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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 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Deformation of Néel-type skyrmions revealed by Lorentz transmission electron microscopy

Néel-type magnetic skyrmions in multilayers are promising candidates for ultra-low power spintronic devices. To image the Néel-type skyrmions using Lorentz transmission electron microscopy (L-TEM), the samples must be tilted. Thus, the external magnetic field consists of both in-plane and out-of-plane components. To date, it is still not well known on the effect of the in-plane magnetic field on the L-TEM images, leading to ambiguities in retrieving the structure of Néel-type skyrmions. Here, Néel-type skyrmions in three [Pt/Co/Ta]$_{20}$ multilayer samples, with the easy magnetization axis being tuned from the out-of-plane to the in-plane direction by increasing the Co thickness from 1.8 to 2.2 nm, are imaged. When using a smaller defocus value (-2 mm) and a higher magnification (×9100) of L-TEM, a surprising dark-bright-dark-bright double contrasted pattern, instead of the previously reported dark-bright contrasted pattern, is observed. The additional dark-bright contrasted pattern becomes more evident for thicker Co layer samples in which the magnetization axis tilts more toward the in-plane direction. Further analysis, via a combination of magnetic force microscopy experiments, micromagnetic simulations, and micromagnetic analysis to Lorentz TEM simulation, shows that the additional dark-bright features originate from the deformation of the Néel-type skyrmions within an in-plane magnetic field.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Direct processing of PbZr 0.53 Ti 0.47 O 3 films on glass and polymeric substrates

This work reports on direct crystallization of PbZr 0.53 Ti 0.47 O 3 (PZT) thin films on glass and polymeric substrates, using pulsed thermal processing (PTP). Specifically, xenon flash lamps deliver pulses of high intensity, short duration, broadband light to the surface of a chemical solution deposited thin film, resulting in the crystallization of the film. Structural analysis by X-ray diffraction (XRD) and transmission electron microscopy show the existence of perovskite structure in nano-sized grains (≤5 nm). Local functional analysis by band excitation piezoelectric spectroscopy and electrostatic force microscopy confirm the presence of a ferroelectric phase and retention of voltage-written polarization for multiple days. Based on structural and functional analyses, strategies are discussed for optimization of pulse voltage and duration for the realization of crystalline ferroelectric thin films. For ~200 nm-thick PZT films on glass substrates, 500 μs-long pulses were required for crystallization, starting with 100 pulses at 350 V, 10 or 25 pulses at 400 V and in general lower number of pulses at higher voltages (resulting in higher radiant energy). Overall power densities of >6.4 kW/cm 2 were needed for appearance of peaks corresponding to the perovskite phase in the XRD. Films on glass processed at 350–400 V had a higher degree of 111-oriented perovskite grains. Higher applied radiant energy (through increased pulse voltage or count) resulted in more random and/or partially 001-oriented films. For ~1 μm-thick PZT films on polymeric substrates, 10 to 25 250 μs-long pulses at voltages ranging between 200 to 250 V, corresponding to power densities of ~2.8 kW/cm 2 , were optimal for maximized perovskite phase crystallization, while avoiding substrate damage.

36 MATERIALS SCIENCE↗
NASA NTRS1985

Survey of probable micrometer-sized Earth-orbital debris fragments in the NASA-JSC cosmic dust sample collection

A program to collect extraterrestrial dust samples from the stratosphere using impactors mounted on NASA U-2 and WB-57F aircraft is discussed. Sample collection, preparation, and analysis techniques are described and the particle types found are reviewed. Preliminary examination of the particles indicates that they represent not only extraterrestrial material, but some fraction of terrestrial contamination from both natural and manmade sources. This examination involves a combination of optical microscopy, scanning electron microscopy (SEM) and qualitative bulk elemental analysis using an energy-dispersive X-ray spectrometer (EDS) to characterize each particle. The cosmic dust collection contains samples of at least three classes of material that may present some hazard to extended spacecraft operations in near-Earth orbit: (1) micrometeorites/cosmic dust, (2) aluminum oxide spheres, and (3) alloy spherules and fragments.

