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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Resolution of Virtual Depth Sectioning from Four-Dimensional Scanning Transmission Electron Microscopy

Abstract One approach to three-dimensional structure determination using the wealth of scattering data in four-dimensional (4D) scanning transmission electron microscopy (STEM) is the parallax method proposed by Ophus et al. (2019. Advanced phase reconstruction methods enabled by 4D scanning transmission electron microscopy, Microsc Microanal25, 10–11), which determines the scattering matrix and uses it to synthesize a virtual depth-sectioning reconstruction of the sample structure. Drawing on an equivalence with a hypothetical confocal imaging mode, we derive contrast transfer and point spread functions for this parallax method applied to weakly scattering objects, showing them identical to earlier depth-sectioning STEM modes when only bright field signal is used, but that improved depth resolution is possible if dark field signal can be used. Through a simulation-based study of doped Si, we show that this depth resolution is preserved for thicker samples, explore the impact of shot noise on the parallax reconstructions, discuss challenges to making use of dark field signal, and identify cases where the interpretation of the parallax reconstruction breaks down.

3D imaging↗
NASA NTRS1977

Depositional history of core section 74001 - Depth profiles of maturity, FeO, and metal

Samples from every 0.5-cm interval of soil in core section 74001 have been studied by ferromagnetic resonance (FMR) and magnetic techniques. The values of the FMR maturity index show that the 74001 samples are very immature (the index ranges from 0.14 to 0.29 units) and have not seen appreciable, if any, surface exposure since their deposition. In fact, the small amount of fine-grained metal in the 74001 samples is probably not acquired as a result of their exposure to the micrometeoroid flux at the lunar surface. Thus, the black-glass soil of 74001 was deposited very rapidly, probably in a single episode or several closely spaced episodes of lunar fire fountaining. The average concentration of FeO and its standard deviation for all the 74001 samples are 22.5 + or - 0.3 wt.%. Since the FeO concentration is so uniform, no large variations in the major-element chemistry of 74001 are expected, with the possible exception of the volatile elements. The concentration of coarse-grained metal, which is measured magnetically, and its standard deviation are 0.15 + or - 0.01 wt.%. The coarse-grained metal probably precipitated contemporaneously with the silicate and oxide phases in the black-glass droplets.

Morris, R. V.↗
NASA NTRS1993

Effects of orbital exposure on RTV during the LDEF mission

Thermomechanical analysis (TMA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) were performed on samples of RTV 511 exposed on the Long Duration Exposure Facility (LDEF) mission for 6 years in orbit and unexposed RTV 511 control samples. Slices 20- to 400-microns thick were removed from the exposed surface down to a depth of 1,500 microns through the 3-mm thick samples. The TMA and DSC results, which arise from the entire slice and not just its surface, showed no significant differences between the LDEF exposed and the control samples. TMA scans were run from ambient to 500 C; results were compared by a tabulation of the onset temperatures for flow. DSC scans were run from ambient to 600 C; no endotherms or exotherms occurred over the range observed. What appear to be glass transition temperatures were compared for the samples as a function of section depth within the sample and between the exposed and control samples. The TGA scans from 25 to 900 C, which arise from the surface of the sample initially, showed a slight increase in the top most 105-micron slice (the exposed, discolored side) in the weight loss at 600 C in oxygen. This weight loss dropped to bulk values at the next slice below the top section, a mean depth of 258 microns. The control sample also showed an increase in weight loss as the top surface was approached, but the 600 C weight losses were very inconsistent. The LDEF RTV sample appears to be mechanically undamaged, with a surface layer which oxidizes slightly faster as a result of orbital exposure.

Brower, William E., Jr.↗
DOE OSTI2025

Charge Disproportionation at Twisted SrTiO 3 Bilayer Interface Driven by Local Atomic Registry

The interplay of lattice, orbital, and charge degrees of freedom in complex oxide materials has hosted a plethora of exotic quantum phases and physical properties. Recent advances in the synthesis of freestanding complex oxide membranes and twisted heterostructures assembled from membranes provide diverse opportunities for discovery using moiré design with local lattice control. To this end, we designed moiré crystals at the coincidence site lattice condition, providing commensurate structure within the moiré supercell arising from the multiatom complex oxide unit cell. We fabricated such twisted bilayers from freestanding SrTiO 3 membranes and used depth-sectioning-based electron microscopic methods to investigate ordered charge states at the moiré interface. By selectively imaging SrTiO 3 atomic planes at different depths through the bilayer, we clearly resolved the moiré periodic structure at the twisted interface and found that it exhibits lattice-dependent charge disproportionation in the local atomic registry within the moiré supercell. Density functional modeling of the twisted oxide interface predicts that these moiré phenomena are accompanied by a two-dimensional flat band that can drive exceptional electronic phases. Our work provides a robust strategy for controlling moiré periodicity in twisted oxides and paves pathways to exploit the extraordinary functionalities via moiré lattice-driven charge-orbital correlation.

