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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 415 records · Page 23
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

The Inner Shell Spectroscopy beamline at NSLS-II: a facility for in situ and operando X-ray absorption spectroscopy for materials research

The Inner Shell Spectroscopy (ISS) beamline on the 8-ID station at the National Synchrotron Light Source II (NSLS-II), Upton, NY, USA, is a high-throughput X-ray absorption spectroscopy beamline designed for in situ, operando, and time-resolved material characterization using high monochromatic flux and scanning speed. This contribution discusses the technical specifications of the beamline in terms of optics, heat load management, monochromator motion control, and data acquisition and processing. Results of the beamline tests demonstrating the quality of the data obtainable on the instrument, possible energy scanning speeds, as well as long-term beamline stability are shown. The ability to directly control the monochromator trajectory to define the acquisition time for each spectral region is highlighted. Examples of studies performed on the beamline are presented. The paper is concluded with a brief outlook for future developments.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effect of Remnant Carbon and Etching of Particles on Pyrolysis Bonded Silicon Carbide (PBSC)

Silicon carbide (SiC) formed through pyrolysis of preceramic polymers loaded with SiC particles has gained significant attention for applications such as coatings, composite matrix modifications, and most importantly additive manufacturing. This work presents combined synchrotron XRD, Raman spectroscopy, scanning electron microscopy, nano-indentation, and Vickers indentation of pyrolysis bonded SiC to shed light on the changes of composition and mechanical properties of these materials. Characterization was performed on samples that were heat treated ranging from the synthesis 850 °C up to 1500 °C. Pre-treatments of the powders prior to pellet synthesis, such as heat treatment and etching using a hydrofluoric acid (HF), were investigated. It is shown that the degradation of mechanical properties when exposed to higher temperatures is due to the burnout of amorphous carbon clusters remnant of the pyrolysis process of the preceramic polymer. Furthermore, prior HF etching and removal of the native oxide layer of the powders showed improved density and hardness values in the final pellets. The average Vickers hardness of the control samples were 4.59 GPa and later 3.74 GPa when exposed to 1500 °C, while the samples synthesized using powders that were etched with HF had an average hardness value of 9.37 GPa and later 6.86 GPa when exposed to 1500 °C.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

In situ characterization of residual stress evolution during heat treatment of SiC/SiC ceramic matrix composites using high-energy X-ray diffraction

Volumetric strains were measured in silicon carbide/silicon carbide melt-infiltrated ceramic matrix composites (CMCs) at ambient and high temperatures using high-energy synchrotron X-ray diffraction (XRD). Both silicon and silicon carbide constituents were interrogated utilizing a broad spectrum of diffracting planes that would be largely inaccessible to common laboratory XRD equipment. Residual room-temperature principal strains in the melt-infiltrated silicon phase were found to be approximately 1100 mu epsilon in compression, corresponding to stresses of approximately 300 MPa using simplifying constitutive assumptions. Residual room-temperature principal strains in silicon carbide particles found throughout the matrix were approximately 500 mu epsilon in tension, corresponding to approximately 300 MPa. Residual strains were found to decrease considerably as temperatures increased from ambient temperature to 1250 degrees C. Additionally, residual strains returned to approximately preheat treatment values after cool-down to ambient temperature. Strain measurements in the silicon phase were found to be significantly affected by dissolved boron dopant levels causing contraction of the silicon lattice. This contraction must be accounted for in high-temperature experiments for accurate calculation of stresses in the silicon phase.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The diversity of aluminum-based drinking water treatment residuals for use in environmental remediation