Clanton, U. S.↗
DOE OSTI2021

Investigating phase transitions from local crystallographic analysis based on statistical learning of atomic environments in 2D MoS 2 -ReS 2

Traditionally, phase transitions are explored using a combination of macroscopic functional characterization and scattering techniques, providing insight into the average properties and symmetries of the lattice but local atomic level mechanisms during phase transitions generally remain unknown. Here, we explore the mechanisms of a phase transition between the trigonal prismatic and distorted octahedral phases of layered chalcogenides in the 2D MoS 2 - ReS 2 system from the observations of local degrees of freedom, namely atomic positions by Scanning Transmission Electron Microscopy (STEM). We employ local crystallographic analysis based on statistical learning of atomic environments to build a picture of the transition from the atomic level up and determine local and global variables controlling the local symmetry breaking. In particular, we argue that the dependence of the average symmetry breaking distortion amplitude on global and local concentration can be used to separate local chemical as well as global electronic effects on transition. This approach allows exploring atomic mechanisms beyond the traditional macroscopic descriptions, utilizing the imaging of compositional fluctuations in solids to explore phase transitions over a range of realized and observed local stoichiometries and atomic configurations.

25 ENERGY STORAGE↗
DOE OSTI2023

Targeted Dy intercalation under graphene/SiC for tuning its electronic band structure

Metal intercalation of graphene is a promising method to tune its electronic band structure and generate novel electronic and topological phases. The tuning depends critically on the ability to bond the intercalated atoms at predesigned, subsurface interlayer locations because the emerging band structure depends on metal location. In this work, we have studied Dy intercalation under single-layer graphene (SLG) on SiC using spot profile analysis–low-energy electron diffraction and scanning tunneling microscopy (STM). The experimental work is complemented with density-functional theory (DFT) analysis. Because different diffraction spots originate from different subsurface interlayer regions, it is possible to identify changes in the intercalation location by monitoring the spot intensity as a function of growth conditions. DFT calculations of the chemical potential as a function of intercalated Dy coverage support the variation of the stability of the intercalated phase at different intercalated locations. The preferred location is confirmed from STM studies showing the removal of the 6 × 6 moiré corrugation at the preferred location, observed at higher Dy coverage.

2-dimensional systems↗
NASA NTRS1997

Stressed Oxidation of C/SiC Composites

Constant load, stressed oxidation testing was performed on T-300 C/SiC composites with a SiC seal coat. Test conditions included temperatures ranging from 350 C to 1500 C at stresses of 69 MPa and 172 MPa (10 and 25 ksi). The coupon subjected to stressed oxidation at 550 C/69 MPa for 25 hours had a room temperature residual strength one-half that of the as-received coupons. The coupon tested at the higher stress and all coupons tested at higher temperatures failed in less than 25 hr. Microstructural analysis of the fracture surfaces, using SEM (scanning electron microscopy), revealed the formation of reduced cross-sectional fibers with pointed tips. Analysis of composite cross-sections show pathways for oxygen ingress. The discussion will focus on fiber/matrix interphase oxidation and debonding as well as the formation and implications of the fiber tip morphology.

Halbig, Michael C.↗
DOE OSTI2025

Deep learning of structural morphology imaged by scanning X-ray diffraction microscopy

Scanning X-ray nanodiffraction microscopy is a powerful technique for spatially resolving nanoscale structural morphologies by diffraction contrast. One of the critical challenges in experimental nanodiffraction data analysis is posed by the convergence angle of nanoscale focusing optics which creates simultaneous dependency of the far-field scattering data on three independent components of the local strain tensor-corresponding to dilation and two potential rigid body rotations of the unit cell. All three components are in principle resolvable through a spatially mapped sample tilt series; however, traditional data analysis is computationally expensive and prone to artifacts. In this study, we implement NanobeamNN, a convolutional neural network specifically tailored to the analysis of scanning probe X-ray microscopy data. NanobeamNN learns lattice strain and rotation angles from simulated diffraction of a focused X-ray nanobeam by an epitaxial thin film and can directly make reasonable predictions on experimental data without the need for additional fine-tuning. We demonstrate that this approach represents a significant advancement in computational speed over conventional methods, as well as a potential improvement in accuracy over the current standard.

