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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 37 records · Page 2

Segregation Behavior of Sulfur and Other Impurities Onto the Free Surfaces of ED-Ni Deposits

Most researchers attribute grain boundary embrittlement in electro-deposited Nickel (ED-Ni) to the presence of small quantities of Sulfur as an impurity. It occurs in a highly mobile form that segregates to the grain boundaries. Evaluation of Sulfur segregation requires that a sample be fractured through the grain boundaries. However, this action may not always be possible. ED-Ni is inherently tough at ambient temperature, especially if a low level of Sulfur was intentionally maintained. A new method was developed to study Sulfur and other migrant species to the grain boundaries, which also migrate to free surfaces. A test specimen is heated by a quartz lamp within the sample preparation chamber, allowing the mobile species to migrate to polished free surfaces. There the mobile species are analyzed using X-ray photoelectron spectroscopy (XPS) also known as Electron Spectroscopy for Chemical Analysis (ESCA).

Panda, Binayak↗

Segregation Behavior of Sulfur and Other Impurities onto the Free Surfaces of ED-NI Deposits

Most researchers attribute grain boundary embrittlement in electro-deposited nickel (ED-Ni) to the presence of small quantities of sulfur as an impurity. It occurs in a highly mobile form that segregates to the grain boundaries. Evaluation of sulfur segregation requires that a sample be fractured through the grain boundaries. However, this action may not always be possible. ED-Ni is inherently tough at ambient temperature, especially if a low level of sulfur was intentionally maintained. A new method was developed to study sulfur and other migrant species to the grain boundaries, which also migrate to free surfaces. A test specimen is heated by a quartz lamp within the sample preparation chamber, allowing the mobile species to migrate to polished free surfaces. There the mobile species are analyzed using X-ray photoelectron spectroscopy (XPS) also known as Electron Spectroscopy for Chemical Analysis (ESCA).

Panda, B.↗

Electrodynamic Dust Shield (EDS) for Firefly Aerospace’s Blue Ghost Mission 1

As part of the NASA Commercial Lunar Payload Services (CLPS) program, the EDS payload is manifested as part of Firefly Aerospace’s Blue Ghost Mission 1. Dust will adversely affect the operation of most mechanical systems required by lunar missions. The EDS payload will demonstrate active lunar dust removal from glass and thermal radiator surfaces.

Alexis Hongamen↗

Atomic-Scale Characterization of Dilute Dopants in Topological Insulators via STEM–EDS Using Registration and Cell Averaging Techniques

Magnetic dopants in three-dimensional topological insulators (TIs) offer a promising avenue for realizing the quantum anomalous Hall effect (QAHE) without the necessity for an external magnetic field. Understanding the relationship between site occupancy of magnetic dopant elements and their effect on macroscopic property is crucial for controlling the QAHE. By combining atomic-scale energy-dispersive X-ray spectroscopy (EDS) maps obtained by aberration-corrected scanning transmission electron microscopy (AC-STEM) and novel data processing methodologies, including semi-automatic lattice averaging and frame registration, we have determined the substitutional sites of Mn atoms within the 1.2% Mn-doped Sb 2 Te 3 crystal. More importantly, the methodology developed in this study extends beyond Mn-doped Sb 2 Te 3 to other quantum materials, traditional semiconductors, and even electron irradiation sensitive materials.

36 MATERIALS SCIENCE↗

The effect of temperature and burnup on U-10Zr metallic fuel chemical interaction with HT-9: A SEM-EDS study

The fuel cladding chemical interaction (FCCI) between Uranium-Zirconium-based metallic fuel and cladding materials during in-pile service is one of the most constraining phenomena affecting the performance of this fuel system. In this study, we investigated the effect of temperature and burnup on the FCCI development in two U-10 wt.% Zr (U-10Zr) fuel samples with HT-9 cladding irradiated as part of the MFF-3 irradiation test in the Fast Flux Test Facility (FFTF). One sample achieved a burnup of 13.1 at.% and operated with an average inner cladding temperature of 530°C, while the other achieved a burnup of 8.5 at.% and was subjected to an average inner cladding temperature of 615°C. Automated scanning electron microscopy (SEM) back-scattered electron (BSE) imaging of entire fuel cross-sections and SEM energy dispersive x-ray spectroscopy (EDS) analysis on specific fuel-cladding interface regions successfully provided a comprehensive characterization of the depth and type of interaction happening under different irradiation conditions. Further, our analysis shows that FCCI development on both fuel and cladding side is strongly influenced by the inner cladding temperature and, to some extent, the formation and integrity of Zr-rich layers between the fuel and cladding, while the impact of burnup and power is negligible. Measured FCCI thicknesses were compared to BISON simulations using both an empirical model based upon legacy data from the Experimental Breeder Reactor II (EBR II) irradiations and a mechanistic model currently under development for the Nuclear Energy Advanced Modeling and Simulation (NEAMS) program, showing satisfactory agreement. Nonetheless, this comparison supports the need for additional microstructural characterization in intermediate ranges of temperature, power, and burnups in prototypic-length pins.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Correlated 4D-STEM and EDS for the classification of fine Beta-precipitates in aluminum alloy AA 6063-T6

