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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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29 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Multiscale Cryo Electron Microscopy Reveals Interfacial Degradation and Stabilization in Battery Electrodes

Electrochemical interfaces are dynamic systems, evolving based on their local environment and reactant surface structures. The electrode-electrolyte interface in Li-ion batteries can be protective, limiting parasitic reactions with the electrolyte to passivate the surface [1]. Additionally, this interphase has an impact on the Li-ion transport through that layer based on its composition, bonding environment, and thickness. These parameters are challenging to collect and may vary depending on the electrode surface site investigated relative to its spatial position in a coin cell. This study will detail a multiscale cryogenic electron microscopy approach where millimeter-scale cross-sections through the coin cell batteries were made using a cryogenic stage within a fs-laser plasma focused ion beam (laser PFIB) with complementary energy dispersive X-ray spectroscopy able to detect variations in the composition at electrode interfaces [2]. Microscale cross-sectioning and lamella sample preparation of battery electrodes was conducted at the Center for Integrated Nanotechnologies using a Ga-ion focused ion beam (FIB) with air-free and cryo-transfer [3], followed by nanoscale mapping of composition and bonding within the CEI through cryo-scanning transmission electron microscopy (cryo-STEM) electron energy loss spectroscopy [4]. This multiscale approach enabled identification of millimeter-scale features of a battery stack with visualization of degradation in electrodes such as cracks in cathode particles, gas evolution, and SEI evolution; microscale interfacial characteristics, such as heterogeneity in the SEI or barrier layer and identification of electrolyte networks to the electrode surfaces; and nanoscale measurement of the CEI thickness, mapping of transition metal bonding within the cathode particles to identify loss of active materials, and identification of beneficial electrolyte additives incorporated into the CEI structure. This multiscale approach allows for a statistical understanding of the primary mechanisms and parasitic degradation pathways that impact performance by limiting the ion transport pathways within Li+ batteries.

36 MATERIALS SCIENCE↗
NASA NTRS2017

Experimental Hypervelocity Dust Impact in Olivine: FIB/TEM Characterization of Micron-Scale Craters with Comparison to Natural and Laser-Simulated Small-Scale Impact Effects

The space weathering of regoliths on airless bodies and the formation of their exospheres is driven to a large extent by hypervelocity impacts from the high relative flux of micron to sub-micron meteoroids that comprise approximately 90 percent of the solar system meteoroid population. Laboratory hypervelocity impact experiments are crucial for quantifying how these small impact events drive space weathering through target shock, melting and vaporization. Simulating these small scale impacts experimentally is challenging because the natural impactors are both very small and many have velocities above the approximately 8 kilometers-per-second limit attainable by conventional chemical/light gas accelerator technology. Electrostatic "dust" accelerators, such as the one recently developed at the Colorado Center for Lunar Dust and Atmospheric Studies (CCLDAS), allow the experimental velocity regime to be extended up to tens of kilometers-per-second. Even at these velocities the region of latent target damage created by each impact, in the form of microcraters or pits, is still only about 0.1 to 10 micrometers in size. Both field-emission analytical scanning electron microscopy (FE-SEM) and advanced field-emission scanning transmission electron microscopy (FE-STEM) are uniquely suited for characterizing the individual dust impact sites in these experiments. In this study, we have used both techniques, along with focused ion beam (FIB) sample preparation, to characterize the micrometer to nanometer scale effects created by accelerated dust impacts into olivine single crystals. To our knowledge this work presents the first TEM-scale characterization of dust impacts into a key solar system silicate mineral using the CCLDAS facility. Our overarching goal for this work is to establish a basis to compare with our previous results on natural dust-impacted lunar olivine and laser-irradiated olivine.

