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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 OSTI2026

Nondestructive ultrasonic characterization of a triple-weld-bead wire arc additively manufactured ER70S-6 S-curved wall

Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Imaging atomic-scale chemistry from fused multi-modal electron microscopy

Efforts to map atomic-scale chemistry at low doses with minimal noise using electron microscopes are fundamentally limited by inelastic interactions. Here, fused multi-modal electron microscopy offers high signal-to-noise ratio (SNR) recovery of material chemistry at nano- and atomic-resolution by coupling correlated information encoded within both elastic scattering (high-angle annular dark-field (HAADF)) and inelastic spectroscopic signals (electron energy loss (EELS) or energy-dispersive x-ray (EDX)). By linking these simultaneously acquired signals, or modalities, the chemical distribution within nanomaterials can be imaged at significantly lower doses with existing detector hardware. In many cases, the dose requirements can be reduced by over one order of magnitude. This high SNR recovery of chemistry is tested against simulated and experimental atomic resolution data of heterogeneous nanomaterials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

An ultra-compact x-ray free-electron laser

In the field of beam physics, two frontier topics have taken center stage due to their potential to enable new approaches to discovery in a wide swath of science. These areas are: advanced, high gradient acceleration techniques, and x-ray free electron lasers (XFELs). Further, there is intense interest in the marriage of these two fields, with the goal of producing a very compact XFEL. In this context, recent advances in high gradient radio-frequency cryogenic copper structure research have opened the door to the use of surface electric fields between 250 and 500 MV m -1 . Such an approach is foreseen to enable a new generation of photoinjectors with six-dimensional beam brightness beyond the current state-of-the-art by well over an order of magnitude. This advance is an essential ingredient enabling an ultra-compact XFEL (UC-XFEL). In addition, one may accelerate these bright beams to GeV scale in less than 10 m. Such an injector, when combined with inverse free electron laser-based bunching techniques can produce multi-kA beams with unprecedented beam quality, quantified by 50 nm-rad normalized emittances. The emittance, we note, is the effective area in transverse phase space (x, p x /m e c) or (y, p y /m e c) occupied by the beam distribution, and it is relevant to achievable beam sizes as well as setting a limit on FEL wavelength. These beams, when injected into innovative, short-period (1–10 mm) undulators uniquely enable UC-XFELs having footprints consistent with university-scale laboratories. We describe the architecture and predicted performance of this novel light source, which promises photon production per pulse of a few percent of existing XFEL sources. We review implementation issues including collective beam effects, compact x-ray optics systems, and other relevant technical challenges. To illustrate the potential of such a light source to fundamentally change the current paradigm of XFELs with their limited access, we examine possible applications in biology, chemistry, materials, atomic physics, industry, and medicine—including the imaging of virus particles—which may profit from this new model of performing XFEL science.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Diagnosis of PV Cell Passivation Degradation Resulting from Hot-Humid, High Voltage Potential Aging

Corrosion of the antireflective coating on the cell ("AR c corrosion") was previously observed in studies using hot-humid test conditions with external high voltage (HV) bias. Because AR c corrosion is not well understood, mini-modules (MiMos) were examined in a comparative experiment using PERC and PERT as well as legacy Al-BSF cells. For separate MiMos with the cell circuit electrical at +1500 V, -1500 V, or unbiased "V oc", test conditions in the comparative study included 60degrees C/60% RH for 96 h, as in IEC TS 62804-1; 70degrees C/70%RH for 200 h; and 85degrees C/85% RH for 200 h. Characterizations at each read point included: camera and electroluminescence (EL) imaging, colorimetry, and I-V curve tracing. Characterizations at the final read point included: SunsVoc; spatially mapping external quantum efficiency (EQE); high resolution: photoluminescence (PL), EL, and dark lock-in thermographic (DLIT) imaging. Forensics were performed on extracted cores, including scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS) and scanning Auger microscopy (SAM). Forensics were also conducted on MiMos (stepped HV aging) and full-sized modules (outdoor aging) from previous studies. AR c corrosion was specifically observed for the glass/encapsulant/cell side of +1500 V (HV+) stressed MiMos, where appearance, color, and reflectance were the characteristics most distinguished relative to simultaneously occurring degradation modes. SEM/EDS and SAM identified conversion of silicon nitride to silicon oxide or hydrous silica, preferentially occurring at the edges and tips of the pyramidal textured cell surface.

aging↗
DOE OSTI2023

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterization of Nanoscale Pores in Tight Gas Sandstones Using Complex Techniques: A Case Study of a Linxing Tight Gas Sandstone Reservoir

