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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 307 records · Page 17

Three-dimensional bubble reconstruction in high burnup UO 2

In light water reactor (LWR) UO 2 fuels, the evolution of volatile fission products is one of the critical areas of fuel behavior that is yet to be fully understood. In UO 2 irradiated to high burnups, it is well known that most released fission gases come from the central region of the fuel as opposed to the highly porous high burnup structure (HBS) on the periphery of the pellets. However, fuels with and without interconnected bubble networks at the fuel center showed high to moderate release fractions, which conceals the mechanisms responsible for the gas release in the latter scenario. In this work, focused ion beam tomography was used to investigate the three-dimensional bubble structure in an irradiated LWR UO 2 fuel pellet with high degree of fission gas retention so that the degree of bubble interconnection could be assessed. Six radial locations with different burnups and temperatures were serially sectioned and imaged to reconstruct the three-dimensional bubble structure. As expected, the highest porosity was observed at the periphery of the fuel (HBS). Here, the porosity then decreased towards the pellet center, except for the centermost location. This location had a slightly higher porosity than its adjacent mid-radial location, which was attributed to the temperature difference between the two locations. This study provides a first-time volumetric evaluation of the porosity at different radial locations on a UO 2 fuel pellet. During this investigation, no significant bubble interconnection was noted at any of the six radial locations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Oxide evolution on the SiC layer of TRISO particles during extended air oxidation

Tristructural isotropic (TRISO) fuel particles have been primarily developed for high-temperature gas-cooled nuclear reactors and can be subjected to oxidizing environments for extended periods in an off-normal accident scenario. Surrogate TRISO fuel particles were oxidized in air at 1,000 or 1,100 °C for up to 120 h. Here, the oxide scale morphology and thickness were studied via scanning electron microscopy, focused ion beam, and atomic force microscopy. TRISO particles oxidized at 1,100 °C exhibited a highly crystalline oxide scale, which led to significant cracking and irregularly shaped closed porosity, whereas those oxidized at 1,000 °C possessed a primarily amorphous oxide scale, which contained small, rounded internal pores and no larger defects. The observed phenomena deviated from the expected behavior based on models for oxide growth on flat-plate and fiber SiC. The oxidation kinetics of TRISO fuel particles in high-temperature air were investigated without mechanically deforming the surface and were analyzed with respect to oxide morphology.

36 MATERIALS SCIENCE↗

Determining the tensile strength of fuel surrogate TRISO-coated particle buffer, IPyC, and buffer-IPyC interlayer regions

A novel micro tensile sample fabrication technique for determining the tensile strength of the buffer, IPyC, and buffer -IPyC interlayer regions of surrogate (ZrO2) TRISO fuel particle layers was refined and implemented. Copper micro tensile samples served as baseline materials to verify the methods used. Tensile tests performed in this study, while limited in number, were analyzed using standard and Weibull statistics. As expected, the buffer layer was weakest, with an average ultimate tensile strength of 138.70 MPa, and the IPyC layer samples, were strongest, with an average ultimate tensile strength of 189.74 MPa. In the buffer -IPyC interface samples, all breaks occurred in the buffer region, though the average ultimate tensile strength of the samples, 159.80 MPa, was between the pure buffer and IPyC samples. These results suggest the interlayer region has unique properties, perhaps associated with pyrocarbon infiltration into the buffer layer during particle coating. All interlayer samples fractured within the buffer side; however, the stress strain behavior of some of these samples resembled the behavior of the IPyC layer samples. Here, the buffer and IPyC layer strengths had a normal distribution under Weibull analysis, while the interlayer region had a Rayleigh distribution. Further testing is needed to clarify both the standard and Weibull statistical results

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Micro-tensile characteristics of As-fabricated and irradiated AGR-2 TRISO fuel particle buffer, IPyC, and buffer-IPyC interlayer regions

