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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Colossal Strain Tuning of Ferroelectric Transitions in KNbO 3 Thin Films

Strong coupling between polarization ( P ) and strain (ɛ) in ferroelectric complex oxides offers unique opportunities to dramatically tune their properties. Here colossal strain tuning of ferroelectricity in epitaxial KNbO 3 thin films grown by sub‐oxide molecular beam epitaxy is demonstrated. While bulk KNbO 3 exhibits three ferroelectric transitions and a Curie temperature ( T c ) of ≈676 K, phase‐field modeling predicts that a biaxial strain of as little as −0.6% pushes its T c > 975 K, its decomposition temperature in air, and for −1.4% strain, to T c > 1325 K, its melting point. Furthermore, a strain of −1.5% can stabilize a single phase throughout the entire temperature range of its stability. A combination of temperature‐dependent second harmonic generation measurements, synchrotron‐based X‐ray reciprocal space mapping, ferroelectric measurements, and transmission electron microscopy reveal a single tetragonal phase from 10 K to 975 K, an enhancement of ≈46% in the tetragonal phase remanent polarization ( P r ), and a ≈200% enhancement in its optical second harmonic generation coefficients over bulk values. These properties in a lead‐free system, but with properties comparable or superior to lead‐based systems, make it an attractive candidate for applications ranging from high‐temperature ferroelectric memory to cryogenic temperature quantum computing.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Morphological controls on flow conductivity and viscosity of bentonite–polymer composites

In this study, the authors investigate the morphological organisation of polymers in bentonite–polymer composites (BPCs) used in geosynthetic clay liners and controls on hydraulic conductivity and viscosity. A limited understanding of the relationship between the microstructure of BPCs and their macroscopic engineering behaviour motivates this study. The polymer resides in the inter-granular pores of bentonite based on synchrotron-based small-angle X-ray scattering measurements, scanning electron microscopy imaging and pore size analyses. On wetting, the polymer swells to produce a swollen hydrogel residing in the inter-granular pores. Enhanced tortuosity arising from hydrogel formation reduces the hydraulic conductivity of BPCs. The higher viscosity of the BPC slurry is attributed to the higher shear resistance emerging from swelling of the polymer fraction on wetting. These findings link the morphological features of BPCs to the observed hydraulic conductivity and viscosity of these materials.

Engineering↗
DOE OSTI2021

In Situ Synchrotron X-ray Micro-Diffraction Investigation of Elastic Strains in Laminated Ti-Al Composites

Spatially resolved elastic strains in the bulk interior of a laminated Ti-Al metal composite were studied during in situ tensile loading at strains up to 1.66% by a synchrotron-based micro-diffraction technique, namely differential aperture X-ray microscopy (DAXM). For both Al and Ti grains, deviatoric elastic strains were estimated based on polychromatic X-ray microbeam diffraction, while lattice strains along the normal direction of the tensile sample were directly measured using monochromatic X-ray microbeam diffraction. The estimated deviatoric strains show large spatial variations, and the mean values are consistent with the external loading conditions, i.e., increasing tensile strain along the tensile direction and increasing compressive strain along the sample normal with increasing loading. The directly measured lattice strains also show large spatial variations, although the magnitude of this variation is smaller than that for the estimated deviatoric strain. The directly measured lattice strains in Ti grains are largely consistent with the external loading, whereas those in Al grains are in contradiction with the external loading. The causes of the experimental results are discussed and related to both the laminated microstructure of the composite material and the limitations of the techniques.