Pore structures with rich nanopores and permeability in tight gas reservoirs are poorly understood up to date. Advanced techniques are needed to be employed to accurately characterize pore structures, especially tiny pores which include micron and nanopores. In this study, various experimental techniques such as scanning electron microscopy (SEM), nuclear magnetic resonance (NMR) T 2 , nitrogen adsorption method, and NMR cryoporometry (NMRC) are combined to interrogate the complex pore systems of the tight gas reservoir in the Linxing formation, Ordos Basin, China. Results show that tight gas sandstones are primarily comprised of residual interparticle and clay-dominated pores. Clay and quartz are two dominate minerals while pyrite occupies a nontrivial amount as well. The permeability of tight gas sandstones is very low, exhibiting an extremely poor positive correlation with porosity. While pore types and relative pore contents are more influential factors on the permeability, accurate characterization of pore size distribution is critical for the permeability of tight gas sandstones. Therefore, complementary characterization methods are carried out, indicating that neither small pores with radii < 100 nm (around peak 1 in NMR T 2 distribution) nor large pores with radii > 5 μ m (around peak 3 in NMR T 2 distribution) control the permeability by analyzing the connectivity of the pores in various size ranges, but rather pores averaging approximately 350 ± X nm (around peak 2 in NMR T 2 distribution) have sufficient connectivity to host and transmit hydrocarbons. The pore size of tight gas sandstones is dominated by the clay-rich mineral assemblage. The study shows that the NMRC technique can be a very promising method, especially when referred to as a promising “roadmap” on how to interrogate tight formations such as the tight gas sands or even shale especially for the nanopore characterization.

15 GEOTHERMAL ENERGY↗
DOE OSTI2023

Machine learning for automated experimentation in scanning transmission electron microscopy

Abstract Machine learning (ML) has become critical for post-acquisition data analysis in (scanning) transmission electron microscopy, (S)TEM, imaging and spectroscopy. An emerging trend is the transition to real-time analysis and closed-loop microscope operation. The effective use of ML in electron microscopy now requires the development of strategies for microscopy-centric experiment workflow design and optimization. Here, we discuss the associated challenges with the transition to active ML, including sequential data analysis and out-of-distribution drift effects, the requirements for edge operation, local and cloud data storage, and theory in the loop operations. Specifically, we discuss the relative contributions of human scientists and ML agents in the ideation, orchestration, and execution of experimental workflows, as well as the need to develop universal hyper languages that can apply across multiple platforms. These considerations will collectively inform the operationalization of ML in next-generation experimentation.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In-Plane Liftout and Push-to-Pull for In Situ Mechanical Testing of Irradiated Inconel X-750

A streamlined sample preparation method for nanomechanical testing is needed to improve the quality of specimens, reduce the cost, and increase the versatility of specimen fabrication. This work outlines an in-plane liftout focused ion beam (FIB) fabrication procedure to prepare electron-transparent specimens for in situ transmission electron microscopy (TEM) nanomechanical testing. Ion etching and electron backscatter diffraction (EBSD) techniques were used to lift out a [110] oriented grain from a neutron-irradiated bulk X-750 alloy. Careful control of voltages and currents ensured precision. Top surface thinning sweeps prevented resurfacing and redeposition while dog-bone geometries were shaped with a 1:4 gauge width-to-milling pattern diameter ratio. Nanotensile testing in the TEM with a picoindenter allowed for the estimation of an ultimate tensile strength of 2.41 GPa, and inspection revealed a high density of bubbles in the X-750 matrix. The proposed fabrication procedure is significant for preparing samples from radioactive materials, studying complex structures that are orientation-dependent, and analyzing desired planar areas.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Isotope effects in dynamics of water isotopologues induced by core ionization at an x-ray free-electron laser

Dynamical response of water exposed to x-rays is of utmost importance in a wealth of science areas. We exposed isolated water isotopologues to short x-ray pulses from a free-electron laser and detected momenta of all produced ions in coincidence. By combining experimental results and theoretical modeling, we identify significant structural dynamics with characteristic isotope effects in H 2 O 2+ , D 2 O 2+ , and HDO 2+ , such as asymmetric bond elongation and bond-angle opening, leading to two-body or three-body fragmentation on a timescale of a few femtoseconds. A method to disentangle the sequences of events taking place upon the consecutive absorption of two x-ray photons is described. The obtained deep look into structural properties and dynamics of dissociating water isotopologues provides essential insights into the underlying mechanisms.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Measurement of the dynamic charge susceptibility near the charge density wave transition in ErTe 3