Luo, Aileen [Cornell Univ., Ithaca, NY (United Sta↗
NASA NTRS1992

Compositional analysis of projectile residues on LDEF instrument AO187-1

Impact craters greater than 30 microns and associated projectile residues were analyzed by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDXA). Objectives were to analyze a statistically significant number of projectiles to evaluate their chemical variability and possible clustering into discrete particle types. Bay A11 exposed six collector surfaces of anodized 1100-T4 (greater than 99 percent pure) aluminum sheets, 0.32 cm thick, yielding an exposed surface area of 1.1 sq. m. Four of the six panels have been retained at JSC, and were optically scanned, one (A11E00E) was prepared for SEM/EDX analysis. Bay A03 was occupied by high purity (99.99 percent) gold sheets, 0.5 mm thick, yielding an exposed surface area of 0.85 sq. m. Sample processing included the optical scanning (6X), labeling, and dislodging (by a punch-die device) of each individual impact greater than 75 microns for the aluminum and 30 microns for the gold. The 209 craters were dislodged form A11E00E, having crater diameters up to 3500 microns. Optical examination of the gold surfaces detected 238 craters, 198 of which were retained at JSC and analyzed via SEM/EDX. The analytical procedures included maximizing the geometric efficiency (take-off angles), using relatively long count times (500-1000 sec) and sufficiently high accelerating currents (25-30Kev). Despite diligent examination, a large number of craters did not exhibit measurable signals above background. Detectable resides were classified as either micrometeoritic or as man-made debris.

Bernhard, Ronald P.↗
DOE OSTI2022

From ammonium Hexahalorhenates(IV) to nanocrystalline rhenium metal: A combined thermal, diffraction and microscopic analysis

Rhenium metal powder is a material of industrial importance. Several industrial and laboratory methods have been developed for the preparation of ultrafine Re metal powder and nanoparticles. The present study provides a better understanding of the characteristic and formation of Re metal powder from the decomposition of (NH4)2ReX6 salt (X = F, Cl, Br, I) at high temperature in inert atmosphere. Such analysis resulted in the formation of nanocrystalline Re metal as characterized by powder XRD. Williamson-Hall, Scherrer, and Williamson-Smallman methods were employed to study the effect of crystallize size, lattice strain, and dislocation density as analyzed from powder XRD peak broadening. Here, the morphology and composition of the metal were analyzed using scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Size-Resolved Shape Evolution in Inorganic Nanocrystals Captured via High-Throughput Deep Learning-Driven Statistical Characterization

Precise size and shape control in nanocrystal synthesis is essential for utilizing nanocrystals in various industrial applications, such as catalysis, sensing, and energy conversion. However, traditional ensemble measurements often overlook the subtle size and shape distributions of individual nanocrystals, hindering the establishment of robust structure–property relationships. In this study, we uncover intricate shape evolutions and growth mechanisms in Co 3 O 4 nanocrystal synthesis at a subnanometer scale, enabled by deep-learning-assisted statistical characterization. By first controlling synthetic parameters such as cobalt precursor concentration and water amount then using high resolution electron microscopy imaging to identify the geometric features of individual nanocrystals, this study provides insights into the interplay between synthesis conditions and the sizedependent shape evolution in colloidal nanocrystals. Utilizing population-wide imaging data encompassing over 441,067 nanocrystals, we analyze their characteristics and elucidate previously unobserved size-resolved shape evolution. This high-throughput statistical analysis is essential for representing the entire population accurately and enables the study of the size dependency of growth regimes in shaping nanocrystals. Our findings provide experimental quantification of the growth regime transition based on the size of the crystals, specifically (i) for faceting and (ii) from thermodynamic to kinetic, as evidenced by transitions from convex to concave polyhedral crystals. Additionally, we introduce the concept of an “onset radius,” which describes the critical size thresholds at which these transitions occur. This discovery has implications beyond achieving nanocrystals with desired morphology; it enables finely tuned correlation between geometry and material properties, advancing the field of colloidal nanocrystal synthesis and its applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