Tuning the properties of aluminum alloys AA 6063-T6 involves artificial aging to induce precipitate formation, particularly β’’ and β’ phases. Previous characterization challenges due to their similar appearance are addressed here by correlating 4D scanning transmission electron microscopy (4DSTEM) and energy-dispersive spectroscopy (EDS) mapping. This approach allows us to analyze the structure and composition of precipitates individually, overcoming limitations of conventional imaging and structural analysis techniques when the precipitates appear simultaneously, as is often the case. We present detailed characterizations of needle-shaped Beta precipitates, revealing distinct diffraction patterns (DPs) and compositional differences. The method's applicability extends beyond aluminum alloys, offering a promising strategy for complex composite material characterization with multimodal scanning transmission electron microscopy (STEM) techniques.

36 MATERIALS SCIENCE↗

ED-cPSD: Fast Phase-Size Distribution via Sequential Erosion-Dilation

The Erosion-Dilation continuous Phase-Size Distribution, ED-cPSD, is an application for calculating continuous pore and particle-size distribution from digital reconstructions and/or image-based structural data. It is based on the erosion-dilation continuous phase-size distribution method. A continuous size distribution is a measure of the probability density of finding a particle or pore of a certain size. These distributions are of interest in any field of study involving porous media, including but not limited to electrochemistry, petroleum engineering, geology, and food science. The algorithm behind the software provides a computationally efficient way to calculate phase-size distributions for large domains. For a 3D battery electrode reconstruction with 1.3 x 10 8 voxels, the particle size distribution is derived in under 2 min on a desktop, while also retaining flexibility and computational efficiency for HPC-scale multi-threading. The software can handle structures with over 10 9 voxels. The algorithm is roughly 280 times faster than a previous version on the same task.

Characterization↗

Phosgene Neutralization Chemistry for the Explosive Destruction System (EDS)

This report summarizes activities at Sandia National Laboratories as part of the Explosive Destruction System (EDS) Phase 3 (P3) System design. An exploration of chemical neutralization strategies of phosgene was conducted for safe disposal of recovered mortars and M79 1000 lb. bombs filled with carbonyl dichloride "phosgene" or "CG agent" (molecular formula = COCl 2 ). The incumbent strategy utilized aqueous sodium hydroxide was found to be the worst-case scenario, producing enough CO 2 gas that would cause an unacceptable pressure and temperature spike. Several chemical neutralization strategies were evaluated based on criteria set by the operating envelope of the P3 design. In the end, it was determined that a pure solution of N-methyl ethanolamine (MeEA) or 90% monoethanolamine (MEA)(aqueous) provided the best balance reaction profile, cost, and safety.

36 MATERIALS SCIENCE↗

Inter-year Variability in EDS Standards

This report provides a deep dive into how the stability of energy dispersive spectroscopy (EDS) standards yielded insight into the shortfalls of using software to randomly select points for spectral acquisition when using heterogeneous standards. Some procedural recommendations are included which are meant to minimize the impact of anomalous reference standard spectra by detecting them before the standard is implemented into data processing.

36 MATERIALS SCIENCE↗

SEM-EDS Analyses of Small Craters in Stardust Aluminum Foils: Implications for the Wild-2 Dust Distribution

Aluminium foils were used on Stardust to stabilize the aerogel specimens in the modular collector tray. Part of these foils were fully exposed to the flux of cometary grains emanating from Wild 2. Because the exposed part of these foils had to be harvested before extraction of the aerogel, numerous foil strips some 1.7 mm wide and 13 or 33 mm long were generated during Stardusts's Preliminary Examination (PE). These strips are readily accommodated in their entirety in the sample chambers of modern SEMs, thus providing the opportunity to characterize in situ the size distribution and residue composition - employing EDS methods - of statistically more significant numbers of cometary dust particles compared to aerogel, the latter mandating extensive sample preparation. We describe here the analysis of nearly 300 impact craters and their implications for Wild 2 dust.

