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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 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Multislice Electron Tomography Using Four-Dimensional Scanning Transmission Electron Microscopy

Electron tomography offers useful three-dimensional (3D) structural information, which cannot be observed by two-dimensional imaging. By combining annular dark-field scanning transmission electron microscopy (ADF STEM) with aberration correction, the resolution of electron tomography has reached atomic resolution. However, tomography based on ADF STEM inherently suffers from several issues, including a high electron-dose requirement, poor contrast for light elements, and artifacts from image-contrast nonlinearity. Here, we develop an alternative method called multislice electron tomography (MSET) based on four-dimensional STEM tilt series. In this study, our simulations show that multislice-based 3D reconstruction can effectively reduce undesirable reconstruction artifacts from the nonlinear contrast, allowing precise determination of atomic structures with improved sensitivity for low-Z elements, at considerably low electron-dose conditions. We expect that the MSET method can be applied to a wide variety of materials, including radiation-sensitive samples and materials containing light elements whose 3D atomic structures have never been fully elucidated due to electron-dose limitations or nonlinear imaging contrast.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2023

Mending cracks atom-by-atom in rutile TiO2 with electron beam radiolysis

Abstract Rich electron-matter interactions fundamentally enable electron probe studies of materials such as scanning transmission electron microscopy (STEM). Inelastic interactions often result in structural modifications of the material, ultimately limiting the quality of electron probe measurements. However, atomistic mechanisms of inelastic-scattering-driven transformations are difficult to characterize. Here, we report direct visualization of radiolysis-driven restructuring of rutile TiO 2 under electron beam irradiation. Using annular dark field imaging and electron energy-loss spectroscopy signals, STEM probes revealed the progressive filling of atomically sharp nanometer-wide cracks with striking atomic resolution detail. STEM probes of varying beam energy and precisely controlled electron dose were found to constructively restructure rutile TiO 2 according to a quantified radiolytic mechanism. Based on direct experimental observation, a “two-step rolling” model of mobile octahedral building blocks enabling radiolysis-driven atomic migration is introduced. Such controlled electron beam-induced radiolytic restructuring can be used to engineer novel nanostructures atom-by-atom.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Formation of Mn-rich interfacial phases in Co 2 Fe x Mn 1-x Si thin films

Here, we report the formation of Mn-rich regions at the interface of Co 2 Fe x Mn 1-x Si thin films grown on GaAs substrates by molecular beam epitaxy (MBE). Scanning transmission electron microscopy (STEM) with electron energy loss (EEL) spectrum imaging reveals that each interfacial region: (1) is 1–2 nm wide, (2) occurs irrespective of the Fe/Mn composition ratio and in both Co-rich and Co-poor films, and (3) displaces both Co and Fe indiscriminately. We also observe a Mn-depleted region in each film directly above each Mn-rich interfacial layer, roughly 3 nm in width in the x = 0 and x = 0.3 films, and 1 nm in the x = 0.7 (less Mn) film. We posit that growth energetics favor Mn diffusion to the interface even when there is no significant Ga interdiffusion into the epitaxial film. Element-specific X-ray magnetic circular dichroism (XMCD) measurements show larger Co, Fe, and Mn orbital to spin magnetic moment ratios compared to bulk values across the Co 2 Fe x Mn 1-x Si compositional range. The values lie between reported values for pure bulk and nanostructured Co, Fe, and Mn materials, corroborating the non-uniform, layered nature of the material on the nanoscale. Finally, SQUID magnetometry demonstrates that the films deviate from the Slater-Pauling rule for uniform films of both the expected and the measured composition. The results inform a need for care and increased scrutiny when forming Mn-based magnetic thin films on III-V semiconductors like GaAs, particularly when films are on the order of 5 nm or when interface composition is critical to spin transport or other device applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Using X-ray spectrum imaging to quantify fission gas in high-burnup UO2 fuel

Analysis of fission gas bubbles (FGBs) in light-water reactor (LWR) fuel is needed to improve the understanding and predictive capability of fuel evolution under normal- and transient conditions. One of the most important parameters of a FGB is the pressure of the gas, primarily Xe, inside it. Bubble volume and location (inter- vs. intragranular) are important considerations as well. However, experimental analysis of such bubbles is challenging due to their small size and embedded nature, and usefulness of the data requires large numbers be analyzed. This paper proposes a method to measure the pressure of Xe bubbles using X-ray spectrum imaging (XSI) in scanning transmission electron microscopy (STEM). From X-ray generation and instrumental parameters, the number of Xe atoms yielding a given number of Xe L-series X-ray counts is estimated, and then from the estimated volume of the bubble the Xe density is estimated, which can then be converted to pressure via an equation-of-state. We apply the method to XSI datasets from high burnup (HBu) fuel from North Anna 1 reactor in as-irradiated and post-LOCA-test conditions and find Xe pressures in the FGBs clustered around 1 GPa.

