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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Recent Developments in Femtosecond Laser-Enabled TriBeam Systems

Streams of multimodal three-dimensional (3D) and four-dimensional (4D) data are revolutionizing our ability to design and predict the behavior of a broad array of advanced materials systems. Over the last 10 years, a new 3D imaging platform consisting of a femtosecond (fs) pulsed laser coupled with a focused ion beam scanning electron microscope (FIB SEM) has been developed by UC Santa Barbara in collaboration with Thermo Fisher Scientific (formerly FEI). The femtosecond-laser-enabled FIB SEM, called the TriBeam, has become one of the only 3D serial sectioning methods available that can gather millimeter-scaled multimodal datasets at sub-μm voxel resolutions; these length scales are critical for many materials problems. Multimodal chemical, crystallographic, and morphological information can be gathered rapidly on a layer-by-layer basis and reconstructed in 3D. Large (gigabyte to terabyte scale) 3D datasets have been generated for a broad array of materials systems, including metallic alloys, ceramics, biomaterials, polymer- and ceramic-matrix composites, and semiconductors. The research tasks conducted have resulted in a completely new design, operating with a dual-wavelength femtosecond-pulsed laser on a plasma focused ion beam (PFIB) platform.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Focused ion beam deposited carbon-platinum nanowires for cryogenic resistive thermometry

The study of thermal effects, both classical and quantum, at cryogenic temperatures requires the use of on-chip, local, high-sensitivity thermometry. Carbon-platinum composites fabricated using focused ion beam (FIB) assisted deposition form a granular structure which is shown in this study to be uniquely suited for this application. Carbon-platinum thermometers deposited using a 24 pA ion beam current have high sensitivities below 1 K, comparable to the best cryogenic thermometers. In addition, these thermometers can be accurately placed to within 10s of nanometers on the chip using a mask-free process. Furthermore, they also have a weak magnetic field dependence, 3% change in resistance with applied magnetic fields from 0 to 8 T. Finally, these thermometers are integrable into a variety of nanoscale devices due to the existing wide spread use of FIB.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

Evidence of an oxidation induced phase transformation for a delta phase plutonium-gallium alloy

The oxidation of an ~1.5 at% Ga plutonium metal alloy in dry air as a function of time was studied using a combination of FIB-SEM, AES, and XRD. Analysis of SEM images of FIB cross-sections of the oxide allowed for direct measurement of the oxide thickness as well as determination of heterogeneity in the extent of the oxide. AES analysis performed on cross-sections of the oxide allowed for quantitative analysis of the atomic composition and semi-quantitative analysis of the chemical composition. Initial preparation of the sample was found to induce a martensitic transformation to α' - Pu with an average thickness of 233 nm. Electropolishing was found to be sufficient to fully remove the α' layer with creation of only a minimum oxide layer. Growth of the oxide in dry air was found to initially follow parabolic kinetics, with a parabolic rate constant orders of magnitude higher than expected for δ-Pu but in-line with values extrapolated to room temperature for α-Pu. Following complete oxidation of the initial α` layer, further regions of plutonium metal depleted in gallium were observed to form at the oxide / metal interface. However, gallium, as Ga 2 O 3 , was found to be enriched at the surface and present in the oxide in an amount comparable to the relative Ga:Pu ratio of the bulk metal alloy. Finally, the results presented here serve to bridge a diverse array of previous experimental and theoretical data and provide the first comprehensive view of the fate of the δ-stabilizer during formation of an oxide.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Focused ion beam milling of polycrystalline diamond

Focused ion beam (FIB) technology has a large potential for precise milling of ultrahard materials such as diamond. However, studies of the sputtering of diamond with ion species and energies relevant to the FIB technology are scarce. Here, we report a systematic study of the sputtering of polycrystalline diamond surfaces with ion beams in a wide range of ion energies (2 - 30 keV), incident beam angles (0 - 80°), and ion masses (N, O, Ar, and Xe). Results show that the sputter yield is relatively insensitive to ion energy but strongly depends on the ion species and incident beam angles. Bombardment with O ions results in sputter yields that are significantly larger than ballistic predictions due to chemical etching effects. Characteristic surface ripples develop for oblique beam incidence angle irradiation. The critical beam tilt angle for the onset of ripple formation and the wavelength of the ripples depend on ion species and energies. Ripples appear to suppress ion reflection at high beam tilt angles and, hence, a peak in the sputter yield angular dependence. In conclusion, these results have direct implications for the development of process parameter maps for high-precision ion-beam milling of diamond.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Investigating the Chemical Reactivity of Lithium Silicate Model SEI Layers