Borg, J.↗

Towards Understanding the DO-178C / ED-12C Assurance Case

This paper describes initial work towards building an explicit assurance case for DO-178C / ED-12C. Two specific questions are explored: (1) What are some of the assumptions upon which the guidance in the document relies, and (2) What claims are made concerning test coverage analysis?

Holloway, C M.↗

EDS Analysis of FCCI in AFC-FAST Fuel Pins

The Advanced Fuel Campaign’s Fission Accelerated Steady-state Testing (FAST) program uses metallic fuel pins with small diameters to reach a desired burnup more quickly. This enables accelerated testing of advanced fuel designs and decreases the time between idea conception and commercial usage. Post-irradiation examination is critical in this process, especially with respect to the fuel-cladding chemical interactions (FCCI). In this work, energy dispersive X-ray spectroscopy (EDS) is used to track how elements from the fuel and fission products have diffused through the cladding. Elemental redistribution along the fuel-cladding interface is mapped and FCCI region thicknesses are measured. The correlations between geometry, temperature, burnup, and FCCI thickness are presented.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Cross-section SEM-EDS Analysis of Corroded 316 Steel Samples Using JEOL 6610 SEM

Comparison of SEM images obtained for samples 316H-1, 5, 7, and 10 revealed that samples 1 and 5 were subjected to more corrosion than the other two samples. Pores of an average of 1µm size were also observed scattered near the edge of each sample. Corrosion layer thickness was measured from edge of the corroded surface to the pore region. It was found that 316H-1 and 316H-5 had more corrosion damage with 82.40µm and 100µm respectively. Sample 316H-5 posed a challenge in measuring the corrosion layer thickness due to it breaking off from the parent sample during polishing. Samples 316H-7 and 316H-10 are less corroded with 26.57µm and 39.94µm thickness respectively.

36 - MATERIALS SCIENCE↗

Back Cover: Influence of Intracrystalline Ionic Strength in MFI Zeolites on Aqueous Phase Dehydration of Methylcyclohexanols (Angew. Chem. Int. Ed. 47/2021)

Here the impact of the concentration of hydrated hydronium ions and in turn of the local ionic strength in MFI zeolites has been investigated for the aqueous phase dehydration of 4-methylcyclohexanol (E1 mechanism) and cis-2-methylcyclohexanol (E2 mechanism). The E2 pathway with the latter alcohol led to a 2.5-fold higher activity. The catalytic activity normalized to the hydronium ions (turnover frequency, TOF) passed through a pronounced maximum, which is attributed to the increasing excess chemical potential of the alcohols in the pores, increasing in parallel with the ionic strength and the additional work caused by repulsive interactions and charge separation induced by the bulky alcohols. While the maximum in rate observed is invariant with the mechanism or substitution, the reaction pathway is influencing the activation parameters differently.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigation of Off-Stoichiometry in Ternary Nitrides by EDS and HRTEM

We demonstrate an inverted metamorphic multijunction (IMM) photovoltaic cell comprising lattice-mismatched 1.2 eV AlGaInAs and 1.0 eV GaInAs junctions optimized for high-temperature thermophotovoltaic (TPV) applications. This device differs from traditional IMM solar cells because the mismatched junctions are grown at a single lattice constant. This architecture enables removal of the compositionally graded buffer which otherwise filters light from the junctions below and absorbs sub-bandgap light via free-carrier absorption. Sub-bandgap absorption dramatically reduces the efficiency of TPV systems using high reflectivity cells to enable bandedge spectrum filtering. Three components required development to enable this device: 1) a lattice-mismatched 1.2 eV AlGaInAs junction, 2) a metamorphic contact layer grown after the graded buffer, and 3) a transparent tunnel junction that sits in front of the 1.0 eV GaInAs junction. Growth conditions that minimize oxygen defect incorporation maximize AlGaInAs cell quality, enabling a 0.41 V bandgap open circuit voltage offset at 22 mA/cm2 under AM1.5D. A mismatched GaInAs:Se layer is developed as a low resistance contact. Lastly we develop a GaAsSb:C/GaInP:Se tunnel junction suitable for high-power densities with more transparency than the GaAsSb:C/GaInP:Se structure used in past IMM cells. We characterize the tandem device under a high-intensity spectrum that approximates the emission from a 2150 °C blackbody radiator and deduce a projected ideal TPV efficiency of 39.9% at ~30% of the blackbody irradiance, and 36% ideal TPV efficiency under the full 118 W/cm2 irradiance. Improvements to the back-surface reflectivity and series resistance are expected to increase the ideal TPV efficiency well above 40%.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