A recently developed micro-tensile sample preparation technique was implemented to evaluate the tensile strengths of the buffer, IPyC, and buffer-IPyC interlayer regions of the unirradiated and irradiated AGR-2 TRISO fuel particles. Understanding the mechanical properties of the buffer-IPyC interlayer is essential for developing thermomechanical models of buffer-IPyC separation, yet there is a lack of experimental data on its micro-tensile properties. TEM analysis was conducted on these regions to determine the microstructural changes relevant to the samples' tensile properties. In the unirradiated TRISO particle samples, the buffer layer demonstrated the weakest tensile strength, while the IPyC layer exhibited the highest. Conversely, in the irradiated TRISO particle samples, the buffer-IPyC interlayer region showed the lowest tensile strength, with the IPyC layer being the strongest. Fractures in the samples from the buffer-IPyC region predominantly occurred either in the buffer layer or at the buffer-IPyC interface. However, some buffer-IPyC interlayer samples displayed stress-strain and fracture behaviors more akin to the IPyC layer than the buffer layer. Analysis of diffraction patterns suggests that irradiation may have increased anisotropy in the three regions tested. Despite this suggested increase in anisotropy, there was no evidence that it affected the measured strengths. The irradiated TRISO particles demonstrated a considerable increase in void space and a decrease in ultimate tensile strength within the buffer-IPyC interlayer region due to the densification and contraction of the buffer layer. Minor variations in diffraction ring patterns were also observed. These changes, coupled with a significant reduction in the Weibull modulus/shape parameter, imply that irradiation-induced densification leads to tearing between the buffer and IPyC layers at locations of elevated porosity in the buffer-IPyC interlayer region.

Tristructural isotropic (TRISO)↗

Mapping the Microhardness of Al Matrix in U-7Mo/Al Dispersion Fuels at Medium and High Burn-up by in situ Nanoindentation

The mechanical degradation of the Al matrix in U-7Mo dispersion fuels was detected after irradiation in previous studies, but more details of the degradation mechanism are not clear yet to clarify the root cause. In this study, microhardness mapping in fresh and irradiated U-7Mo dispersion fuels coated with ZrN, with burn-up of 3.35 × 10 21 and 6.28 × 10 21 f/cm 3 , are measured to reveal the hardening of the Al matrix as a function of distance to fuel particles. Micro cubes were pulled by plasma focused ion beam scanning electron microscopy and tested by in situ nanoindenter with Berkovitch tip. Size effects are measured in medium and high burn-up samples. The higher burn-up specimen exhibits a more pronounced size effect when indent load is lower than 20 mN. Size effect correction models are also calculated by plots fitting, which predicts the true microhardness without size effect. Results shows that the hardness of the Al matrix near the ZrN coating has the highest value, then decreases moving away from the coating and become stable when the distance reaches ∼10 µm. The hardness starts increasing again getting closer to the next fuel particle, which makes the hardness distribution between two fuel particles to be “U” shape.

36 - MATERIALS SCIENCE↗

New frontiers in atom probe tomography: a review of research enabled by cryo and/or vacuum transfer systems

There has been a recent surge in the use of cryo and/or vacuum specimen preparation and transfer systems that are broadening the scope of research enabled by the microscopy technique of atom probe tomography. This is driven by the fact that, like for many microscopes, the application of atom probe to air and temperature sensitive materials or wet biological specimens has previously been limited by through-air-transfer and through-vacuum-transfer at room temperature. Here we provide an overview of the critical areas of research that require these new transfer and analysis protocols, as well as a review of current advances in transfer devices, environmental cells and glove boxes for controlled sample manipulation. This includes the study of catalysis and corrosion, the application of atom probe to biological samples, the study of liquid-solid interfaces, natural ageing investigations and the analysis of hydrogen in metals.