A hybrid topological quantum state in an elemental solid

Topology and interactions are foundational concepts in the modern understanding of quantum matter. Their nexus yields three important research directions: (1) the competition between distinct interactions, as in several intertwined phases, (2) the interplay between interactions and topology that drives the phenomena in twisted layered materials and topological magnets, and (3) the coalescence of several topological orders to generate distinct novel phases. The first two examples have grown into major areas of research, although the last example remains mostly unexplored, mainly because of the lack of a material platform for experimental studies. Here, using tunnelling microscopy, photoemission spectroscopy and a theoretical analysis, we unveil a ‘hybrid’ topological phase of matter in the simple elemental-solid arsenic. Through a unique bulk-surface-edge correspondence, we uncover that arsenic features a conjoined strong and higher-order topology that stabilizes a hybrid topological phase. Although momentum-space spectroscopy measurements show signs of topological surface states, real-space microscopy measurements unravel a unique geometry of topologically induced step-edge conduction channels revealed on various natural nanostructures on the surface. Using theoretical models, we show that the existence of gapless step-edge states in arsenic relies on the simultaneous presence of both a non-trivial strong Z 2 invariant and a non-trivial higher-order topological invariant, which provide experimental evidence for hybrid topology. Finally, our study highlights pathways for exploring the interplay of different band topologies and harnessing the associated topological conduction channels in engineered quantum or nano-devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2005

Crystallization Kinetics of a Solid Oxide Fuel Cell Seal Glass by Differential Thermal Analysis

Crystallization kinetics of a barium calcium aluminosilicate glass (BCAS), a sealant material for planar solid oxide fuel cells, have been investigated by differential thermal analysis (DTA). From variation of DTA peak maximum temperature with heating rate, the activation energy for glass crystallization was calculated to be 259 kJ/mol. Development of crystalline phases on thermal treatments of the glass at various temperatures has been followed by powder x-ray diffraction. Microstructure and chemical composition of the crystalline phases were investigated by scanning electron microscopy and energy dispersive spectroscopic (EDS) analysis. BaSiO3 and hexacelsian (BaAl2Si2O8) were the primary crystalline phases whereas monoclinic celsian (BaAl2Si2O8) and (Ba(x), Ca(y))SiO4 were also detected as minor phases. Needle-shaped BaSiO3 crystals are formed first, followed by the formation of other phases at longer times of heat treatments. The glass does not fully crystallize even after long term heat treatments at 750 to 900 C.

Bansal, Narottam P.↗
DOE OSTI2023

Post irradiation examination of a uranium-zirconium hydride TRIGA fuel element

Low-enriched (LEU) U-ZrH fuel, with a 235 U content less than 20% of the total uranium, is being evaluated for possible use in different types of reactors, including space nuclear systems, light water reactors (LWRs) and micro-reactors. As a result, it is beneficial to better understand the macrostructural and microstructural changes that occur in this fuel during irradiation. This paper reports the results of the post irradiation examination of an LEU U-ZrH fuel element (30 wt.% U, <20% 235 U) using neutron radiography, precision gamma scanning, chemical analysis, optical metallography and scanning electron microscopy combined with energy dispersive spectroscopy and wavelength dispersive spectroscopy, where the fuel element was irradiated in a Training, Research, Isotope, General Atomics (TRIGA) reactor. Results of microstructural characterization indicated some dehydriding and cracking of the U-ZrH fuel occurred during irradiation; an axial and radial burnup gradient existed in the fuel during irradiation, as measured by gamma scanning and chemical analysis; negligible microstructural changes transpired during irradiation, based on comparison of irradiated and as-fabricated U-ZrH fuel microstructures; and, negligible, fission product-rich, phases could be resolved in a U-ZrH fuel that was irradiated to a calculated 20% depletion of 235 U.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2012