charge disproportionation↗
DOE OSTI2024

A Comprehensive Stress Drop Map From Trench to Depth in the Northern Chilean Subduction Zone

We compute stress drops for earthquakes in Northern Chile recorded between 2007 and 2021. By applying two analysis techniques, (a) the spectral ratio (SR) method and (b) the spectral decomposition (SDC) method, a stress drop map for the subduction zone consisting of 51,510 stress drop values is produced. We build an extended set of empirical Green’s functions (EGF) for the SR method by systematic template matching. Outputs are used to compare with results from the SDC approach, where we apply cell-wise obtained global EGF's to compensate for the structural heterogeneity of the subduction zone. We find a good consistency of results of the two methods. The increased spatial coverage and quantity of stress drop estimates from the SDC method facilitate a consistent stress drop mapping of the different seismotectonic domains. Albeit only small differences of median stress drop, strike-perpendicular depth sections clearly reveal systematic variations, with earthquakes at different seismotectonic locations exhibiting distinct values. In particular, interface seismicity is characterized by the lowest observed median value, whereas upper plate earthquakes show noticeably higher stress drop values. Intermediate depth earthquakes show comparatively high average stress drop and a rather strong depth-dependent increase of median stress drop. Additionally, we observe spatio-temporal variability of stress drops related to the occurrence of the two megathrust earthquakes in the study region. The presented study is the first coherent large scale 3D stress drop mapping of the Northern Chilean subduction zone. It provides an important component for further detailed analysis of the physics of earthquake ruptures.

58 GEOSCIENCES↗
DOE OSTI2026

Atomic-Scale Imaging of Lithium Vacancies in a Battery Cathode by Multislice Electron Ptychography

Atomic-resolution imaging of battery materials is critical for identification of local defects and structural variations, which are tied to battery performance. However, since battery materials are, by design, optimized to allow ion motion in response to an applied electric field, they are also very sensitive to radiation damage by an electron beam. Image resolution is therefore severely constrained by the dose applied. Here, we show that multislice electron ptychography (MEP) can provide sub-ångström lateral resolution images of both light and heavy elements of a Li-ion battery cathode, along with nanometer-scale depth information and greater dose efficiency than conventional electron microscopy methods. Using the depth-sectioning capability of MEP, we have been able to obtain direct visualizations of Li vacancy clusters, atom column by atom column, in Li x Ni 0.33 Mn 0.33 Co 0.33 O 2 (NMC111) cathodes. This capability to track Li distributions will be valuable in understanding, informing, and optimizing electrode material design for ion storage and transfer.

batteries↗
DOE OSTI2022

A Three-Dimensional Reconstruction Algorithm for Scanning Transmission Electron Microscopy Data from a Single Sample Orientation

Abstract Increasing interest in three-dimensional nanostructures adds impetus to electron microscopy techniques capable of imaging at or below the nanoscale in three dimensions. We present a reconstruction algorithm that takes as input a focal series of four-dimensional scanning transmission electron microscopy (4D-STEM) data. We apply the approach to a lead iridate, PbIrO, and yttrium-stabilized zirconia, YZrO, heterostructure from data acquired with the specimen in a single plan-view orientation, with the epitaxial layers stacked along the beam direction. We demonstrate that Pb–Ir atomic columns are visible in the uppermost layers of the reconstructed volume. We compare this approach to the alternative techniques of depth sectioning using differential phase contrast scanning transmission electron microscopy (DPC-STEM) and multislice ptychographic reconstruction.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Evaluation of Copper Catalytic Effects in Cable Insulation Polymers