Christoffersen, R.↗
DOE OSTI2024

Proton surface exchange kinetics of perovskite triple conducting thin films for protonic ceramic electrolysis cells: BaPr 0.9 Y 0.1 O 3–δ (BPY) vs. Ba 1–x Co 0.4 Fe 0.4 Zr 0.1 Y 0.1 O 3–δ (BCFZY)

Protonic ceramic electrolysis cells (PCECs) are an attractive green H 2 production technology, given their intermediate-temperature operating range and ability to produce dry H 2 . However, PCECs will benefit from development of more efficient and durable “triple conducting” anodes where steam is split, H incorporated, and oxygen evolved. In this work, we evaluated the kinetics of the steam-splitting/H incorporation reaction on BaPr 0.9 Y 0.1 O 3–δ (BPY) in comparison to the benchmark Ba 1–x Co 0.4 Fe 0.4 Z r0.1 Y 0.1 O 3–δ (BCFZY) composition, replacing most of the transition metal elements (Co, Fe, Zr) with the lanthanide Pr. We prepared geometrically well-defined perovskite BPY and BCFZY thin films by pulsed laser deposition and performed simultaneous optical transmission relaxation and electrical conductivity relaxation measurements at 400–500 °C in 0.21 atm O 2 during switching of the steam partial pressure to isolate and compare their proton surface exchange coefficients (k). The k values of BPY were comparable to those of BCFZY and more stable over time. According to angle-resolved XPS and STEM-EDS mapping of FIB cross-sections, the surface of BPY exhibited Ba enrichment, Pr deficiency, and Si contamination. In contrast, BCFZY exhibited Ba deficiency throughout, no obvious surface segregation, and less Si contamination. The Ba segregation on the BPY film appears to have promoted steam splitting/H incorporation kinetics even though the more basic surface reacted with the acidic environmental SiO x H y . Faster kinetics observed on stoichiometric BCFZY vs. Ba-deficient BCFZY confirmed the benefit of a high A-site Ba concentration. This result contrasts with most work on perovskites applied in solid oxide electrolysis cell anodes, in which A-site segregation is considered deleterious for surface reaction kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2012

Characterization of 4H <000-1> Silicon Carbide Films Grown by Solvent-Laser Heated Floating Zone

Commercially available bulk silicon carbide (SiC) has a high number (>2000/sq cm) of screw dislocations (SD) that have been linked to degradation of high-field power device electrical performance properties. Researchers at the NASA Glenn Research Center have proposed a method to mass-produce significantly higher quality bulk SiC. In order for this bulk growth method to become reality, growth of long single crystal SiC fibers must first be achieved. Therefore, a new growth method, Solvent-Laser Heated Floating Zone (Solvent-LHFZ), has been implemented. While some of the initial Solvent-LHFZ results have recently been reported, this paper focuses on further characterization of grown crystals and their growth fronts. To this end, secondary ion mass spectroscopy (SIMS) depth profiles, cross section analysis by focused ion beam (FIB) milling and mechanical polishing, and orientation and structural characterization by x-ray transmission Laue diffraction patterns and x-ray topography were used. Results paint a picture of a chaotic growth front, with Fe incorporation dependant on C concentration.

Woodworth, Andrew, A↗
DOE OSTI2024

Optimal Geometry for Focused Ion Beam-Milled Samples for Direct-Pull Micro-Tensile Testing Performed In Situ in a Scanning Electron Microscope