A charge density wave (CDW) is a phase of matter characterized by a periodic modulation of valence electron density coupled with lattice distortion. Its formation is closely tied to the dynamical charge susceptibility, χ(q, ω) , which reflects the collective electron dynamics of the material. Despite decades of study, χ(q, ω) near a CDW transition has never been measured at nonzero momentum, q, with meV energy resolution. Here, we investigate the canonical CDW transition in ErTe 3 using momentum-resolved electron energy loss spectroscopy, a technique uniquely sensitive to valence band charge excitations. Unlike phonons, which soften via the Kohn anomaly, we find the electronic excitations exhibit purely relaxational dynamics well described by a diffusive model, with the diffusivity peaking just below the critical temperature, T C1 . Additionally, we report for the first time a divergence in the real part of χ(q, ω) in the static limit (ω → 0), a long-predicted hallmark of CDWs. Unexpectedly, this divergence occurs as T → 0, with only a weak thermodynamic signature at T = T C1 . Our study necessitates a reexamination of the traditional description of CDW formation in quantum materials.

M-EELS↗
DOE OSTI2022

An insight into microscopy and analytical techniques for morphological, structural, chemical, and thermal characterization of cellulose

Cellulose obtained from plants is a bio-polysaccharide and the most abundant organic polymer on earth that has immense household and industrial applications. Hence, the characterization of cellulose is important for determining its appropriate applications. In this article, we review the characterization of cellulose morphology, surface topography using microscopic techniques including optical microscopy, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy. Additionally, other physicochemical characteristics like crystallinity, chemical composition, and thermal properties are studied using techniques including X-ray diffraction, Fourier transform infrared, Raman spectroscopy, nuclear magnetic resonance, differential scanning calorimetry, and thermogravimetric analysis. This review may contribute to the development of using cellulose as a low-cost raw material with anticipated physicochemical properties.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Fuel-cladding chemical interaction of a prototype annular U-10Zr fuel with Fe-12Cr ferritic/martensitic HT-9 cladding

As an alternative fuel form, the annular metallic fuel design eliminates the liquid sodium bond between the fuel and the cladding, providing back-end fuel cycle and other benefits. The fuel-cladding chemical interaction (FCCI) of annular fuel also presents new features. In this work, state-of-the-art electron microscopy and spectroscopy techniques were used to study the FCCI of a prototype annular U-10wt%Zr (U-10Zr) fuel with ferritic/martensitic HT-9 cladding irradiated to 3.3% fission per initial heavy atom. Compared with sodium-bonded solid fuels, negligible amounts of lanthanides were found in the FCCI layer in the investigated helium-bonded annular fuel. Instead, most lanthanides were retained in the newly formed UZr 2 phase in the fuel center region. The interdiffusion of iron and uranium resulted in tetragonal ( U ,Zr) 6 Fe phase (space group I4/mcm) and cubic ( U ,Zr)( Fe ,Cr) 2 phase (space group Fd 3 ¯ m). The ( U ,Zr)( Fe ,Cr) 2 phase contains a high density of voids and intergranular uranium monocarbides of NaCl-type crystal structure (space group Fm 3 ¯ m). At the interdiffusion zone and inner cladding interface, a porous lamellar structure composed of alternating Cr-rich layers and U-rich layers was observed. Next to the lamellar region, the unexpected phase transformation from body-centered cubic ferrite (α-Fe) to tetragonal binary Fe-Cr σ phase (space group P4 2 /mnm) occurred, and tetragonal Fe-Cr-U-Si phase (space group I4/mmm) was identified. Due to the diffusion of carbon into the interdiffusion zone, carbon depletion inside the HT-9 led to the disappearance of the martensite lath structure, and intergranular U-rich carbides formed as a result of the diffusion of uranium into the cladding. These detailed new findings reveal the unique features of the FCCI behavior of annular U-Zr fuels, which could be a promising alternative fuel form for high burnup fast reactor applications.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Mechanochemically Robust LiCoO 2 with Ultrahigh Capacity and Prolonged Cyclability