Silicon anodes suffer from an unstable solid electrolyte interphase (SEI) layer that contributes to undesirable capacity fade with cycling. A key part to addressing this unstable SEI formation is to examine how certain components of the SEI react with the electrolyte over time. One SEI component that has not been thoroughly studied in the context of the chemical reactivity against the electrolyte is lithiated silicate. Four model silicate thin films with increasing lithium content were deposited by radio frequency (RF) magnetron sputtering to study how the lithiation of the native oxide on a silicon anode affects the chemical stability of the anode surface. SiO2, Li2Si2O5, Li2SiO3, and Li3SiOx films were exposed to 1.2 M LiPF6 in the 3:7 wt% ethylene carbonate/ethyl methyl carbonate (EC/EMC) electrolyte for periods of time that are representative of the amount of time it takes to undergo cell formations. Soaked samples were rinsed, dried, and characterized by a combination of attenuated total reflectance-infrared spectroscopy (ATR-IR), focused ion beam-secondary electron microscopy (FIB-SEM), and X-ray photoelectron spectroscopy (XPS) depth profiling. It was found that the rate of the decrease in film thickness of the silicates exposed to the electrolyte over time increases as a function of the lithium content in the thin film. This reaction involves HF etching and LiPF6 salt degradation leading to silicate loss and fluorination throughout the bulk. Understanding this chemical instability is critical to determining the overall mechanism of SEI degradation over time.

ADVANCED PROPULSION SYSTEMS,ENERGY STORAGE↗
DOE OSTI2022

Ionic Liquid Gating of SrTiO 3 Lamellas Fabricated with a Focused Ion Beam

Here, in this work, we combine two previously incompatible techniques for defining electronic devices: shaping three-dimensional crystals by focused ion beam (FIB), and two-dimensional electrostatic accumulation of charge carriers. The principal challenge for this integration is nanometer-scale surface damage inherent to any FIB-based fabrication. We address this by using a sacrificial protective layer to preserve a selected pristine surface. The test case presented here is accumulation of 2D carriers by ionic liquid gating at the surface of a micron-scale SrTiO 3 lamella. Preservation of surface quality is reflected in superconductivity of the accumulated carriers. This technique opens new avenues for realizing electrostatic charge tuning in materials that are not available as large or exfoliatable single crystals, and for patterning the geometry of the accumulated carriers.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Crack-Free Silicon Monoxide as Anodes for Lithium-Ion Batteries

The volume expansion of Si and SiO particles was investigated using a single-particle battery assembled with a focused ion beam and scanning electron microscopy (FIB-SEM) system. Single Si and SiO particles were galvanostatically charged and discharged as in real batteries. Microstructural changes of the particles were monitored in situ using FIB-SEM from two different angles. The results revealed that the volume expansion of micrometer size particle SiO was not only much smaller than that of Si, but it also kept its original shape with no sign of cracks. Additionally, this isotropic mechanical property of a SiO particle can be attributed to its microstructure: nanosized Si domains mixed with SiO 2 domains. The nanosized Si domains can mitigate the anisotropic swelling caused by the orientation-dependent lithium-ion insertion; the surrounding SiO 2 domains can act as a buffer to further constrain the localized anisotropic swelling.

25 ENERGY STORAGE↗
DOE OSTI2024

Structural Changes in YBa 2 Cu 3 O 7 Thin Films Modified with He + -Focused Ion Beam for High-Temperature Superconductive Nanoelectronics

Irradiation of high-temperature superconductor YBa 2 Cu 3 O 7 (YBCO) with high-energy He + ions is known to cause structural changes in the YBCO film, decreasing the critical temperature T C and finally leading to a superconductor-to-insulator transition. Here, this allows one to pattern narrow insulating regions with a focused ion beam (FIB) and thus fabricate nanoscale Josephson junctions on YBCO films. Moreover, such ion irradiation is known to cause structural changes in the YBCO film. However, details of how these structural changes occur in nanoscale devices produced by FIB remain unknown. Using nanofocus X-ray diffraction, we study the changes in the YBCO crystal lattice and investigate how the nature of these changes depends on the size of the irradiated regions. These data provide an important understanding of how oxide superconductors can be tailored at the nanometer scale for various applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Optical interference for the guidance of cryogenic focused ion beam milling beyond the axial diffraction limit

Cryogenic focused ion beam (Cryo-FIB) milling has become a standard step in the cryogenic electron tomography (Cryo-ET) workflow and is required to thin cells to electron-semitransparency. However, this destructive process removes the vast majority of the cellular material and raises a critical question: what thin section should be preserved for Cryo-ET analysis? Using a tri-coincident cryogenic FIB-SEM-LM system, we identify an interferometric optical response that can be used for targeting lamella production to fluorescently labeled structures with accuracy beyond the diffraction limit. Here we demonstrate this approach using synthetic samples of fluorescent beads embedded in micron-scale droplets of amorphous ice. We then apply the approach to capture virions inside host cells. Successful targeting is confirmed by Cryo-ET revealing clusters of virions in intracellular vesicles. The method does not require any fluorescent fiducials or axial registration and can be performed on any fluorescently labeled structure that is visible in widefield fluorescence microscopy.