Drinking water treatment residuals (DWTRs) are complex mixtures of organic and inorganic phases generally disposed of as waste materials. However, their strong sorptive properties could be further exploited to immobilize contaminants. To characterize these materials, we applied a range of analytical techniques to a set of aluminum-based DWTRs. Here we determined surface areas, elemental compositions using CHNS analysis and X-ray fluorescence (XRF), performed thermogravimetric analyses paired with mass spectrometry (TGA-MS), and used synchrotron-based methods: X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). Elemental analyses and specific surface area measurements – that vary between 7.23 ± 0.03 and 197.6 ± 0.9 m 2 g –1 – indicate that non-coagulant additives must play an important role in controlling sorption. High resolution powder XRD reveals the presence of only a few crystalline minerals mostly derived from source waters or additives. Fe was detected by XRF in all samples, whereas Mn was present in significant levels in samples with potassium permanganate as additive. The chemical speciation of these elements was characterized by performing spectral decompositions of XAS spectra. The spectral features of Fe are consistent with iron(III) oxides/hydroxides and structural iron in clays. On the other hand, Mn is predominantly present under its reduced form, Mn(II).

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Successful Cleanroom Installation of PIP-II SSR2 Coupler Using Robotic Arm

The Fermilab Side-Coupled Linac accelerates H- beam from 116 MeV to 400 MeV through seven 805 MHz modules. Twelve wire scanners are present in the Side Coupled Linac and four are present in the transfer line between the Linac and the Booster synchrotron ring. These wire scanners act as important diagnostic instruments to directly collect information on the beam s transverse distribution. The manipulation of the conditions of wire scanner data collection enables further characterization of the beamline, such as calculating emittance and the Twiss parameters of the beam at select regions. Here we present the results of these studies and characterization of the non-Gaussian transverse beam distribution observed.

Narug, C.↗
DOE OSTI2024

Emittance Measurements with Wire Scanners in the Fermilab Side-coupled Linac

The Fermilab Side-Coupled Linac accelerates H-beam from 116 MeV to 400 MeV through seven 805 MHz modules. Twelve wire scanners are present in the Side Coupled Linac and four are present in the transfer line between the Linac and the Booster synchrotron ring. These wire scanners act as important diagnostic instruments to directly collect information on the beam's transverse distribution. The manipulation of the conditions of wire scanner data collection enables further characterization of the beamline, such as calculating emittance and the Twiss parameters of the beam at select regions, which we present here.

43 PARTICLE ACCELERATORS↗
DOE OSTI2022

Atomic layer deposition of lithium zirconium oxides for the improved performance of lithium-ion batteries

Recently there has been increasing interest to develop lithium-containing films as solid-state electrolytes or surface coatings for lithium-ion batteries (LIBs) and related systems. Here, in this study, we for the first time investigated the thin film growth of lithium zirconium oxides (Li x Zr y O or LZOs) through combining two individual atomic layer deposition (ALD) processes of ZrO 2 and LiOH, i.e., sub-ALD of ZrO 2 and LiOH. We revealed that the hygroscopic nature of the LiOH component has a big impact on the growth of LZOs. We found that an increased temperature to 225 °C was more effective than an elongated purge to mitigate the adverse effects of physisorbed H 2 O. We further discovered that, during the resultant LZO super-ALD processes, the growth of sub-ALD LiOH has been promoted while the growth of sub-ALD ZrO 2 has been inhibited. In this study, a suite of instruments has been applied to characterize the LZO super-ALD processes and the resultant LZO films, including in situ quartz crystal microbalance (QCM), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), atomic force microscopy (AFM), synchrotron-based X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Furthermore, we applied the resulting LZO films over LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) cathodes in LIBs and demonstrated that the LZO coating films could evidently improve the lithium-ion insertion and extraction rates of the NMC622 electrodes up to 3.4 and 2.6 times, respectively. The LZO-coated NMC622 cathodes exhibited much better performance than the uncoated NMC622 ones.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Neutron Total Scattering Analysis of Materials for the Nuclear Fuel Cycle