This paper summarizes work performed to evaluate a phenomenon that occurs in electrical cable insulation polymers subjected to accelerated aging while in contact with copper metal. This effect, commonly known as the copper catalytic effect, is a result of chemical reactions that occur when copper ions diffuse into insulation polymers. This diffusion process is observed in various types of polymeric materials exposed to elevated temperatures and happens at the interface between the insulation and metallic components (e.g., conductor, shielding, etc.) in a cable. This polymer-metal interaction has only been observed in cables constructed with copper components (i.e., no interactions observed in cables with aluminum or other metal conductor/shielding) and results in a significant catalytic effect that increases the oxidation rate (e.g., aging) of the material. Under this research, the copper catalytic effects observed in cross-linked polyethylene, cross-linked polyolefin and ethylene propylene rubber insulated cables subjected to thermal accelerated aging were evaluated. These evaluations involved applying infrared spectroscopy, microscopy, and energy dispersive X-ray spectroscopy cross-sectional depth profiling to obtain an in-depth understanding of the aging characteristics of the materials under accelerated conditions. Based on the results of these assessments, the copper catalytic effect can have a significant impact on the mechanical, thermal, chemical, and electrical properties of cable insulation polymers. Here, the results acquired from this research provided the information needed to characterize the copper catalytic effects observed in these polymers, analyze how this phenomenon affected the polymer degradation process, and compare and understand the differences in the properties of the materials.

42 ENGINEERING↗
DOE OSTI2023

Evidence of cryptic methane cycling and non-methanogenic methylamine consumption in the sulfate-reducing zone of sediment in the Santa Barbara Basin, California

The recently discovered cryptic methane cycle in the sulfate-reducing zone of marine and wetland sediment couples methylotrophic methanogenesis to anaerobic oxidation of methane (AOM). Here we present evidence of cryptic methane cycling activity within the upper regions of the sulfate-reducing zone, along a depth transect within the Santa Barbara Basin, off the coast of California, USA. The top 0–20 cm of sediment from each station was subjected to geochemical analyses and radiotracer incubations using 35 S–SO$^{2-}_{4}$, 14 C–mono-methylamine, and 14 C–CH 4 to find evidence of cryptic methane cycling. Methane concentrations were consistently low (3 to 16 µM) across the depth transect, despite AOM rates increasing with decreasing water depth (from max 0.05 nmol cm -3 d -1 at the deepest station to max 1.8 nmol cm -3 d -1 at the shallowest station). Porewater sulfate concentrations remained high (23 to 29 mM), despite the detection of sulfate reduction activity from 35 S–SO$^{2-}_{4}$ incubations with rates up to 134 nmol cm -3 d -1 . Metabolomic analysis showed that substrates for methanogenesis (i.e., acetate, methanol and methylamines) were mostly below the detection limit in the porewater, but some samples from the 1–2 cm depth section showed non-quantifiable evidence of these substrates, indicating their rapid turnover. Estimated methanogenesis from mono-methylamine ranged from 0.2 to 0.5 nmol cm -3 d -1 . Discrepancies between the rate constants (k) of methanogenesis (from 14 C–mono-methylamine) and AOM (from either 14 C–mono-methylamine-derived 14 C–CH 4 or from directly injected 14 C–CH 4 ) suggest the activity of a separate, concurrent metabolic process directly metabolizing mono-methylamine to inorganic carbon. We conclude that the results presented in this work show strong evidence of cryptic methane cycling occurring within the top 20 cm of sediment in the Santa Barbara Basin. The rapid cycling of carbon between methanogenesis and methanotropy likely prevents major build-up of methane in the sulfate-reducing zone. Furthermore, our data suggest that methylamine is utilized by both methanogenic archaea capable of methylotrophic methanogenesis and non-methanogenic microbial groups. We hypothesize that sulfate reduction is responsible for the additional methylamine turnover, but further investigation is needed to elucidate this metabolic activity.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Spatially Averaged Ice Contents of Ice-Wedge Polygon Cross-Sections to 3-m Depth, July 2013, Utqiagvik, Alaska

This dataset contains spatially averaged estimates of ice content (volume percent) for two-dimensional cross-sectional profiles (from trough center to trough center to a depth of 3 meters) of low- and flat-centered ice-wedge polygons (three of each type) located near Utqiagvik, Alaska. A combination of soil pits, trenches, and cores were used to describe, sample, and map the cross-section stratigraphy of soil horizons and ice wedges for each polygon at 6 depth intervals. Observed soil horizons were assigned to four types with increasing amounts of organic components (mineral, mineral/organic, organic/mineral, and organic). The average ice contents of each soil horizon type below the permafrost boundary and wedge ice were weighted by their cross-sectional area fractions to calculate spatially averaged estimates of ice content for each polygon. In the active layer, spatially averaged estimates of volumetric water contents were similarly determined and reported here as “ice” content to enable estimates of the soil’s structurally competent porosity and excess ice in permafrost layers. In this dataset, the file AK13_ice_contents.csv includes cross-sectional area fractions and spatially averaged ice contents for soil layers and horizon types at the six depth intervals. The file AK13_permafrost_ice_fractions.csv contains the calculated partitioning of ice contents into pore ice and excess ice fractions for the three permafrost-dominated depth intervals. In addition, there is a data dictionary file for each of these data files and a file-level metadata file. These data were generated by the Department of Energy’s Soil Carbon Response to Environmental Change Scientific Focus Area and were used as inputs to model simulations examining the consequences of thaw-affected subsidence and microtopography change on active layer thickness of low-relief polygonal tundra landscapes in a warming Arctic.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1994