Cryoelectron microscopy↗
DOE OSTI2021

Laser-induced fluorescence of filament-produced plasmas

Self-guided ultrafast laser filaments are a promising method for laser beam delivery and plasma generation for standoff and remote detection of elements and isotopes via filament-induced breakdown spectroscopy (FIBS). Yet, there are several challenges associated with the practical application of FIBS, including delivery of sufficient laser energy at the target for generating plasma with a copious amount of emission signals for obtaining a high signal-to-noise ratio. Here, in this study, we use laser-induced fluorescence (LIF) to boost the emission signal and reduce self-reversal in the spectral profiles. Ultrafast laser filaments were used to produce plasmas from an Al 6061 alloy target at various standoff distances from 1 to 10 m. For LIF emission enhancement, a narrow linewidth continuous-wave laser was used in resonance with a 394.40 nm Al I resonant transition, and the emission signal was monitored from the directly coupled transition at 396.15 nm. Emission signal features of Al I are significantly enhanced by resonant excitation. In addition, LIF of filament ablation plumes reduces the self-reversal features seen in the thermally excited spectral profiles. Time-resolved two-dimensional fluorescence spectroscopy was performed for evaluating the optical saturation effects, which are found to be non-negligible due to high Al atomic densities in the filament-produced plasmas.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

A reliable workflow for improving nanoscale X-ray fluorescence tomographic analysis on nanoparticle-treated HeLa cells

Abstract Scanning X-ray fluorescence (XRF) tomography provides powerful characterization capabilities in evaluating elemental distribution and differentiating their inter- and intra-cellular interactions in a three-dimensional (3D) space. Scanning XRF tomography encounters practical challenges from the sample itself, where the range of rotation angles is limited by geometric constraints, involving sample substrates or nearby features either blocking or converging into the field of view. This study aims to develop a reliable and efficient workflow that can (1) expand the experimental window for nanoscale tomographic analysis of local areas of interest within a laterally extended specimen, and (2) bridge 3D analysis at micrometer and nanoscales on the same specimen. We demonstrate the workflow using a specimen of HeLa cells exposed to iron oxide core and titanium dioxide shell (Fe3O4/TiO2) nanocomposites. The workflow utilizes iterative and multiscale XRF data collection with intermediate sample processing by focused ion beam (FIB) sample preparation between measurements at different length scales. Initial assessment combined with precise sample manipulation via FIB allows direct removal of sample regions that are obstacles to both incident X-ray beam and outgoing XRF signals, which considerably improves the subsequent nanoscale tomography analysis. This multiscale analysis workflow has advanced bio-nanotechnology studies by providing deep insights into the interaction between nanocomposites and single cells at a subcellular level as well as statistical assessments from measuring a population of cells.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2022

Submicrometer spectromicroscopy of UO 2 aged under high humidity conditions

We report the oxidation of uranium dioxide is a complicated process, depending on factors including humidity, temperature, and microstructure. To further determine the characteristics of this process, UO 2 particles were allowed to age and agglomerate under 98% relative humidity at room temperature for 378 days. A focused ion beam (FIB) section of this agglomeration was then measured at the O K-edge, U N 5 -edge, and C K-edge using the scanning transmission x-ray microscope (STXM) at the Advanced Light Source. O K-edge and U N 5 -edge x-ray absorption measurements allowed for the elemental and chemical species mapping of the agglomerates and indicated the formation of schoepite at the submicrometer scale in specific locations. Non-negative matrix factorization was employed to elucidate the main components at the O K-edge, which were uranyl (schoepite) formed primarily at the interface of the sample with controlled atmosphere, a UO 2 -like bulk component present in the majority of the sample, and an oxygen species present at the surface of the FIB section, which is likely adsorbed water. STXM spectromicroscopy measurements at the U N 5 -edge measurements also confirmed the location of oxidized uranium. This analysis is a valuable insight into the formation of schoepite on UO 2 and shows the sensitivity to and utility of STXM spectromicroscopy for uranium speciation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Multidimensional Diagnostics of the Interface Evolutions in Solid-State Lithium Batteries