Here, this paper reviews recent experimental efforts at the University of Tennessee and Oak Ridge National Laboratory to comprehensively characterize the structural details of materials relevant for the nuclear fuel cycle by employing advanced neutron scattering techniques. For the study of nuclear ceramics, neutron scattering offers distinct advantages over traditional laboratory or synchrotron X-ray diffraction, including enhanced sensitivity to elements with a low atomic mass, such as oxygen, nitrogen, and carbon. The key to these efforts is the recent advancement in the neutron scattering infrastructure at the high-flux diffractometers at the Spallation Neutron Source. The high neutron flux at these instruments enables neutron total scattering, a nondestructive bulk technique that simultaneously captures both short-range structural effects through pair distribution function analysis and long-range order through diffraction pattern analysis. This approach is particularly important for a comprehensive description of defective, disordered, or amorphous nuclear materials. The case studies presented here include analyses of the local defect structure in hyperstoichiometric uranium oxides and short-range order of ion-irradiated ceramics. This advanced analytical methodology will improve our understanding of the behavior of materials in extreme environments and contribute to the development of more resilient nuclear materials.

Neutron scattering↗
DOE OSTI2021

Seeing through nuclear fuel: Three-dimensional, nondestructive X-ray microscopy and volumetric analyses of neutron-irradiated TRISO-coated fuel kernels

The three-dimensional (3D) characterization of nuclear fuel with X-ray microscopy has historically proven difficult, due to uranium’s high attenuation of easily accessible X-rays, both in a laboratory setting and at a synchrotron user facility. However, this imaging modality provides nondestructive information that can be used to investigate morphological changes arising from external stimuli (e.g., neutron irradiation, high-temperature testing). Using an appropriate X-ray energy spectrum and an adequate X-ray filter, suitable transmissions through properly sized nuclear fuel specimens can be achieved. Here, in this study, we present the methods and results of using a commercially available, laboratory-based X-ray microscope (XRM) to examine the extent of 3D morphological changes of tristructural isotropic (TRISO)-coated fuel particles, specifically uranium oxide/uranium carbide fuel kernels, after high-temperature neutron irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Using Complementary Methods of Synchrotron Radiation Powder Diffraction and Pair Distribution Function to Refine Crystal Structures with High Quality Parameters—A Review

Determination of the atomic-scale structures of certain fine-grained minerals using single-crystal X-ray diffraction (XRD) has been challenging because they commonly occur as submicron and nanocrystals in the geological environment. Synchrotron powder diffraction and scattering techniques are useful complementary methods for studying this type of minerals. In this review, we discussed three example studies investigated by combined methods of synchrotron radiation XRD and pair distribution function (PDF) techniques: (1) low-temperature cristobalite; (2) kaolinite; and (3) vernadite. Powder XRD is useful to determine the average structure including unit-cell parameters, fractional atomic coordinates, occupancies and isotropic atomic displacement parameters. X-ray/Neutron PDF methods are sensitive to study the local structure with anisotropic atomic displacement parameters (ADP). The results and case studies suggest that the crystal structure and high-quality ADP values can be obtained using the combined methods. The method can be useful to characterize crystals and minerals that are not suitable for single-crystal XRD.

58 GEOSCIENCES↗
DOE OSTI2025

In-Situ Synchrotron X-Ray Diffraction of Ultrasonic Microstructural Refinement During Solidification in a Commercial Al–Si–Mg Alloy

This study reports the first use of in-situ synchrotron X-ray diffraction (SXRD) to study the effects of ultrasonic melt processing (USMP) on phase and grain size evolution during solidification in a commercial Al–Si–Mg casting alloy. USMP is a technique that, when applied to aluminum as it solidifies, can be used to refine the local microstructure of large-scale castings. Analysis of the in-situ SXRD data to estimate the average grain size of primary α-Al grains during USMP demonstrates that USMP slows the growth rate of α-Al grains and reduces grain size by 36 pct. Furthermore, there is also evidence that USMP causes the primary α-Al grains to move relative to the X-ray beam; such motion increases the probability of primary α-Al grains colliding and fragmenting. This movement becomes constrained at the onset of the Al–Si binary eutectic, suggesting that USMP ceases to effectively refine the microstructure once the Al–Si binary eutectic begins to form. Complementary laboratory-scale X-ray diffraction (XRD) data were used to correlate the lattice parameters of the α-Al and Si (D-A4) phases with temperature to estimate cooling rate during solidification. Thus, this study can guide the design of novel castings with spatially distributed fine-grained regions produced using local ultrasonic processing.