Parish, Chad [ORNL] (ORCID:0000000312097439)↗
DOE OSTI2024

Domain nucleation across the metal-insulator transition of self-strained V 2 O 3 films

Bulk V 2 O 3 features concomitant metal-insulator (MIT) and structural (SPT) phase transitions at T C ~ 160 K. In thin films, where the substrate clamping can impose geometrical restrictions on the SPT, the epitaxial relation between the V 2 O 3 film and substrate can have a profound effect on the MIT. Here we present a detailed characterization of domain nucleation and growth across the MIT in (001)-oriented V 2 O 3 films grown on sapphire. By combining scanning electron transmission microscopy (STEM) and photoelectron emission microscopy (PEEM), we imaged the MIT with planar and vertical resolution. We observed that upon cooling, insulating domains nucleate at the top of the film, where strain is lowest, and expand downwards and laterally. This growth is arrested at a critical thickness of 50 nm from the substrate interface, leaving a persistent bottom metallic layer. As a result, the MIT cannot take place in the interior of films below this critical thickness. However, PEEM measurements revealed that insulating domains can still form on a very thin superficial layer at the top interface. Our results demonstrate the intricate spatial complexity of the MIT in clamped V 2 O 3 , especially the strain-induced large variations along the c axis. Finally, engineering the thickness-dependent MIT can provide an unconventional way to build out-of-plane geometry devices by using the persistent bottom metal layer as a native electrode.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2007

Simulation Studies of Forest Structure using 3D Lidar and Radar Models

The use of lidars and radars to measure forest structure attributes such as height and biomass are being considered for future Earth Observation missions. Large footprint lidar makes a direct measurement of the heights of scatterers in the illuminated footprint and can yield information about the vertical profile of the canopy. Synthetic Aperture Radar (SAR) is known to sense the canopy volume, especially at longer wavelengths and is useful for estimating biomass. Interferometric SAR (InSAR) has been shown to yield forest canopy height information. For example, the height of scattering phase retrieved from InSAR data is considered to be correlated with the three height and the spatial structure of the forest stand. There is much interest in exploiting these technologies separately and together to get important information for carbon cycle and ecosystem science. More detailed information of the electromagnetic radiation interactions within forest canopies is needed. And backscattering models can be of much utility here. As part of a NASA funded project to explore data fusion, a three-dimensional (3D) coherent radar backscattering model and a 3D lidar backscatter models were used to investigate the use of large footprint lidar, SAR and InSAR for characterizing realistic forest scenes. For this paper, we use stem maps and other forest measurements to develop a realistic spatial structure of a spruce-hemlock forest canopy found in Maine, USA. The radar and lidar models used measurements of the 3D forest scene as input and simulated the coherent radar backscattering signature and 1064nm energy backscatter, respectively. The relationships of backscatter derived forest structure were compared with field measurements. In addition, we also had detailed airborne lidar (Laser Imaging Vegetation Sensor, LVIS) data available over the stem map sites that was used to study the accuracies of tree height derived from modeled SAR backscatter and the scattering phase center retrieved from the simulated InSAR data will be compared with the height indices, or other structure parameters derived from the lidar data. These results will address the possible synergies between lidar and radar in data in terms of forest structural information.