36 MATERIALS SCIENCE↗
NASA NTRS2002

STARDUST and Interplanetary Dust Particles - Big Science from Small Samples

Comets are primitive bodies that are widely believed to be a reservoir of preserved interstellar and circumstellar grains, and molecular cloud materials (organics). Direct samples of cometary dust along with interstellar grains will be returned by the STARDUST Mission in 2006. Analyses of interplanetary dust particles (IDPs) and analogue materials in the laboratory provide constraints and serve as "ground truth" for evaluating various hypotheses on the nature of comets and interstellar grains. Anhydrous IDPs are the most primitive remnants of the primordial Solar System, and are our only known samples of comets. These cometary lDPs are rich in preserved interstellar organic compounds II]. In addition, abundant interstellar silicates have recently been discovered in cluster lDPs [2]. In some of these IDPs, the presolar silicate abundance reaches 1 wt %, exceeding the total presolar grain abundance in meteorites by three orders of magnitude, where presolar silicates are still notably absent. The results to date support the idea that comets are rich in presolar materials, but are at odds with the common perception that they are 'pristine aggregates of interstellar grains'. These results underscore the scientific importance of sample return missions to comets. The technology for the analysis of micrometer-sized samples is well advanced. The newest generation of ion probe instruments allow for isotopic analyses at the submicrometer level. The nature of the organic matter is analyzed using Infrared and soft X-ray spectroscopy techniques on synchrotron-based instruments, also at the micrometer-scale and smaller. Electron microscopy and spectroscopy provide details on the mineralogy and chemistry of constituent grains in !DPs at nearly the atomic scale. Novel sample preparation techniques have been developed such that all of these measurements can now be made on the same 10 micrometer diameter particle. Returned comet samples captured in aerogel will pose new challenges in sample analysis, but should provide a major leap in our understanding of the fundamental building blocks of our Solar System.

Keller, L. P.↗
DOE OSTI2020

Impact of krypton irradiation on a single crystal tungsten: Multi-modal X-ray imaging study

Understanding microstructural and strain evolutions induced by noble gas production in the nuclear fuel matrix or plasma-facing materials is crucial for designing next generation nuclear reactors, as they are responsible for volumetric swelling and catastrophic failure. In this paper we describe a multimodal approach combining synchrotron-based nanoscale X-ray imaging techniques with atomic-scale electron microscopy techniques for mapping chemical composition, morphology and lattice distortion in a single crystal W induced by Kr irradiation. We report that Kr-irradiated single crystal W undergoes surface deformation, forming Kr containing cavities. Furthermore, positive strain fields are observed in Kr-irradiated regions, which lead to compression of underlying W matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Hg Accumulation by Single-Cell Sulfate-Reducing Bacteria Methylating Mercury

Methylmercury (MeHg) is a potent neurotoxin that poses risks to ecosystems and human health. MeHg is produced by microbes following saturating-like kinetics. We hypothesize that this saturation reflects a limited intracellular mercury (Hg) accumulation. Here, in this study, we investigated Hg accumulation in Pseudodesulfovibrio hydrargyri BerOc1, a sulfate-reducing model strain able to methylate Hg. Cells were incubated with 0.5 and 2 μM of mercury (HgCl 2 ), and mercury localization was studied using synchrotron-based nano-X-ray fluorescence and high-resolution analytical electron microscopy. For both concentrations, Hg was detected in the bacterial cytosol, in addition to extracellular (Hg, S)-containing nanoparticles. Intracellular Hg levels were slightly higher at 2 μM than at 0.5 μM (1.61 vs 1.40 pg.mm –2 ), suggesting a regulated accumulation. However, the population exhibited heterogeneity in Hg accumulation, particularly at the highest Hg exposure, with some cells being Hg hyperaccumulators. Correlative imaging between Hg localization and cell viability revealed that these hyperaccumulating cells were non-active. Our results suggest that active cells regulate Hg accumulation. From an analytical perspective, a minor subpopulation of hyperaccumulating cells can bias bulk measurements and should be considered in interpreting Hg accumulation in microorganisms. Environmentally, these cells can impact Hg cycling by acting as a metal sink.

Intracellular accumulation↗
DOE OSTI2021

Structural and chemical changes from CO2 exposure to self-healing polymer cement composites for geothermal wellbores

Wellbore cement is subjected to a number of mechanical, thermal and chemical stress regimes over its lifetime. Therefore, next generation wellbore cement formulations need to be evaluated in conditions relevant to these environments. In this work, we investigate the mechanism of the alteration of a novel self-healing polymer-cement composite recently reported by our group after exposure to a CO2-rich environment by using synchrotron based X-ray Fluorescence (XRF) and X-ray absorption near edge structure (XANES) and scanning electron microscopy coupled with energy dispersive spectroscopy. Results showed that chemical alteration of the polymer-cement follows the rim carbonation mechanism, similar to conventional cement although carbonation takes place to a lesser extent in polymer-cements despite the higher porosity. Along with detailed mechanistic insights on carbonation in polymer-cement composite, the performance of these in CO2-rich environment is further studied using standard compressive strength analysis.