A thorough procedure was developed to efficiently manufacture dogbone samples using focused ion beam (FIB) milling for micro-tensile testing. A Bruker PI 89 PicoIndenter, Billerica, MA, USA, was used as a case study, although the analysis and results are applicable to other micro-mechanical testing systems capable of mounting a standard, Ø12.7 mm × Ø3.2 mm pin, scanning electron microscopy (SEM) pin stub (Ted Pella, Redding, CA, USA). Nine dogbones were made from an Fe-45Cu alloy additively manufactured using powder-fed laser-directed energy deposition (DED-LB). Testing showed that fracture was confined to the gauge section for all dogbones and that the fracture mode, ductile vs. brittle, was entirely dependent on the grain orientation relative to the loading direction. The analysis showed that the measured plastic strain to failure can vary from >11% (optimal geometry) to <1% (non-optimal geometry) in micro-tensile testing of high-tensile-strength (>1 GPa) metallic materials. Subsequently, a finite element analysis (FEA) was conducted to identify the improved dogbone geometries. A total of ten thousand dogbone geometries were tested, and their dimensions were defined by a set of four adjustable parameters (corner radius, load surface angle, load surface length, and dogbone head length). The gauge width and gauge length were fixed to 4 µm and 10 µm, respectively. Three-dimensional surface plots of the stress concentration as a function of two parameters were used to identify the optimal ranges of parameter values. The addition of maximum width and length constraints, measuring 25 µm and 30 µm, respectively, allowed us to identify an optimal geometry at load surface angles of 30° and 45°. Their respective dimensions (corner radius, load surface length, and dogbone head length) are, in µm, 12, 6, and 7 and 10, 7, and 7. Testing these two optimal geometries with a range of gauge lengths from 4 to 20 µm showed that smaller gauge lengths only slightly reduced the detrimental stress concentration outside the gauge section. However, smaller gauge lengths will notably improve the FIB surface polishing step as tapering is reduced with smaller dogbone lengths.

Chemistry↗
NASA NTRS2010

Metal/Silicate Partitioning at High Pressures and Temperatures

The behavior of siderophile elements during metal-silicate segregation, and their resulting distributions provide insight into core formation processes. Determination of partition coefficients allows the calculation of element distributions that can be compared to established values of element abundances in the silicate (mantle) and metallic (core) portions of the Earth. Moderately siderophile elements, including W, are particularly useful in constraining core formation conditions because they are sensitive to variations in T, P, oxygen fugacity (fO2), and silicate composition. To constrain the effect of pressure on W metal/silicate partitioning, we performed experiments at high pressures and temperatures using a multi anvil press (MAP) at NASA Johnson Space Center and laser-heated diamond anvil cells (LHDAC) at the University of Maryland. Starting materials consisted of natural peridotite mixed with Fe and W metals. Pressure conditions in the MAP experiments ranged from 10 to 16 GPa at 2400 K. Pressures in the LHDAC experiments ranged from 26 to 58 GPa, and peak temperatures ranged up to 5000 K. LHDAC experimental run products were sectioned by focused ion beam (FIB) at NASA JSC. Run products were analyzed by electron microprobe using wavelength dispersive spectroscopy. Liquid metal/liquid silicate partition coefficients for W were calculated from element abundances determined by microprobe analyses, and corrected to a common fO2 condition of IW-2 assuming +4 valence for W. Within analytical uncertainties, W partitioning shows a flat trend with increasing pressure from 10 to 16 GPa. At higher pressures, W becomes more siderophile, with an increase in partition coefficient of approximately 0.5 log units.

