor Thermometry instrumentation was developed with the objective of expanding capabilities of the technique, using a synchronized acquisition method on sensing coatings. Experiments on an innovative Erbium-Europium co-doped Yttria-Stabilized Zirconia coating have demonstrated the effectiveness of this advanced Phosphor Thermometry instrument with enhanced sensitivity and extended temperature range. Delamination progression monitoring was achieved for the first time using a Thermal Barrier Coating configuration subjected to indentation that includes a thin luminescent layer deposited on the surface and associating the multi-layer configuration with a predictive model that evaluates the advancement of the degradation of the coatings. To further ensure the integrity of the phosphor doped coatings, synchrotron X-ray diffraction was performed to characterize the specific residual strains and thermal expansion of the materials, determining mechanical robustness and compatibility with state-of-the-art Thermal Barrier Coatings. The outcomes of this work pave the way for in-situ temperature measurements on phosphor-doped turbine blade coatings with increased performance and accuracy.

Fouliard, Quentin↗
DOE OSTI2021

Poisson’s ratio of eTPU molded bead foams in compression via in situ synchrotron X-ray microtomography

In situ synchrotron X-ray microtomography was used to characterize the bulk deformation behavior by computing the Poisson's ratio of expanded thermoplastic polyurethane (eTPU) molded bead foams used in footwear midsole during compression. Quantitative data on morphological characteristics were obtained using an iterative image processing workflow. Image correlation on the 4D datasets using DVC was performed to calculate the volumetric and axial strain to estimate the Poisson ratio. Strain maps from DVC showed the influence of variability in ligament thickness distribution on the global mechanical behavior exhibited which dominated the response seen in these bead foams. Lastly, our results showed a strong correlation between Poisson ratio and distribution of ligament thickness in foams.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Impact of nano-scale cavities on hydrogen storage and retention in yttrium hydride

Here, in situ synchrotron high-energy x-ray diffraction experiments and detailed transmission electron microscopy (TEM) characterization were conducted on as-fabricated and neutron-irradiated yttrium hydrides. The high-resolution synchrotron x-ray diffraction revealed minor α yttrium and major δ yttrium hydride phases in all specimens. Specimens were subject to heat treatments (heating-cooling cycles), and the intensity of α yttrium partially and completely disappeared in as-fabricated and neutron-irradiated specimens, respectively. The disappearance of α yttrium was unforeseen because hydrogen was expected to leave δ phase, causing an increase in α yttrium diffraction peak intensity. This observation indicated a surplus of hydrogen in the specimens where it was odd for hydride-forming early transition metal elements. The subsequent through-focus TEM characterization discovered nanometric cavities in both as-fabricated and neutron-irradiated yttrium hydride specimens for the first time. Two types of cavities were identified as fabrication-caused and irradiation-induced. The fabrication-caused cavities were associated with regions having linear deformation features, interfaces, and inclusions. The irradiation-induced cavities were observed as being formed isolated in the yttrium hydride phase. The presence of such nanometric cavities was considered as potential hydrogen storage pockets where the overall hydrogen storing capacity of yttrium hydride would be enhanced.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Grain Boundary Segregation Suppresses Local Short‐Range Ordering in Nanocrystalline High‐Entropy Alloys

Multi-principal-element alloys like high-entropy alloys (HEAs) have potential applications in many engineering fields due to their unique mechanical/functional properties. While HEAs are generally considered random solid solutions, recent studies revealed that they are prone to short-range-ordering (SRO) due to the complex multi-pair-wise interactions among the constituent elements. Meanwhile, SROs' evolution can sometimes be deleterious, and it is necessary to have control over their evolution. Examining the AlCoCrFe-Zr model alloy, long-range ordering occurs following the expectation of enthalpic predictions. Advanced characterization techniques—transmission electron microscopy, high-energy synchrotron X-ray diffraction/pair distribution function, and atom probe tomography, reveal that SRO is suppressed in as-milled and GB-decorated NC-(AlCoCrFe)100-xZrx (x = 0–1.5 atomic %). Warren-Cowley coefficient calculations are further used to validate the suppression of SRO. Besides the low segregation enthalpies of Cr, Fe, and Zr, and the high-mixing enthalpy of Cr and Fe, the short diffusion path to GBs due to high-GB density in the NC-HEAs and the higher energy state of the GBs than the matrix promotes GB-segregation that further alters the matrix chemistry and consequently disfavors SRO formation within the matrix. Despite the GB-segregation of Cr, Fe, and Zr, the matrices and GBs remain in a random solid solution.

36 MATERIALS SCIENCE↗
DOE OSTI2021

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

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

36 MATERIALS SCIENCE↗
DOE OSTI2024

A survey study on arsenic speciation in coal fly ash and insights into the role of coal combustion conditions

Coal fly ashes (CFAs) are the low-density byproducts of the coal combustion process. Improper or uncontrolled CFA disposal poses significant environmental and health concerns due to the potential leaching of toxic heavy metals such as arsenic (As). Previous studies have investigated the content and speciation of As in different CFA samples, yet systematic information on As speciation in CFA with representative coal source and combustion conditions is still missing. Based on a recent survey study on the typical coal sources and combustion conditions across the U.S., this study selected 19 representative CFA samples to systematically investigate As speciation and potential correlations with these parameters. The composition, morphology, mineralogy, and As speciation of these CFA samples were characterized by complementary analytical, microscopic, and spectroscopic techniques. Synchrotron X-ray spectroscopy and microscopy analyses revealed the dominant As oxidation state to be As(V) and with strong associations to Ca, with the exception of 3 samples that had 19–51% As(III), likely due to the use of selective catalytic reduction (SCR) process. Principal component analysis was conducted to identify potential correlations of As concentration and oxidation state with parameters such as major element content, loss on ignition (LOI), average particle size, coal source, and combustion condition. Al 2 O 3 and FeO content were found to capture a majority of the variability. Further, results from this study provide fundamental basis for understanding the correlations between coal source, combustion conditions, CFA characteristics, and As speciation, and providing insights for downstream beneficial utilization or disposal management.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2026