Hydrographic section across the Kuroshio near 35 deg N, 143 deg E

A closely spaced conductivity-temperature-depth/hydrographic section was conducted off the east coast of Japan in July 1992. The southeastward section crossed the Japan Trench and the Kuroshio in the vicinity of the Kashima 1 seamount. Vertical sections of temperature, salinity, density, oxygen, and nutrients are discussed in conjunction with the movement and interleaving of water masses. Complicated vertical and horizontal mixings of water masses are inferred from the temperature and salinity relationships. Mixing processes are patchy and not continuous beneath the front. Warm, salty water found beneath the Kurishio may result from upward mixing of water from intermediate depths. The main axis of the Kurishio, indicated by the 14 C isotherm at 200 m, is at 35.7 deg N, 142.6 deg E, about 20 km from the north wall surface thermal front. Geostrophic speeds exceed 170 cm/s at the surface; volume transport through the section is 81 x 10(exp 6) cu m/s.

Teague, W. J.↗
DOE OSTI2025

High-Spectral Resolution Lidar (HSRL) Instrument Handbook

High-spectral-resolution lidar (HSRL) systems provide vertical profiles of optical depth, backscatter cross-section, depolarization, and backscatter phase function. All HSRL measurements are calibrated by reference to molecular scattering, which is measured at each point in the lidar profile. Like the Raman lidar (RL), but unlike simple backscatter lidars such as the micropulse lidar (MPL), this enables the HSRL to measure backscatter cross-sections and optical depths without prior assumptions about the scattering properties of the atmosphere. The depolarization observations allow robust discrimination between ice and water clouds. Rigorous error estimates can be computed for all measurements. A very narrow angular field of view reduces multiple scattering contributions. The small field of view, coupled with a narrow optical bandwidth, nearly eliminates noise due to scattered sunlight. The laser transmitter is a diode-pumped, frequency-doubled Nd:YAG laser. Narrow-band, single-frequency operation is provided by injection seeding with a single-frequency, cw-diode-pumped diode laser. The main laser cavity is maintained in resonance with the seed laser by adjusting the cavity length to minimize the time between the Q-switch trigger and the emission of the laser pulse. The emission wavelength is tuned via temperature control of the seed laser crystal and is locked to line #1109 of the iodine absorption spectra. Locking is accomplished by minimizing the transmission through a 2-cm-long iodine absorption cell. Use of a high-repetition-rate laser and expansion of the transmitted beam through a 400-mm telescope reduces the transmitted energy density to eye-safe levels. It is possible to look directly into the output beam without hazard. The receiver and transmitter use the same afocal telescope, simplifying the maintenance of stable alignment of the transmitter and receiver although the angular FOV is only 100 μrad. The small FOV and the 4-kHz repetition rate also limit the near-field signal strength, making it possible to record continuous profiles that start at an altitude of ~100 m and extend to 30 km using photon counting detectors. The small FOV also suppresses multiple scattering contributions.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1982

A study of resonant-cavity and fiberglass-filled parallel baffles as duct silencers

Acoustical performance and pressure drop were measured for two types of splitters designed to attenuate sound propagating in ducts - resonant-cavity baffles and fiberglass-filled baffles. Arrays of four baffles were evaluated in the 7- by 10-foot wind tunnel number 1 at Ames Research Center at flow speeds from 0 to 41 m/sec. The baffles were 2.1 m high, 305 to 406 mm thick, and 3.1 to 4.4 m long. Emphasis was on measurements of silencer insertion loss as affected by variations of such parameters as baffle length, baffle thickness, perforated skin geometry, cavity size and shape, cavity damping, wind speed, and acoustic field directivity. An analytical method for predicting silencer performance is described and compared with measurements. With the addition of cavity damping in the form of 25-mm foam linings, the insertion loss above 250 Hz of the resonant-cavity baffles was improved 2 to 7 db compared with the undamped baffles; the loss became equal to or greater than the insertion loss of comparable size fiberglass baffles at frequencies above 250 Hz. Variations of cavity size and shape showed that a series of cavities with triangular cross-sections (i.e., variable depth) were superior to cavities with rectangular cross sections (i.e., constant depth). In wind, the undamped, resonant-cavity baffles generated loud cavity-resonance tones; the tones could be eliminated by cavity damping.