Aluminum Alloys↗
DOE OSTI2023

In situ spin coater for multimodal grazing incidence x-ray scattering studies

We present herein a custom-made, in situ, multimodal spin coater system with an integrated heating stage that can be programmed with spinning and heating recipes and that is coupled with synchrotron-based, grazing-incidence wide- and small-angle x-ray scattering. The spin coating system features an adaptable experimental chamber, with the ability to house multiple ancillary probes such as photoluminescence and visible optical cameras, to allow for true multimodal characterization and correlated data analysis. This system enables monitoring of structural evolutions such as perovskite crystallization and polymer self-assembly across a broad length scale (2 Å–150 nm) with millisecond temporal resolution throughout a complete thin film fabrication process. The use of this spin coating system allows scientists to gain a deeper understanding of temporal processes of a material system, to develop ideal conditions for thin film manufacturing.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

High-energy synchrotron x-ray study of deformation-induced martensitic transformation in a neutron-irradiated Type 316 stainless steel

An unusual tensile deformation behaviour in the form of a propagating band along the sample gauge was observed in two neutron-irradiated 316 stainless steel samples during room-temperature tests, leading to a combination of high strength and high ductility. These bands were not observed in an unirradiated counterpart. With the help of in situ high-energy synchrotron x-ray diffraction, the phase-specific crystal information was tracked at different deformation levels in each sample. Post-irradiation and post-deformation samples were examined using electron microscopy to characterize various microstructural features. All samples displayed a deformation-induced martensitic phase transformation, which was identified as a second strain-hardening mechanism accompanying the dislocation hardening. The deformation-induced martensitic transformation was rationalized by the effect of applied stress on the effective martensite start temperature. The results showed that the irradiation did not alter the dislocation hardening and the martensitic transformation mechanisms, but the increased yield strength in irradiated materials facilitated the localized phase transformation at the onset of plastic deformation, in contrast to the unirradiated material which required pre-straining. The hardening effect of the martensitic transformation reduced the tendency towards necking and mitigated the loss of ductility in the irradiated material by carrying the deformation in the form of a propagating band. Despite the beneficial effect from the martensitic transformation, this study indicates that this mechanism cannot not be activated at typical operating temperatures of nuclear reactors.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Neutron-Friendly Li-Ion Battery Coin Cell for In Situ 3D Visualization of Li Plating

Advanced battery characterization using in situ/operando neutron imaging is critical for uncovering degradation modes such as lithium (Li) plating in Li-ion batteries (LIBs). However, conventional LIBs hinder operando neutron radiography (NR) and in situ neutron micro-computed tomography (N-μCT) for visualizing Li plating near the graphite-separator interface due to strong attenuation from hydrogen-rich components like PP–PE–PP separators, electrolyte, and Fe-based spacers. In this work, we designed and tested a neutron-friendly battery (NFB) optimized for in situ Li detection during extreme fast charging (XFC). Guided by neutron attenuation cross-sections and material transmission, the NFB enables clear visualization at the graphite–separator interface, which is typically opaque in standard LIBs. Electrochemical tests show the NFB exhibits voltage/current responses like standard cells for up to 50 XFC cycles. However, its lower reversibility and capacity are likely due to Cu-coated Al spacer degradation from delamination or corrosion. We propose titanium spacers as a more stable alternative, albeit requiring custom machining. Using this optimized cell, we achieved simultaneous neutron tomography of multiple cells, capturing in situ 3D images of dead Li accumulation, particularly near graphite edges. These heterogeneous deposits and disconnected Li clusters suggest localized current density hotspots during XFC.