Sun, Guoqing↗
DOE OSTI2021

4D-STEM of Beam-Sensitive Materials

We report that a scanning electron nanobeam diffraction, or 4D-STEM (four-dimensional scanning transmission electron microscopy), is a flexible and powerful approach to elucidate structure from "soft" materials that are challenging to image in the transmission electron microscope because their structure is easily damaged by the electron beam. In a 4D-STEM experiment, a converged electron beam is scanned across the sample, and a pixelated camera records a diffraction pattern at each scan position. This four-dimensional data set can be mined for various analyses, producing maps of local crystal orientation, structural distortions, crystallinity, or different structural classes. Holding the sample at cryogenic temperatures minimizes diffusion of radicals and the resulting damage and disorder caused by the electron beam. The total fluence of incident electrons can easily be controlled during 4D-STEM experiments by careful use of the beam blanker, steering of the localized electron dose, and by minimizing the fluence in the convergent beam thus minimizing beam damage. This technique can be applied to both organic and inorganic materials that are known to be beam-sensitive; they can be highly crystalline, semicrystalline, mixed phase, or amorphous. One common example is the case for many organic materials that have a π-π stacking of polymer chains or rings on the order of 3.4-4.2 Å separation. If these chains or rings are aligned in some regions, they will produce distinct diffraction spots (as would other crystalline spacings in this range), though they may be weak or diffuse for disordered or weakly scattering materials. We can reconstruct the orientation of the π-π stacking, the degree of π-π stacking in the sample, and the domain size of the aligned regions. This Account summarizes illumination conditions and experimental parameters for 4D-STEM experiments with the goal of producing images of structural features for materials that are beam-sensitive. We will discuss experimental parameters including sample cooling, probe size and shape, fluence, and cameras. 4D-STEM has been applied to a variety of materials, not only as an advanced technique for model systems, but as a technique for the beginning microscopist to answer materials science questions. It is noteworthy that the experimental data acquisition does not require an aberration-corrected TEM but can be produced on a variety of instruments with the right attention to experimental parameters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Physics Discovery in Nanoplasmonic Systems via Autonomous Experiments in Scanning Transmission Electron Microscopy

Abstract Physics‐driven discovery in an autonomous experiment has emerged as a dream application of machine learning in physical sciences. Here, this work develops and experimentally implements a deep kernel learning (DKL) workflow combining the correlative prediction of the target functional response and its uncertainty from the structure, and physics‐based selection of acquisition function, which autonomously guides the navigation of the image space. Compared to classical Bayesian optimization (BO) methods, this approach allows to capture the complex spatial features present in the images of realistic materials, and dynamically learn structure–property relationships. In combination with the flexible scalarizer function that allows to ascribe the degree of physical interest to predicted spectra, this enables physical discovery in automated experiment. Here, this approach is illustrated for nanoplasmonic studies of nanoparticles and experimentally implemented in a truly autonomous fashion for bulk‐ and edge plasmon discovery in MnPS 3 , a lesser‐known beam‐sensitive layered 2D material. This approach is universal, can be directly used as‐is with any specimen, and is expected to be applicable to any probe‐based microscopic techniques including other STEM modalities, scanning probe microscopies, chemical, and optical imaging.

42 ENGINEERING↗
DOE OSTI2020

Atomic-Scale Structural Mapping of Active Sites in Monolayer PGM-Free Catalysts by Low-Voltage 4D-STEM

Two-dimensional (2D) materials have attracted a large amount of attention in both basic and applied fields, and scanning transmission electron microscopy (STEM) is often uniquely well-suited for characterizing the atomic-scale structure of these materials [1-4]. As a result, STEM is poised to significantly impact progress on platinum group metal (PGM)-free catalysts, which are currently under intense development to enable low-cost, commercially viable hydrogen fuel cells [5]. While recent advancements have resulted in fuel cell performance comparable to Pt catalysts by some measures [6], cell durability remains a significant challenge, limiting practical applications [7]. Catalytically active sites in PGM-free materials are proposed to be FeN4 complexes embedded in a graphene lattice (Fig. 1b) within layered or other larger materials, but this is still under debate largely due to the range of potential actives sites predicted by computational methods and lack of methods for directly validating these models [5]. Fundamental insights into the atomic structure and resulting degradation pathways of proposed active sites are therefore needed to fully understand and control cell performance and durability [6].2D materials typically make ideal samples for STEM, but those within PGM-free catalysts present additional challenges since these materials are often defect-rich, with a high density of edges, dopant atoms, etc., which significantly increase susceptibility to beam damage at standard operating voltages. This makes analysis of potential FeN4 active sites particularly challenging, since a large proportion of Fe exists at edge sites where beam-induced atomic displacements can prohibit high-resolution structural characterization [6]. Conventional dark-field imaging compounds this problem by producing less signal for a given dose and being less sensitive to light elements than dose-efficient phase contrast imaging techniques such as those enabled by four-dimensional (4D)-STEM [8-10] (Fig. 1a). Consequently, active site structural analysis is often left to methods such as low-resolution imaging combined with quantum chemical calculations [6], which hinders accurate determination of reaction and degradation mechanisms.Here, we demonstrate direct atomic-scale structural mapping of FeN4 sites by performing low-voltage 4D-STEM on a model PGM-free catalyst system with many exposed monolayer regions. To accomplish this, we pair a 30 keV aberration-corrected probe with a fast pixelated detector that has optimal performance at low beam voltages [11]. This enables us to simultaneously image light and heavy elements with high signal-to-noise by center-of-mass analysis (Fig. 1c) while minimizing beam-induced atomic displacements at sensitive sites. The monolayer nature of these materials additionally allows for experimental validation by direct comparison with multislice simulations [12] of model structures (Fig. 1d-e). This work demonstrates how low-voltage 4D-STEM will provide new insights into the atomic-scale structure and degradation mechanisms of active sites in PGM-free catalysts, facilitating the development of low-cost hydrogen fuel cells and other energy conversion technologies in the future [13].