Shofner, G.↗
NASA NTRS2013

Miniature Trace Gas Detector Based on Microfabricated Optical Resonators

While a variety of techniques exist to monitor trace gases, methods relying on absorption of laser light are the most commonly used in terrestrial applications. Cavity-enhanced absorption techniques typically use high-reflectivity mirrors to form a resonant cavity, inside of which a sample gas can be analyzed. The effective absorption length is augmented by the cavity's high quality factor, or Q, because the light reflects many times between the mirrors. The sensitivity of such mirror-based sensors scales with size, generally making them somewhat bulky in volume. Also, specialized coatings for the high-reflectivity mirrors have limited bandwidth (typically just a few nanometers), and the delicate mirror surfaces can easily be degraded by dust or chemical films. As a highly sensitive and compact alternative, JPL is developing a novel trace gas sensor based on a monolithic optical resonator structure that has been modified such that a gas sample can be directly injected into the cavity. This device concept combines ultra-high Q optical whispering gallery mode resonators (WGMR) with microfabrication technology used in the semiconductor industry. For direct access to the optical mode inside a resonator, material can be precisely milled from its perimeter, creating an open gap within the WGMR. Within this open notch, the full optical mode of the resonator can be accessed. While this modification may limit the obtainable Q, calculations show that the reduction is not significant enough to outweigh its utility for trace gas detection. The notch can be milled from the high- Q crystalline WGMR with a focused ion beam (FIB) instrument with resolution much finer than an optical wavelength, thereby minimizing scattering losses and preserving the optical quality. Initial experimental demonstrations have shown that these opened cavities still support high-Q whispering gallery modes. This technology could provide ultrasensitive detection of a variety of molecular species in an extremely compact and robust package. With this type of modified WGMR, one can inject a gas sample into the open gap, allowing highly sensitive trace molecule detection within a roughly 1-cm volume. Other critical components of the instrument, such as the detector and a semiconductor laser, could be directly packaged with the resonator so as to not significantly increase the size of the device. Besides its low mass, volume, and power consumption, the monolithic design makes these resonators intrinsically robust devices, capable of handling significant temperature excursions, without moving parts to wear out or delicate coatings that can be easily damaged. A sensor could integrate with microfluidics technology for a chip-scale device. It could be mounted to the end of a deployable arm, or inserted into a borehole. Also, a network of individual sensors could be dispersed to monitor conditions over a wide region

Aveline, David C.↗
NASA NTRS2005

Ultrasonic Micro-Blades for the Rapid Extraction of Impact Tracks from Aerogel

The science return of NASA's Stardust Mission with its valuable cargo of cometary debris hinges on the ability to efficiently extract particles from silica aerogel collectors. The current method for extracting cosmic dust impact tracks is a mature procedure involving sequential perforation of the aerogel with glass needles on computer controlled micromanipulators. This method is highly successful at removing well-defined aerogel fragments of reasonable optical clarity while causing minimal damage to the surrounding aerogel collector tile. Such a system will be adopted by the JSC Astromaterials Curation Facility in anticipation of Stardust s arrival in early 2006. In addition to Stardust, aerogel is a possible collector for future sample return missions and is used for capture of hypervelocity ejecta in high power laser experiments of interest to LLNL. Researchers will be eager to obtain Stardust samples for study as quickly as possible, and rapid extraction tools requiring little construction, training, or investment would be an attractive asset. To this end, we have experimented with micro-blades for the Stardust impact track extraction process. Our ultimate goal is a rapid extraction system in a clean electron beam environment, such as an SEM or dual-beam FIB, for in situ sample preparation, mounting and analysis.

Ishii, H. A.↗
DOE OSTI2025

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗
DOE OSTI2021

Transformations of Ti-5Al-5V-5Cr-3Mo powder due to reuse in laser powder bed fusion: A surface analytical approach

Reactive Ti-5Al-5 V-5Cr-3Mo (Ti5553) alloy feedstock powder is used in laser powder-bed fusion (LPBF). Due to the large quantity of powder necessary for LPBF, powder is reused numerous times under oxidizing environments. Transformations to the powder’s native surface oxide may impact the LPBF process and lead to deviations from expected behavior of printed parts. In this work, we present a multimodal characterization of new and reused powder by combining X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS), and transmission electron microscopy (TEM) of focused ion beam (FIB)-prepared cross sections of individual powder particles to understand how the surface oxide composition changes, grows, and becomes hydroxylated and hydrated due to reuse. We show that the native oxide film of Ti5553 powder is a hydroxylated mixed oxide composed of TiO 2 and Al 2 O 3 that grows from 5.6 +/- 0.7 nm to 8.3 +/- 1.1 nm due to reuse. Al oxide regions of the surface oxide become more hydroxylated during reuse in comparison to Ti oxide regions. This indicates that an outer oxide of pure TiO 2 may enhance recyclability of Ti5553 powder while the presence of Al oxides may decrease recyclability. Further characterization of surface transformations due to recyclability may eliminate unnecessary variation in LPBF.

36 MATERIALS SCIENCE↗
DOE OSTI2025

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↗