25 ENERGY STORAGE↗
DOE OSTI2025

One-dimensional heterocyclic carbene–Au metal–organic frameworks bridging ultra-high vacuum models and scalable liquid-phase growth

The controlled design of molecule–metal interfaces is central to the development of functional nanomaterials for catalysis, sensing, and molecular electronics. Here we show that the adsorption of a Janus-type diimidazolium precursor on gold yields one-dimensional (1D) N-heterocyclic carbene (NHC)–Au–NHC metal organic frameworks (MOFs) featuring positively charged gold nodes. Using synchrotron X-ray photoemission spectroscopy (XPS), near edge X-ray adsorption fine structure (NEXAFS) spectroscopy and scanning tunnelling microscopy (STM), we demonstrate that thermal activation promotes counterion removal and drives the formation of extended 1D arrays, characterized by ∼1.0 nm Au–Au spacing and adatom densities up to 0.6 atom nm −2 (∼4% of surface atoms). Importantly, we translate this ultra-high vacuum (UHV) benchmark into a scalable solution-phase protocol in ethanol, enabling 1D-MOF growth under mild, base-free, open-air conditions. The resulting films retain structural and electronic signatures of UHV-grown systems, bridging model studies and practical synthesis. This approach establishes NHC–metal frameworks as accessible, tunable platforms for catalysis and materials design.

Gold adatoms↗
DOE OSTI2020

Build Orientation Dependent Microstructure in Polymer Laser Sintering: Relationship to Part Performance and Evolution with Aging

Laser sintering (LS) is widely used to produce functional polymeric parts; however, the resulting parts are often limited by their porous structure, and performance of the part may be strongly anisotropic. Relating the structural features of parts to build process conditions or powder feedstock has been explored previously. In contrast, little is known regarding how the unique internal structures of LS parts evolve and relate to their performance later in their life cycle, for example, after use in a real-world operating environment. In this study, a tightly controlled LS build process and measurement campaign by standard X-ray computed tomography (XCT), supported by high-resolution synchrotron XCT, was used to benchmark the internal microstructure (e.g. porosity) as a function of four different build orientations in printed polyamide-12 (PA-12) parts. The initial performance of the parts after printing was characterized by tensile testing and dynamic mechanical analysis (DMA). Arrays of PA-12 parts in different build orientations were exposed to steam (under pressure) and air across multiple temperature and time points for the purposes of accelerated aging through oxidative and hydrolytic breakdown. Exposing parts to steam dramatically altered the internal microstructure and functional properties such as the glass transition temperature, tensile properties, and damping behavior. Notably, post-aging XCT revealed large microstructural changes after only 40 h of steam treatment relative to the as-printed specimens. Furthermore, pore reorganization and changes in crystallinity occurred regardless of whether the steam temperature was aggressive enough to induce a significant loss in mechanical properties. The build orientation dependence on the aging rate was minimal with the relative trend in performance persisting across most metrics among the different orientations even after aging.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Design Rules for Carboborothermic Reduction Synthesis of High Uranium Density UB 4 –UBC Composites

Uranium borides are promising candidate fuel forms for use in advanced nuclear reactors due to their high thermal conductivity and potential for dual use as both fuel and burnable absorber. In this work, uranium tetraboride () and uranium monoboroncarbide (UBC) composite were synthesized by using industrially scalable carboborothermic reduction method. The final uranium boride phase composition is sensitive to the sample holding crucibles ( and graphite) such that graphite supply excess carbon, promoting the formation of a predominant UBC phase. The high‐temperature in situ synchrotron X‐ray diffraction of pristine –UBC show persistence , UBC, and phases while preoxidized –UBC leads to predominant and formation due to progressive oxidation and boron loss at high temperature. The oxidation behavior was further characterized using thermogravimetric analysis, allowing direct comparison with other potential accident tolerant fuels such as , , UC, and UN. The –UBC shows higher uranium loading than monolithic and demonstrates promising oxidation behavior at high temperature, pointing to its potential as an improved uranium boride‐based fuel form.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