Status and new features of the topography beamline 1-BM after the Advanced Photon Source upgrade

The beamline 1-BM of the Advanced Photon Source (APS), a bending-magnet beamline with an effective X-ray beam size of ~100×4 mm2, has relatively comprehensive synchrotron topography and rocking curve imaging capabilities for characterization of crystals (particularly wide-bandgap semiconductors SiC, AlN, GaN, Ga2O3 etc). It is equipped with a white-beam topography stage for imaging large wafers up to 8 inches. It also has a double-crystal setup, of which the second stage can be used for monochromatic-beam topography. The first stage has different beam conditioners in the grazing-incidence geometry that can expand the vertical beam size from 4 to ~100 mm for double-crystal rocking curve imaging when it is combined with the second stage. Recently APS has been upgraded to a modern 4th-generation light source, and 1-BM has been recommissioned to its normal operation for general users with better performance. The upgraded APS leads to new features at 1-BM. The much smaller source size and higher X-ray coherence significantly improve the image resolution and contrast. The higher flux and brightness of the new source reduce exposure time, which mitigates the mechanical drifting and vibration issues. Here the main capabilities and status of 1-BM together with these new features are introduced.

X-ray topography↗
DOE OSTI2025

Identification of uranium oxidation states using oxygen K-edge scanning transmission X-ray microscopy

The field of nuclear forensics is growing in importance, and the increasing capabilities at synchrotron radiation light sources enable non-destructive characterization of oxide particles with better spatial, compositional, and oxidation state speciation resolution than ever before. Here, uranium oxide particles derived from multiple wet chemical processing methods were examined using a scanning transmission X-ray microscope (STXM), and a weakly-supervised method was developed to automatically analyze the collected data. Multiple uranium oxidation states were observed and quantified within and between samples, yielding information about differences between particles produced via the various processing routes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Understanding improved cycling and thermal stability of compositionally graded Ni-rich layered LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode materials

The concentration gradient is a strategic design, adjusting the distribution of Ni, typically with a higher Ni content in the core and a higher Mn content toward the surface. This design leverages the pivotal role of the Ni/Mn ratio, seeking to optimize cathode performance by balancing Ni's high capacity with Mn's stabilizing effects, particularly at the surface where degradation commonly occurs during cycling. Here, our study delves into the intricate structural and chemical transformations within concentration gradient cathode materials during electrochemical cycling. Utilizing advanced synchrotron X-ray techniques, including hard and soft X-ray absorption spectroscopy (hXAS, sXAS), and nanoscale X-ray imaging, we investigate buried changes in concentration gradient LiNi 0.6 Mn 0.2 Co 0.2 O 2 (CG NMC622). Contrary to conventional assumptions, our findings challenge the notion that cycling stability relies solely on Mn stability. Unraveling the roles of Ni and Mn, we uncover how their individual and collective contributions impact the cathode's overall performance. This investigation transcends established paradigms, shedding light on the crucial mechanisms governing the enhanced cycling stability of Nirich layered cathode materials.

25 ENERGY STORAGE↗
DOE OSTI2022

Bond valence sum analysis of pyrochlore oxides including the novel dielectric Te 6+ pyrochlores: A Bi M TeO 7-y ( A = Cd, Ca; M = Cr, Ga, Sc, In, Fe)

Bond valence sum analysis is a powerful tool used in evaluating and validating crystal structures; especially when those structures are complex in nature. The pyrochlore structure type is versatile in not only the unique bonding that it exhibits, but also in the properties that results from the structure. Here this paper aims to center the discussion of evaluating the pyrochlore structure using the bond valence sum method. In this study, novel quaternary pyrochlores with a general stoichiometry of ABiMTeO 7 (A = Cd, Ca; M = Cr, Ga, Sc, In, Fe) were synthesized and characterized for their structural, magnetic, and dielectric properties. Two representative compounds within this series of pyrochlores, BiCaFeTeO7 and BiCdFeTeO 7 , were structurally characterized utilizing a combination of high-resolution synchrotron X-ray diffraction and neutron diffraction revealing oxygen deficient pyrochlore systems which were off from the expected stoichiometry with respect to the M site. The A site of both pyrochlores were found to be moved off-center from the expected 16d site to the 96h displaced position at a magnitude of 0.25 Å and 0.22 Å for the Bi/Ca and Bi/Cd systems, respectively. These structures were evaluated using the bond valence sum method and compared with trends in the literature. The properties are also reported for the Bi/Ca system for the first time, showing relatively high dielectric constants with a low dielectric loss which are primarily independent of frequency and temperature. The magnetic measurements for the Bi/Ca system for the magnetic substitutions reveal a paramagnet and antiferromagnetic properties for the Fe and Cr analogs, respectively. The novel BiCaMTeO 7 quaternary pyrochlore system shows great promise as an emerging dielectric material.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