Elbakhshwan, Mohamed↗
DOE OSTI2021

Evaluating the grain-scale deformation behavior of a single-phase FCC high entropy alloy using synchrotron high energy diffraction microscopy

We report although the deformation behavior of high-entropy alloys (HEAs) has been extensively studied at the macroscale, many important properties have yet to be explored for these alloys at the microscale, thus hampering accurate prediction of damage and failure processes. Synchrotron high-energy diffraction microscopy (HEDM) and fast-Fourier transform-based crystal plasticity modeling was conducted to investigate the three-dimensional (3D) grain-resolved micromechanical response for approximately 1,900 constituent grains within a single-phase FCC HEA up to 1% applied strain. The evolution of grain-resolved elastic strains, lattice reorientations, and maximum resolved shear stresses (mRSS) were evaluated to quantify elastic, yield, and fully plastic behavior. Overall, the initial critical resolved shear stress (CRSS), determined via in situ HEDM and companion modeling, was found to be > 20% higher than estimated using the classical polycrystalline Taylor factor (M = 3.06). However, a descriptive parameter based on the average grain-resolved Taylor factor ($\overline{M}$) was found to show excellent agreement with plastic yielding behavior observed within HEDM datasets. Noticeable deviations in HEDM lattice reorientations compared to both EVP-FFT simulations and classical predictions for FCC polycrystals were discovered, highlighting the complexity in correlating local lattice reorientations, Taylor, and Schmid factors with plastic response for this material at the grain-scale. Therefore, it is anticipated that the overall trends and parameter identification of 3D grain-resolved properties in this study can serve as an important foundation for continued mesoscale investigation on both well-established and newly developed Cantor-like HEAs.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Unraveling the Early-Stage Ordering of Krypton Solid Bubbles in Molybdenum: A Multimodal Study

Self-organization of defects such as fission gas bubbles in materials can lead to high inventory capacity for fission gas storage and help mitigate swelling caused by fission gases in nuclear fuel materials under radiation in nuclear reactors. Here, we report the physical mechanism of self-organization of krypton (Kr) gas bubbles in molybdenum (Mo) under ion implantation. The ion fluence and temperature-dependent formation of Kr solid bubble superlattice (SBS) in Mo were investigated by using both synchrotron-based small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). Early stage self-organization of gas bubbles is observed at a fluence of 2.5 × 10 16 ions/cm 2 at temperatures of 300–400 °C. The bubble lattice constant increases with increasing implantation temperature from 300 to 400 °C. Both experiments and atomic kinetic Monte Carlo modeling indicate that the Kr solid bubbles are weakly ordered in comparison to previously studied helium (He) gas bubble superlattice (GBS) while the lattice constant are relatively smaller for Kr SBS compared to that of He GBS. The irradiation conditions suggest that spinodal decomposition, which is a form of phase separation, probably precedes gas bubble ordering in Mo. Altogether, our work sheds light on the formation mechanism of noble gas superlattice toward the development of radiation-tolerant materials which are important for the design of advanced nuclear reactors.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Revolutionizing Lithium Storage Capabilities in TiO 2 by Expanding the Redox Range

TiO 2 is a widely recognized intercalation anode material for lithium-ion batteries (LIBs), yet its practical capacity is kinetically constrained due to sluggish lithium-ion diffusion, leading to a lithiation number of less than 1.0 Li + (336 mAh g -1 ). Here, the growth of TiO 2 crystallites is restrained by integrating Si into the TiO 2 framework, thereby enhancing the charge transfer and creating additional active sites potentially residing at grain boundaries for Li + storage. This strategy is corroborated by the expanded redox range of Ti, as thoroughly demonstrated via synchrotron radiation-based X-ray spectroscopy and Cs-corrected electron microscopy. Consequently, when deployed for lithium storage, the tailored material achieves an extraordinarily high reversible capacity of 559 mAh g -1 , 116% of the theoretical maximum of 483 mAh g -1 calculated based on all active species, while simultaneously retaining superior rate capability and robust cycling stability. Further, this work offers fresh perspectives on the revitalization of traditional electrode materials to achieve enhanced capacities.