All-solid-state lithium metal batteries hold tremendous potential as next-generation energy storage solutions. However, their performance is hindered by complex chemo-mechanical instabilities at the interface, which encompass electrolyte decomposition, loss of contact due to volume changes, and the growth of lithium filaments. Given the complexity of these failure mechanisms, it is imperative to employ multidimensional diagnostics that leverage a combination of tools capable of quantifying formed voids and filaments, identifying the chemical and mechanical properties of lithium dendrites and electrolyte decomposition products, as well as monitoring the evolution of these processes in situ. The primary objective of this project is to develop a comprehensive characterization platform for solid-state battery interfaces, integrating FIB-SEM tomography, ToF-SIMS, in-SEM nanoindentation, and in-SIMS AFM-based stiffness mapping to enable structural, chemical, and mechanical analyses. The project team has accomplished significant milestones, including: 1) The successful development of a characterization platform that combines FIB-SEM, ToF-SIMS, nanoindentation, and AFM. 2) The creation of solid-state cells at various scales. 3) Real-time visualization of the plating and stripping of lithium. 4) Operando analysis of the chemical composition and evolution of electrolyte decomposition products, encompassing intermediate and metastable species, at both the cathode and anode interfaces. 5) In situ analysis of mechanical properties coupled with chemical mapping. 6) The implementation of the multiscale characterization technique has yielded valuable insights into cell failure mechanisms and has led to the development of a solid-state lithium cell that exhibits exceptional durability, surpassing 2500 cycles. This project has resulted in 10 publications, 1 invention disclosure, 8 manuscripts under review or in preparation.

25 ENERGY STORAGE↗
DOE OSTI2022

In-situ Characterizations of Microstructural Degradation of Perovskite Solar Cells

Rapid progress has been achieved in perovskite solar cells (PSCs), and their efficiencies have improved from 3.8 % to 24.2 % in less than a decade. With low-cost processing, PSCs have shown exciting photovoltaic (PV) properties, such as effective optical absorption, a long carrier lifetime, and unique defect tolerance. While recent studies demonstrated improved stability up to 100 days, PSC technology is still challenged to meet the stringent industry requirements for commercialization. Despite considerable efforts, the underlying physical mechanisms for the inferior stability of PSCs are not well understood. One reason for this divergence is that many established measurement techniques (e.g., quantum efficiency, photoluminescence) probe the properties on length scales far greater than that of electronic and/or structural inhomogeneity (i.e., < 1 μm near grain boundaries) and therefore characterize convoluted and/or averaged properties. Ion/electron beam-based techniques have been extensively used to access the microstructures of PSCs, enabling atomic/nanoscale structural, chemical, optical, and electrical characterizations. For example, focused ion beam (FIB) milling produces an atomically smooth surface that minimizes the artifacts attributed to the surface roughness. FIB techniques can also create a well-defined cross-section of PSCs without mechanical damage in a physical cleaving sample preparation. While powerful, there are some concerns about possible beam damage of inorganic-organic perovskites via chemical-bond breakage and local heating. This project aims to comprehensively understand how the microstructural/interfacial properties of PSCs (e.g., Methylammonium Lead Iodide [MAPbI 3 ]) are modified under the irradiating ion beams. Specifically, we investigate the sub-surface properties of PSCs before and after Ar-ion beam injections. Kelvin probe force microscopy (KPFM) measures the contact potential differences (CPDs). Photoluminescence (PL) microscopy in conjunction with Finite-Difference Time-Domain (FDTD) simulations infers the formation of a “dead layer” (< 15 nm) on the subsurface of MAPbI 3 during Ar+ milling processes while preserving the initial bulk properties. The x-ray photoemission spectroscopy (XPS) confirms this modified surface is a lead-rich and iodine-deficient surface. We initiate customizing in-situ measurement setup while measuring the local optical and electrical properties of PSC under thermal (cooling, heating) and light stressors. Our results provide in-depth knowledge of the ion-beam impact on metal-halide perovskites and how this modified sub-surface impacts their properties under accelerated stressors of light and heat. Intensive Monte Carlo simulations of an electron beam interacting with PSCs provide the beam energy distribution in PSCs, proposing possible measurement conditions of using e-beam with minimizing beam damage. Our in-situ measurement platform can accommodate the diverse architecture of PSC devices for studying deterioration mechanisms under mixed environmental stressors.