36 MATERIALS SCIENCE↗

Microscale spatial distribution and soil organic matter persistence in top and subsoil

The spatial distribution of organic substrates and microscale soil heterogeneity significantly influence organic matter (OM) persistence as constraints on OM accessibility to microorganisms. However, it is unclear how changes in OM spatial heterogeneity driven by factors such as soil depth affect the relative importance of substrate spatial distribution on OM persistence. This work evaluated the decomposition and persistence of 13 C and 15 N labeled water-extractable OM inputs over 50 days as either hotspot (i.e., pelleted in 1–2 mm-size pieces) or distributed (i.e., added as OM < 0.07 μm suspended in water) forms in topsoil (0–0.2 m) and subsoil (0.8–0.9 m) samples of an Andisol. We observed greater persistence of added C in the subsoil with distributed OM inputs relative to hotspot OM, indicated by a 17% reduction in cumulative mineralization of the added C and a 10% higher conversion to mineral-associated OM. A lower substrate availability potentially reduced mineralization due to OM dispersion throughout the soil. NanoSIMS (nanoscale secondary ion mass spectrometry) analysis identified organo-mineral associations on cross-sectioned aggregate interiors in the subsoil. On the other hand, in the topsoil, we did not observe significant differences in the persistence of OM, suggesting that the large amounts of particulate OM already present in the soil outweighed the influence of added OM spatial distribution. Here, we demonstrated under laboratory conditions that the spatial distribution of fresh OM input alone significantly affected the decomposition and persistence of OM inputs in the subsoil. On the other hand, spatial distribution seems to play a lower role in topsoils rich in particulate OM. The divergence in the influence of OM spatial distribution between the top and subsoil is likely driven by differences in soil mineralogy and OM composition.

59 BASIC BIOLOGICAL SCIENCES↗

Tomographic assessment of peening for metallurgical bonding in cold spray

It is widely asserted that peening densifies cold spray coatings and improves particle–particle and particle–substrate bonding, yet systematic studies analyzing the evolution of bonding due to peening particle strikes are scarce. We explore peening at the level of individual particle impacts, by creating two-particle Cu-on-Cu stacks using laser-induced particle impact testing. Exploring impact velocities that range from the onset of bonding at the “critical velocity”, V cr , to its peak near 1.4⋅V cr , we perform full 3D tomography of the particle stacks to characterize the bonding state at the particle-substrate interface. Direct labeling of non-bonded patches and the total particle-substrate interface permits quantification and comparison of bonding in single impacts with bonding after subsequent impacts to reveal the origins of the peening effect. The data reveal a surprising finding: although a second impact directly atop the first particle increases the area of the particle-substrate interface (~40% area increase), there is no improvement in metallurgical bonding. Analysis of these data suggest that not only area expansion (and associated oxide rarefication), but also stress-induced extrusion of metal at that interface needs to occur to achieve metal-on-metal contact to see an enhancement in bonding. Furthermore, our analysis suggests that the subsequent impacting particle needs to have ~70% more kinetic energy to produce additional bonding; this implies that particle and velocity distributions within a spray may be helpful, and that peening may rely on unaligned impacts.

Bonding↗

Electro-Chemo-Mechanical Evolution at the Garnet Solid Electrolyte–Cathode Interface

Solid-state batteries promise higher energy density and improved safety compared with lithium-ion batteries. However, electro-chemomechanical instabilities at the solid electrolyte interface with the cathode and the anode hinder their large scale implementation. Here, in this study, we focus on resolving electro-chemo-mechanical instability mechanisms and their onset conditions between a state-of-the-art cathode, LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and the garnet Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte. We used thin-film NMC622 on LLZO pellets to place the interfacial region within the detection depth of the X-ray characterization techniques. The experimental probes of the near-interface region included in operando X-ray absorption spectroscopy and ex situ focused ion beam scanning electron microscopy. Electrochemical degradation was not observable during cycling at room temperature with 4.3 V versus Li/Li + charge voltage cutoff, or with stepwise potentiostatic hold up to 4.1 V versus Li/Li + . In contrast, secondary phases including reduced transition metal species (Ni 2+ , Co 2+ ) were found after cycling up to 4.3 V versus Li/Li + at 80 °C and during potentiostatic hold at 4.3 V versus Li/Li + (Ni 2+ ). Intergranular cracks between NMC622 grains and delamination at the NMC622|LLZO interface occurred readily after the first charge. These interface reaction products and mechanical failure lowered the capacity and cell efficiency due to partial loss of the NMC622 phase, partial loss of contact at the interface, and a higher polarization resistance. Electrochemical instability between delithiated NMC622 and LLZO could be mitigated by using a low charge voltage cutoff or cycling at lower temperature. Ways to engineer the mechanical properties to avoid crack deflection and delamination at the interface are also discussed for enhancing mechanical stability.