25 ENERGY STORAGE↗
DOE OSTI2025

Bridging multimodal microscopy for advanced characterization on nuclear fuel using machine learning

Uranium dioxide (UO 2 ), widely used as driver fuel in light water reactors, experiences microstructure and property change by nuclear fission reactions. This paper bridges the characterization of fresh UO 2 fuel at different length scales, serving as a baseline for future post irradiation examination of irradiated UO 2 fuel. To characterize the microstructural change of nuclear fuel, modern approaches cover a wide range of length scales through different characterization techniques, such as mm scale for Synchrotron-based X-ray computed tomography (SXCT) and microscale for focused ion beam (FIB) and scanning electron microscopy (SEM). It is challenging to bridge the data and knowledge of the same sample in different length scales. This paper proposed a deep learning framework leveraging transfer learning to detect microstructural defects, trained from a sparse FIB, SEM, and SXCT images. The proposed model achieved superior performance in defect segmentation on multiscale microscopic data compared to four of the latest deep learning models.

36 MATERIALS SCIENCE↗
DOE OSTI2020

FeS colloids – formation and mobilization pathways in natural waters

For this study, we have used synchrotron-based X-ray absorption spectroscopy (structure of Fe–S clusters), transmission electron microscopy (solid-phase crystallinity), Fourier-transform ion-cyclotron-resonance mass spectrometry (identity and composition of natural organic carbon compounds), inductively coupled plasma optical emission spectrometry (total aqueous Fe), and the revised ferrozine method (aqueous Fe( II ) and Fe( III ) concentrations) to determine the stability and nature of colloids generated by sulfidation of ferrihydrite nanoparticles in the absence and presence of organic compounds. We observed that reductive dissolution of ferrihydrite by aqueous sulfide generates nm-scale FeS clusters. Their subsequent aggregation, which promotes settling of FeS aggregates into the solid fraction, was directly correlated with sulfide/Fe ratio. At sulfide/Fe ratios ≤0.5, FeS clusters and larger colloids remained in suspension for at least 14 days (and up to several months). At sulfide/Fe ratios >0.5, sulfidation reaction rates were rapid and FeS cluster aggregation was accelerated. Moreover, the presence of organic compounds increased the time of suspension of FeS colloids, whereas increased ionic strength inhibited the generation of FeS colloids. We present a general conceptual model to predict when and where FeS colloids can form and enhance or inhibit the mobility of contaminants and nutrients associated with them. Our study indicates that in lowsalinity fresh groundwater systems poor in sulfate (i.e. low sulfidation; lakes, floodplains, peatlands etc.), the ferrihydrite sulfidation reaction generates aqueous FeS clusters and larger colloids that remain suspended over long time periods, thus mobilizing a substantial fraction of the total aqueous Fe and S.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Simultaneous bright- and dark-field X-ray microscopy at X-ray free electron lasers

Abstract The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $$10^{12}$$ 10 12 photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

In Situ Studies of Methanol Decomposition Over Cu(111) and Cu2O/Cu(111): Effects of Reactant Pressure, Surface Morphology, and Hot Spots of Active Sites

The dissociative adsorption of methanol was investigated on Cu(111) and ultrathin Cu 2 O films. We employed synchrotron-based Ambient Pressure X-ray Photoelectron Spectroscopy (AP-XPS) and Scanning Tunneling Microscopy (STM) to study the dynamics of gas–solid interactions, and calculations based on Density Functional Theory (DFT) were used to examine the reaction path. C 1s XPS spectra revealed that methanol underwent dissociative adsorption on plain Cu(111) to form methoxy (CH 3 O), formaldehyde (H 2 CO), and formate (HCOO) at a pressure range of 0.5–10 mTorr, with these species remaining on the surface after evacuation. This was accompanied by the appearance of a low coverage (~0.05 ML) of O ads in the O 1s which can be considered a highly active site for methanol activation. The high activity is apparent by a coverage of 0.8 ML of methoxy at room temperature. STM was unable to image these species at room temperature as they were highly mobile on metallic copper. In contrast, for CH 3 OH on Cu 2 O/Cu(111), STM showed clear hot spots for reaction and a complex array of adsorption structures. On the oxide substrate, there was decomposition of methanol to H 2 CO, CH 3 O, HCOO, and hydrocarbon species (CH x ) due to the subsequent interactions of methanol with lattice oxygen. Cu(111) remained entirely saturated with decomposition products under 10 mTorr of methanol (θ ≈ 0.97 ML), whereas the Cu 2 O overlayer was saturated at a much lower coverage (θ ≈ 0.30 ML). STM revealed rows and step edges of Cu 2 O decorated with decomposition products and metallic Cu islands ~5 nm in size. The difference in activity between Cu(111) and Cu 2 O/Cu(111) is attributed to the significant amount of O present on the oxide surface. Additionally, Density Functional theory (DFT) calculations described the XPS measurements well, showing a likely methanol dissociation to *CH 3 O and therefore a surface reduction. More importantly, the DFT results revealed that it was the chemisorbed oxygen on Cu 2 O/Cu(111) which oxidized the dissociated *CH 3 O to *HCOO and eventually CO 2 , while the reaction only involving upper oxygen on the Cu 2 O hexagonal ring led to the formation of H 2 CO.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Stratospheric ozone depletion in the Antarctic region triggers intense changes in sea salt aerosol geochemistry