Soderman, P. T.↗
NASA NTRS2014

A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain

The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically <100micron) from the surface of an asteroid (25143 Itokawa). These precious samples provide important insights into early Solar System processes, but their sizes pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on sample preparation. We developed a hybrid technique combining traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for more thorough in situ investigations of grain surfaces and interiors. Using this method, we increase the number of FIB-prepared sections that can be recovered from a particle with dimensions on the order of tens of microns. These sections can be subsequently analyzed using a variety of analytical techniques. Particle RA-QD02-0211 is a approx. 40×40×20 micron particle from Itokawa containing olivine and Fe sulfides. It was embedded in low viscosity epoxy and partly sectioned to a depth of approx 10 micron; sections are placed on Cu grids with thin amorphous films for transmission electron microscope (TEM) analyses. With the sample surface partly exposed, the epoxy bullet is trimmed to a height of approx. 5mm to accommodate the allowable dimensions for FIB work (FEI Quanta 600 3D dual beam FIB-SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ≳3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.

Berger, Eve L.↗
DOE OSTI2024

Improved Three-Dimensional Reconstructions in Electron Ptychography through Defocus Series Measurements

A detailed analysis of ptychography for three-dimensional (3D) phase reconstructions of thick specimens is performed. Here, we introduce multi-focus ptychography, which incorporates a 4D-STEM defocus series to enhance the quality of 3D reconstructions along the beam direction through a higher overdetermination ratio. This method is compared with established multi-slice ptychography techniques, such as conventional ptychography, regularized ptychography, and multi-mode ptychography. Additionally, we contrast multi-focus ptychography with an alternative method that uses virtual optical sectioning through a reconstructed scattering matrix (S-matrix), which offers more precise 3D structure information compared to conventional ptychography. Our findings from multiple 3D reconstructions based on simulated and experimental data demonstrate that multi-focus ptychography surpasses other techniques, particularly in accurately reconstructing the surfaces and interface regions of thick specimens.

3D reconstruction↗
DOE OSTI2020

Elucidating the effect of preheating temperature on melt pool morphology variation in Inconel 718 laser powder bed fusion via simulation and experiment

In laser powder bed fusion (L-PBF) additive manufacturing, the mechanical performance, microstructure and defects of fabricated parts are closely associated with the melt pool morphology, e.g., its dimension and shape through the building process. Past studies have largely focused on how the process parameters such as laser power and scan speed affect melt pool characteristics. In this study, the melt pool morphology variation as a function of preheating temperature in the conduction, transition, and keyhole regimes and the underlying mechanisms in each regime are investigated through ex-situ sample characterization and computation thermal fluid dynamics (CtFD) simulation. Single tracks with different combinations of laser power and scan speed are deposited on an Inconel 718 bare plate preheated to a temperature range of 100–500 °C in the experiment. Significant changes are observed in melt pool morphology as a function of preheating temperature from optical measurements of melt track cross sections. The depth of melt pool in the three regimes increases monotonically with preheating temperature, e.g., at 500 °C, the experimental melt pool depth is increased by 49% in conduction regime, 34% in transition regime and 33% in keyhole regime, respectively, while the variation of melt pool width in each regime does not all follow an increasing trend but depends on the melt pool regimes. Melt pool width variation in the conduction and transition regimes is found to depend on the enhanced heat conduction directly related to temperature dependent thermal properties. Through validated CtFD simulations, it is found that in the keyhole regime the evaporation mass, recoil pressure, and laser drilling effect is enhanced with higher preheating temperature, which gives rise to a deeper melt pool. The simulations also reveal that preheating temperature significantly elongates the melt track length due to the increased flow rate and strong recoil pressure that accelerates the backward flow.

36 MATERIALS SCIENCE↗
NASA NTRS1974

Computer automation of ultrasonic testing

Report describes a prototype computer-automated ultrasonic system developed for the inspection of weldments. This system can be operated in three modes: manual, automatic, and computer-controlled. In the computer-controlled mode, the system will automatically acquire, process, analyze, store, and display ultrasonic inspection data in real-time. Flaw size (in cross-section), location (depth), and type (porosity-like or crack-like) can be automatically discerned and displayed. The results and pertinent parameters are recorded.

Yee, B. G. W.↗