36 MATERIALS SCIENCE↗

Carbonate-Metal Reactions in the Lower Mantle

Carbonates are important carbon-bearing phases in the mantle. While their role in upper mantle petrologic processes has been well studied, their effect on phase relations, melting, and transport properties in the lower mantle is less understood. The stability of carbonates in the mantle depends on a host of factors, including pressure, temperature, oxygen fugacity, and reactions with surrounding mantle phases. To understand the stability of carbonates in the presence of metal in the lower mantle, carbonate-metal reaction experiments on the Fe–Si–Ca–Mg–C–O system were conducted up to 124 GPa and 3200 K. We find that carbonates react with iron alloys to form silicates, iron carbides, and oxides. However, the temperature at which these reactions occur increases with pressure, indicating that along a geotherm in the lowermost mantle carbonates are the stable carbon-bearing phase. Carbon is found to be less siderophilic at high-pressure compared to silicon.

58 GEOSCIENCES↗

Effect of a Cr-rich surface layer on D retention in various RAFM steels

In this work, deuterium (D) retention is compared between various reduced-activation ferritic/martensitic steels, including CLF-1, Eurofer, F82H, and Rusfer, exposed to pure D plasma (ion flux ~1.5–2 × 10 21 m -2 s -1 , fluence, &straightphi; D , ~1 × 10 25 m -2 , sample temperature ~373 K, and incident ion energy ~100 eV). It is found that there is a large difference (up to ~30x) in the D retention between CLF-1 and F82H even with the same plasma exposure condition and similar nominal composition. The &straightphi; D dependence of the D retention exhibits a peculiar, counterintuitive feature: the D retention decreases with an increase in &straightphi; D from 2 × 10 23 m -2 to 1 × 10 25 m -2 . Surface analyses reveal that a Cr-rich surface layer is formed during outgassing at 773 K for 1 h before plasma exposure, and that there exists a clear correlation between the D retention and the Cr content in the surface layer.

36 MATERIALS SCIENCE↗

Advancing Cross-Sectional Scanning Electron Microscopy of Perovskite Solar Cells

Organic–inorganic perovskites are an emerging class of photovoltaic materials. Despite achieving power conversion efficiencies surpassing 26%, the challenge of perovskite stability including degradation during exposure to operational conditions such as light, heat, humidity, water, oxygen, and electric fields is well known. Related, perovskite instability has limited high-resolution electron imaging and characterization techniques that can be used for understanding degradation mechanisms. Furthermore, we demonstrate perovskite device cross-section preparation using mechanical polishing in a water-free environment with cryogenic Ar ion milling. Scanning electron microscopy was then used in both backscattered electron and secondary electron imaging modes to obtain information about layer structure, grain aggregate structure, and compositional heterogeneity. Monte Carlo CASINO simulations inform optimum beam conditions and image acquisition parameters and the effects of accelerating voltage, dwell times, and frame averaging for practical image acquisition are reported.

14 SOLAR ENERGY↗

Final Report: Performance-structure characterization to improve REBCO Fusion conductor production at SuperPower

Several companies have used ReBCO tapes to make magnets operating at 20 K, at magnetic fields up to 20T suitable for plasma confining for controlled fusion applications. The transport properties of ReBCO conductors should be optimized for such conditions. NHMFL is one of the few laboratories where such tests can be accomplished. Recently, SuperPower Inc. came up with a new product, REBCO MOCVD HM tape, optimized for plasma confining applications. These HM tapes are designed to have increased critical currents at intermediate temperatures of 4.2K

36 MATERIALS SCIENCE↗

MEMS for Space Flight Applications

Micro-Electrical Mechanical Systems (MEMS) are entering the stage of design and verification to demonstrate the utility of the technology for a wide range of applications including sensors and actuators for military, space, medical, industrial, consumer, automotive and instrumentation products.

AFM infrared microscopy IR light emission microsco↗