Abstract Since the early 1980s, the Antarctic environment has served as a natural field laboratory for researchers to investigate the effects of stratospheric ozone depletion, which has resulted in increased surface ultraviolet radiation levels. However, its effective threats still present gaps. We report new pieces of evidence of increased ultraviolet radiation impacting West Antarctica sea salt aerosols. Salt aerosols, particularly in the Southern Ocean Sea, play an important role in the radiative earth balance. To disclose the molecular details of sea salt aerosols, we used a synchrotron-based multi-element microscopic speciation of individual microparticles (Scanning Transmission X-ray Microscopy with Near-Edge X-ray Absorption Fine Structure Spectroscopy combined with Computer-Controlled Scanning Electron Microscopy). Here we identified substantial abundances of chlorine-enriched aerosols in sea salt generated by photolytic products, whereas ice core records revealed increased chlorine depletion from the onset of ozone depletion. Our findings reveal that modern sea salt modification has no Holocene precedent.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Quantification of room temperature strengthening of laser shock peened Ni-based superalloy using synchrotron microdiffraction

Laser shock peening (LSP), a surface modification technique, is promising to enhance the strength and wear resistance for Ni-based superalloys. To understand the strengthening mechanism in a laser shock peened Ni-based superalloy DZ417G, we utilize synchrotron poly- and monochromatic X-ray microdiffraction, as well as electron microscopy and microhardness to quantify the local microstructures and mechanical properties at various depths. In the 1.2-mm-deep hardened layer, the microhardness increases monotonically by ~50% from the unaffected interior to the surface. Quantitative microdiffraction analysis shows that large amounts of dislocations are introduced by LSP. High densities of 7.1 × 10 15 m -2 and 11.8 × 10 15 m -2 are seen close to the peened surface for the γ- and γ'-phases, respectively, which are 5 and 20 times of those in the unaffected region. Different gradients of dislocation density are observed for the two phases from interior to surface, and their combined effect accounts well for the hardness increment. Due to the unaltered γ'-precipitates and chemical composition in the LSP affected zone, the large density of dislocations dominates the observed strengthening. Combined poly- and monochromatic X-ray microdiffraction allows quantifying the local microstructures of plastic deformation over a large sampling scale that can hardly be achieved using other materials characterization techniques.

36 MATERIALS SCIENCE↗
DOE OSTI2022

In situ analysis of the nucleation of O- and Zn-polar ZnO nanowires using synchrotron-based X-ray diffraction

The selection of the polarity of ZnO nanowires grown by chemical bath deposition offers a great advantage for their integration into a wide variety of engineering devices. However, the nucleation process of ZnO nanowires and its dependence on their polarity is still unknown despite its importance for optimizing their morphology and properties and thus to enhance the related device performances. To tackle this major issue, we combine an in situ analysis of the nucleation process of O- and Zn-polar ZnO nanowires on O- and Zn-polar ZnO single crystals, respectively, using synchrotron radiation-based grazing incidence X-ray diffraction with ex situ transmission and scanning electron microscopy. We show that the formation of ZnO nanowires obeys three successive phases from the induction, through nucleation to growth phases. Additionally, the characteristics of each phase, including the nucleation temperature, the shape and dimension of nuclei, as well as their radial and axial development are found to depend on the polarity of ZnO nanowires. A comprehensive description reporting the dominant physicochemical processes in each phase and their dependence on the polarity of ZnO nanowires is presented, revisiting their formation process step-by-step. These findings provide a deeper understanding of the phenomena at work during the growth of ZnO nanowires by chemical bath deposition and open the perspective to develop a more accurate control of their properties at each step of the formation process.

77 NANOSCIENCE AND NANOTECHNOLOGY↗