Pushing intercalation-type cathode materials to their theoretical capacity often suffers from fragile Li-deficient frameworks and severe lattice strain, leading to mechanical failure issues within the crystal structure and fast capacity fading. This is particularly pronounced in layered oxide cathodes because the intrinsic nature of their structures is susceptible to structural degradation with excessive Li extraction, which remains unsolved yet despite attempts involving elemental doping and surface coating strategies. Herein, a mechanochemical strengthening strategy is developed through a gradient disordering structure to address these challenges and push the LiCoO 2 (LCO) layered cathode approaching the capacity limit (256 mAh g -1 , up to 93% of Li utilization). This innovative approach also demonstrates exceptional cyclability and rate capability, as validated in practical Ah-level pouch full cells, surpassing the current performance benchmarks. Comprehensive characterizations with multiscale X-ray, electron diffraction, and imaging techniques unveil that the gradient disordering structure notably diminishes the anisotropic lattice strain and exhibits high fatigue resistance, even under extreme delithiation states and harsh operating voltages. Consequently, this designed LCO cathode impedes the growth and propagation of particle cracks, and mitigates irreversible phase transitions. In conclusion, this work sheds light on promising directions toward next-generation high-energy-density battery materials through structural chemistry design.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Investigation and Suppression of Oxygen Release by LiNi 0.8 Co 0.1 Mn 0.1 O 2 Cathode under Overcharge Conditions

The safety issue of lithium-ion batteries is a crucial factor limiting their large-scale application. Therefore, it is of practical significance to evaluate the impact of their overcharge behavior because of the severe levels of oxygen release of cathode materials during this process. Here, by combining a variety of in situ techniques of spectroscopy and electron microscopy, this work studies the structural degradation of LiNi 0.8 Co 0.1 Mn 0.1 O 2 (NCM811) accompanying the oxygen release in the overcharge process. It is observed that a small amount of O 2 evolves from the initial surface at ≈4.7V. When charging to a higher voltage (≈5.5V), a large amount of O 2 evolves on the newly formed surface due to the occurrence of microcracks. Based on experimental results and theoretical calculations, it is determined that the oxygen release mainly occurs in the near-surface regions, where the remaining oxygen vacancies accumulate to create voids. To suppress the oxygen release, single-crystalline NCM811 with integrated structure is introduced and serves as a cathode, which can effectively inhibit morphology destruction and reduce the activation of lattice oxygen in the surface region. These findings provide a theoretical basis and effective strategy for improving the safety performance of Ni-rich cathode materials in practical applications.

25 ENERGY STORAGE↗
DOE OSTI2022

High performance high-power textured Mn/Cu-doped PIN-PMN-PT ceramics

Piezoelectric ceramics with combinatory soft and hard characteristics are highly desired for high-power applications. However, it remains grand challenge to achieve simultaneous presence of hard (e.g. high coercive field, E c ; high mechanical quality factor, Q m ) and soft (e.g. high piezoelectric constant, d; high electromechanical coupling factor, k) piezoelectric properties in piezoelectric ceramics since the mechanism controlling the hard behavior (pinned domain walls) will significantly reduce the soft behavior. Here, we address this grand challenge and demonstrate <001> textured MnO 2 and CuO co-doped Pb(In 1/2 Nb 1/2 )O 3- Pb(Mg 1/3 Nb 2/3 )O 3- PbTiO 3 (PIN-PMN-PT) ceramics exhibiting ultrahigh combined soft and hard piezoelectric properties (d 33 = 713 pC N –1 , k 31 = 0.52, Q m ≈950, E c = 9.6 kV cm –1 , tan δ = 0.45%). The outstanding electromechanical properties are explained by considering composition/phase selection, crystallographic anisotropy and defect engineering. Phase-field model in conjunction with high resolution electron microscopy and diffraction techniques is utilized to delineate the contributions arising from intrinsic piezoelectric response, domain dynamics, and local structural heterogeneity. Furthermore, these results will have significant impact in the development of high-power transducers and actuators.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Enhanced visible-light-assisted peroxymonosulfate activation on cobalt-doped mesoporous iron oxide for orange II degradation

Sulfate radical-based advanced oxidation processes (SR-AOP) attracted a lot of attention due to their capability and adaptability in wastewater treatment. Although heterogeneous cobalt-based catalysts have been extensively studied and have emerged superior for peroxymonosulfate (PMS) activation, leaching of cobalt is still a major concern. Herein, we report a photo-assisted PMS activation approach using cobalt doped mesoporous iron oxide with exceptional activity and stability up to 7 cycles with very low cobalt leaching (0.5 ppm). The highest activity was obtained by 1 mol % cobalt doped mesoporous iron oxide. Orange II dye was completely degraded by the reactive oxygen species (ROS) generated under visible light irradiation within 1 min. ROS were evaluated using two distinct techniques (Fluorescence probes and Electron Paramagnetic Resonance (EPR). ROS quenching experiments were also used to highlight the dominant pathway. This study correlates the structural and electronic changes induced with cobalt doping to the exceptional activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