14 SOLAR ENERGY↗
DOE OSTI2023

Controlled semiconductor quantum dot fabrication utilizing focus ion beam

In this project, we experimented the focused ion beam (FIB) based fabrications of semiconductor quantum dots (QDs) by using metal nano particles (NPs) (e.g., Al) on semiconductor as a template and by means of the FIB induced direct metal-to-QD conversion. We have examined effect of the experimental conditions, including Ga + ion energy and dose as well as substrate temperature. The results of experiments have shown AlGaSb QD formation on GaSb substrate can be achieved under certain conditions but there are many challenges about the techniques, including compositional nonuniformity of the QDs formed, partial conversion of the metal NP to QD, and high defect concentration in the QDs.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
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

Cytochrome Nanowire XRD

Microbial metabolism plays an important role in the global cycling of carbon, nutrients, and metals. Recent discovery of microorganisms sharing energy using direct electrical connections might represent a prominent strategy by which anaerobic microorganisms interact with the diversity of environments. The purpose of the proposed research is to apply these newly developed principles of electron exchange in microbial communities to the study of biogeochemical cycling in climate and subsurface systems. Previous studies revealed that soil bacteria Geobacter sulfurreducens produce conductive pili nanofilaments that facilitate long-range electron transport to extracellular electron acceptors and other cells. This discovery has already transformed our understanding of the function of microbial communities in diverse environments, making basic contributions to microbial ecology and helping to improve practical applications such as increasing current output of microbial fuel cells and enhancing the conversion of organic waste to methane. Microbial electron exchange via pili may also contribute to methane production in terrestrial environments that are major sources of atmospheric methane. However, the mechanism of electron transport through pili is not well understood. Initial studies have suggested that pili exhibit metallic-like conductivity similar to conducting polymer polyaniline. However, these studies were limited to electrical measurements. X-ray diffraction studies have suggested that aromatic amino acids tyrosine and phenylalanine are closely packed in pili. But these studies used homology modeling to predict the pilus assembly and information about the number of monomers in each pilus assembly unit and their organization are still lacking. The central hypothesis of this proposal is aromatics in pili enable intermolecular electron delocalization due to pi-stacking that can give rise to metallic-like conductivity. By analyzing pili structure using infrared scattering-scanning near field optical microscope (IR s-SNOM) and combining with solution NMR, Focused Ion Beam (FIB and computational capabilities, this work will provide comprehensive understanding of the conduction mechanism from a structure-function perspective. The specific aims are: 1) With infrared scattering scanning near field optical microscope (IR s-SNOM), image the organization and density of pilin monomers and pH-induced conformational changes in a pilus filament. 2) With solution NMR, resolve pH-induced structural changes in the pilin monomer. 3) Using Focused Ion Beam (FIB), draw electrodes on single pili to measure their conductivity. 4) With computational modeling using the NWChem, simulate the effect of environment on the electronic properties of pili as a function of pH. The proposed work will gain the nanoscale insight into the structure of the pili, as the basis for understanding interspecies electrical communications. The improved understanding will be harnessed to accelerate bioenergy production and bioremediation using pili as well as for predictive modeling of carbon cycling in diverse environments to reach the central goals of DOE-BER to develop sustainable energy sources, regulate the contaminants in the subsurface and understand the effects of greenhouse gas emissions on biosphere. The proposed studies will provide design principles for engineering of electrical interactions among these communities by manipulating the amino acid composition of pili. Moreover, these studies will identify the forces that maintain the function of these communities in the face of environmental perturbation. Therefore, these studies will help to address the need "to incorporate process understanding of biogeochemical cycling into a scalable hierarchy of predictive capabilities" specified in EMSL's Science Themes.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Bridging multimodal microscopy for advanced characterization on nuclear fuel using machine learning

Uranium dioxide (UO 2 ), widely used as driver fuel in light water reactors, experiences microstructure and property change by nuclear fission reactions. This paper bridges the characterization of fresh UO 2 fuel at different length scales, serving as a baseline for future post irradiation examination of irradiated UO 2 fuel. To characterize the microstructural change of nuclear fuel, modern approaches cover a wide range of length scales through different characterization techniques, such as mm scale for Synchrotron-based X-ray computed tomography (SXCT) and microscale for focused ion beam (FIB) and scanning electron microscopy (SEM). It is challenging to bridge the data and knowledge of the same sample in different length scales. This paper proposed a deep learning framework leveraging transfer learning to detect microstructural defects, trained from a sparse FIB, SEM, and SXCT images. The proposed model achieved superior performance in defect segmentation on multiscale microscopic data compared to four of the latest deep learning models.

36 MATERIALS SCIENCE↗