Face-Sheet Quality Analysis and Thermo-Physical Property Characterization of OOA and Autoclave Panels

Increased application of polymer matrix composite (PMC) materials in large vehicle structures requires consideration of non-autoclave manufacturing technology. The NASA Composites for Exploration project, and its predecessor, Lightweight Spacecraft Structures and Materials project, were tasked with the development of materials and manufacturing processes for structures that will perform in a heavy-lift-launch vehicle environment. Both autoclave and out of autoclave processable materials were considered. Large PMC structures envisioned for such a vehicle included the payload shroud and the interstage connector. In this study, composite sandwich panels representing 1/16th segments of the barrel section of the Ares V rocket fairing were prepared as 1.8 m x 2.4 m sections of the 10 m diameter arc segment. IM7/977-3 was used as the face-sheet prepreg of the autoclave processed panels and T40-800B/5320-1 for the out of autoclave panels. The core was 49.7 kilograms per square meters (3.1 pounds per cubic feet (pcf)) aluminum honeycomb. Face-sheets were fabricated by automated tape laying 153 mm wide unidirectional tape. This work details analysis of the manufactured panels where face-sheet quality was characterized by optical microscopy, cured ply thickness measurements, acid digestion, and thermal analysis.

Miller, Sandi G.↗
NASA NTRS2012

Face-Sheet Quality Analysis and Thermo-Physical Property Characterization of OOA and Autoclave Panels

Increased application of polymer matrix composite (PMC) materials in large vehicle structures requires consideration of non-autoclave manufacturing technology. The NASA Composites for Exploration project, and its predecessor, Lightweight Spacecraft Structures and Materials project, were tasked with the development of materials and manufacturing processes for structures that will perform in a heavy-lift-launch vehicle environment. Both autoclave and out of autoclave processable materials were considered. Large PMC structures envisioned for such a vehicle included the payload shroud and the interstage connector. In this study, composite sandwich panels representing 1/16th segments of the barrel section of the Ares V rocket fairing were prepared as 1.8 m x 2.4 m sections of the 10 m diameter arc segment. IM7/977-3 was used as the face-sheet prepreg of the autoclave processed panels and T40-800B/5320-1 for the out of autoclave panels. The core was 49.7 kg/sq m (3.1 lb/cu ft (pcf)) aluminum honeycomb. Face-sheets were fabricated by automated tape laying 153 mm wide unidirectional tape. This work details analysis of the manufactured panels where face-sheet quality was characterized by optical microscopy, cured ply thickness measurements, acid digestion, and thermal analysis.

Miller, Sandi G.↗
DOE OSTI2022

High-Energy X-ray Diffraction Microscopy for Nuclear Forensics FY2022 Project Report

Morphological information on nuclear material has been identified using visible light and scanning electron microscopy. These identify qualitative differences in particle morphology. Three-dimensional imaging of materials through alternating scanning electron microscopy imaging and focused ion beam milling has also been used. Unfortunately, these techniques are time- and labor-intensive, with significant sample preparation required and lengthy analysis times. Further, the resulting 3D images are qualitative, require manual identification, and do not capture statistically-representative populations. High energy X-ray 3D imaging using a direct-beam or diffracted-beam (High-Energy Diffraction Microscopy) have been developed at the Advanced Photon Source and can produce quantitative information on grains (phase, location, etc.) and pores (size distribution, sphericity) in a material. These techniques require only minutes to characterize a sample volume and are non-destructive, thus suitable for a wide range of existing samples and for confirmatory analyses to be carried out using conventional microscopy techniques. In this first year of the project, all uranium oxide samples were synthesized and characterized using conventional analyses by the analytical chemistry laboratory. Conventional analysis methods included powder x-ray diffraction, scanning electron microscopy, impurity analysis via inductively coupled plasma mass spectrometry, and infrared spectroscopy. Impurity analysis shows a drop in boron content from UO 3 to the lowest U 3 O 8 calcination temperature, but otherwise no appreciable difference in any sample. Analysis of diffraction data shows a flip of peaks from UO 3 dominated for the 600 °C calcined sample to U 3 O 8 dominated at 700 °C and 800 °C. Analysis of scanning electron microscopy images shows that with increased calcination temperature the size distribution of particles seems to increase and broaden. Both of these last findings are in line with previously published data, though this work used significantly fewer particles to simply show similar trends instead of getting truly quantitative particle analysis. Infrared analysis similarly shows ingrowth of U 3 O 8 as calcination temperature is increased, along with depression of peaks associated with UO 3 and water. Samples were prepared for analysis at the Advanced Photon Source at beamline 1-ID. It is anticipated that analysis will occur in November of 2022. AI/ML techniques to de-noise data coming out of 1-ID during the analyses was also developed during this time using previously gathered data. Preliminary results using a self-supervision technique called Noise2Selfshow good de-noising of data. Once the uranium oxide samples are analyzed, real data will be used to test the de-noising and other AI/ML techniques that may be developed in the second year of the project.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2000