Zachman, Michael↗
DOE OSTI2022

Spatial resolution in secondary-electron microscopy

Here, we first review the significance of resolution and contrast in electron microscopy, and the effect of the electron optics on these two quantities. We then outline the physics of the generation of secondary electrons (SE) and their transport and emission from the surface of a specimen. Contrast and resolution are discussed for different kinds of SE imaging in scanning (SEM) and scanning-transmission (STEM) instruments, with some emphasis on the observation of individual atoms and atomic columns in a thin specimen. The possibility of achieving atomic resolution from a bulk specimen at SEM energies is also considered.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Relaxing Direct Ptychography Sampling Requirements via Parallax Imaging Insights

Direct ptychography enables the retrieval of information encoded in the phase of an electron wave passing through a thin sample by deconvolving the interference effects of a converged probe with known aberrations. Under the weak phase object approximation, this permits the optimal transfer of information using noniterative techniques. However, the achievable resolution of the technique is traditionally limited by the probe step size—setting stringent Nyquist sampling requirements. At the same time, parallax imaging has emerged as a dose-efficient phase technique which relaxes sampling requirements and enables scan-upsampling. Here, we formulate parallax imaging as a quadratic approximation to part of the direct ptychography kernel and use this insight to enable upsampling in direct ptychography. We validate our analytical results numerically using simulated and experimental reconstructions.

direct ptychography, parallax imaging, scan Nyquis↗
NASA NTRS1993

Development Of Software To Recognize Parts Of Plants

Report describes first phase in development of digital image-processing subsystem recognizing parts of plants. Subsystem part of robotic system tending and harvesting plants in automated plant-growth chamber. Initial focus on image-processing software that distinguishes among seed heads, stems, and leaves of wheat plants and further distinguishes between these parts and background. Software adaptable to other types of plants.

Despain, Ronald R.↗
NASA NTRS1997

Combustion of PTFE: The Effects of Gravity and Pigmentation on Ultrafine Particle Generation

Ultrafine particles generated during polymer thermodegradation are a major health hazard, owing to their unique pathway of processing in the lung. This hazard in manned spacecraft is poorly understood, because the particulate products of polymer thermodegradation are generated under low gravity conditions. Particulate generated from the degradation of PolyTetraFluoroEthylene (PTFE), insulation coating for 20 AWG copper wire (representative of spacecraft application) under intense ohmic heating were studied in terrestrial gravity and microgravity. Microgravity tests were done in a 1.2-second drop tower at the Colorado School of Mines (CSM). Thermophoretic sampling was used for particulate collection. Transmission Electron Microscopy (TEM) and Scanning Transmission Electron Microscopy (STEM) were used to examine the smoke particulates. Image software was used to calculate particle size distribution. In addition to gravity, the color of PTFE insulation has an overwhelming effect on size, shape and morphology of the particulate. Nanometer-sized primary particles were found in all cases, and aggregation and size distribution was dependent on both color and gravity; higher aggregation occurred in low gravity. Particulates from white, black, red and yellow colored PTFE insulations were studied. Elemental analysis of the particulates shows the presence of inorganic pigments.