Micromechanical Characterization and Texture Analysis of Direct Cast Titanium Alloys Strips

This research was conducted to determine a post-processing technique to optimize mechanical and material properties of a number of Titanium based alloys and aluminides processed via Melt Overflow Solidification Technique (MORST). This technique was developed by NASA for the development of thin sheet titanium and titanium aluminides used in high temperature applications. The materials investigated in this study included conventional titanium alloy strips and foils, Ti-1100, Ti-24Al-11Nb (Alpha-2), and Ti-48Al-2Ta (Gamma). The methodology used included micro-characterization, heat-treatment, mechanical processing and mechanical testing. Characterization techniques included optical, electron microscopy, and x-ray texture analysis. The processing included heat-treatment and mechanical deformation through cold rolling. The initial as-cast materials were evaluated for their microstructure and mechanical properties. Different heat-treatment and rolling steps were chosen to process these materials. The properties were evaluated further and a processing relationship was established in order to obtain an optimum processing condition. The results showed that the as-cast material exhibited a Widmanstatten (fine grain) microstructure that developed into a microstructure with larger grains through processing steps. The texture intensity showed little change for all processing performed in this investigation.

Source record↗
DOE OSTI2025

3013 Baseline Inner Container Report: Description, Imaging, and Analysis

This report presents consolidated findings from three microscopy studies of baseline Bagless Transfer Containers (BTCs), which are the inner containers used in DOE Standard 3013-compliant plutonium storage packages. The studies were conducted by Los Alamos National Laboratory (LANL), Savannah River National Laboratory (SRNL), and DNV, a subcontractor specializing in corrosion science. The baseline BTCs examined had not been exposed to corrosive environments, serving as control samples for comparison with destructively examined (DE) containers. Additionally, the Background section provides an overview of the BTC design, including manufacturing methods, material properties, and container configurations that may influence corrosion behavior. The primary objective of the LANL and SRNL studies was to establish reference characteristics of BTCs to distinguish manufacturing artifacts from corrosion-induced features observed in DE containers. Both laboratories used advanced microscopy techniques, including Wide Area Microscopy (WAMS), Laser Confocal Microscopy (LCM), Scanning Electron Microscopy (SEM), and Focused Ion Beam (FIB), to reveal that most surface anomalies were shallow and attributable to flow-forming processes, not corrosion. Subsurface impurities, identified as non-metallic inclusions, were also observed. DNV’s investigation focused on characterizing the mechanical and chemical properties of the BTC material to support crack growth modeling. Their findings indicate higher hardness and strength but reduced ductility—consistent with flow-formed 304L stainless steel and a higher-than-expected martensite content, in contrast to manufacturer claims. Ongoing and future studies, including Electron Backscatter Diffraction (EBSD), aim to further understand the microstructural factors influencing crack initiation and propagation. The combined studies provide a crucial baseline for distinguishing corrosion effects in DE containers, contributing to the safe and reliable long-term storage of plutonium-bearing materials.

36 MATERIALS SCIENCE↗