McKinnon, J. Thomas↗
DOE OSTI2023

Starch depletion in the xylem and phloem ray parenchyma of grapevine stems under drought

Abstract While nonstructural carbohydrate (NSC) storage can support long-lived woody plants during abiotic stress, the timing and extent of their use are less understood, as are the thresholds for cell mortality as NSCs and water supplies are consumed. Here, we combine physiological and imaging tools to study the response of Vitis riparia to a 6-week experimental drought. We focused on the spatial and temporal dynamics of starch consumption and cell viability in the xylem and phloem of the stem. Starch dynamics were further corroborated with enzymatic starch digestion and X-ray microcomputed tomography imaging. Starch depletion in the stems of droughted plants was detected after 2 weeks and continued over time. We observed distinct differences in starch content and cell viability in the xylem and phloem. By the end of the drought, nearly all the starch was consumed in the phloem ray parenchyma (98 % decrease), and there were almost no metabolically active cells in the phloem. In contrast, less starch was consumed in the xylem ray parenchyma (30 % decrease), and metabolically active cells remained in the ray and vessel-associated parenchyma in the xylem. Our data suggest that the higher proportion of living cells in the phloem and cambium, combined with smaller potential NSC storage area, rapidly depleted starch, which led to cell death. In contrast, the larger cross-sectional area of the xylem ray parenchyma with higher NSC storage and lower metabolically active cell populations depleted starch at a slower pace. Why NSC source-sink relationships between xylem and phloem do not allow for a more uniform depletion of starch in ray parenchyma over time is unclear. Our data help to pinpoint the proximate and ultimate causes of plant death during prolonged drought exposure and highlight the need to consider the influence of within-organ starch dynamics and cell mortality on abiotic stress response.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1984

Measurement of thigmomorphogenesis and gravitropism by non-intrusive computerized video image processing

A video image processing instrument, DARWIN (Digital Analyser of Resolvable Whole-pictures by Image Numeration), was developed. It was programmed to measure stem or root growth and bending, and coupled to a specially mounted video camera to be able to automatically generate growth and bending curves during gravitropism. The growth of the plant is recorded on a video casette recorder with a specially modified time lapse function. At the end of the experiment, DARWIN analyses the growth or movement and prints out bending and growth curves. This system was used to measure thigmomorphagenesis in light grown corn plants. If the plant is rubbed with an applied force load of 0.38 N., it grows faster than the unrubbed control, whereas 1.14 N. retards its growth. Image analysis shows that most of the change in the rate of growth is caused in the first hour after rubbing. When DARWIN was used to measure gravitropism in dark grown oat seedlings, it was found that the top side of the shoot contracts during the first hour of gravitational stimulus, whereas the bottom side begins to elongate after 10 to 15 minutes.

Jaffe, M. J.↗
NASA NTRSDate not supplied

Dynamic Analysis of Reynolds Number Effects on Trailing Edge Transonic Vortex Shedding and Its Impact on Turbine Blade Aerodynamic Performance

In this work, we will discuss observations from images acquired from a time-resolved, high-speed self-aligned focusing Schlieren campaign that was performed at the CW-22 facility at NASA Glenn Research Center to understand the dynamic behavior of thick trailing-edge high-pressure turbine blades simulating a ceramic matrix composite (CMC) construction at high inlet turbulence conditions. For the CMC-9 blade, which has a trailing edge thickness of 9% of the axial chord, we identified a regime where an excessive total pressure loss (loss anomaly) is observed only for a narrow range of Reynolds numbers at a fixed exit Mach number of 0.74. The loss anomaly is qualitatively explained by our images, which were taken at 10 distinct blade Reynolds numbers spanning a factor of 6. The images show a significant increase in energy related to the oscillations due to transonic vortex shedding at the Reynolds numbers related to the high loss conditions. This increased energy leads to the formation of strong acoustic waves that turn into shock waves at the highest loss conditions. From our observations stemming from Spectral POD analysis of the high-speed images, we see the acoustic waves produced by the trailing edge vortex shedding exist in all conditions tested; but the shedding frequency has a very slight trend upwards as the Reynolds number is increased, varying about 6% in the range tested. Considering this variation of shedding frequency as a function of Reynolds number, which is well-established for other bluff-body flows, we stipulate there may be a potential feedback mechanism involving an acoustic information transfer path across neighboring blades that may explain why only a narrow range of Reynolds numbers displays strong, shock-forming vortex shedding. We consider a few feedback paths and examine the timing based on the mean flow field from a high-resolution LES simulation. It appears that all feedback mechanisms are viable, presenting an integer number of delay cycles with respect to disturbances generated at the trailing edge. Most noteworthy, however, is the acoustic/shock-boundary layer interaction mechanism at the blade geometric throat. Based on our analysis, this mechanism likely plays an important role in realistic, curved turbine blade passages.

Aerodynamics↗