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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 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Building Atomic and Plasmonic Devices via Electron Beams: from Desired Structures to Desired Properties

The evolution of the aberration correction in Scanning Transmission Electron Microscopy (STEM) has enabled multiple advances including high-resolution structural imaging, pm-level position detection of atomic columns, and ~3-5 mV resolution electron energy loss spectroscopy of the chemical and physical functionalities. These developments have further enabled the precise manipulation of the atomic structure of materials, including removal and formation of atomic planes in 3D materials, controlled atomic motion, and even direct atomic assembly of homo- and heteroatomic artificial molecules. Here, we will discuss several recent advances in STEM-EELS automated experiments as applied to quantum and nanoplasmonic systems.

42 ENGINEERING↗
DOE OSTI2024

Simulation Study of High-Precision Characterization of MeV Electron Interactions for Advanced Nano-Imaging of Thick Biological Samples and Microchips

The resolution of a mega-electron-volt scanning transmission electron microscope (MeV-STEM) is primarily governed by the properties of the incident electron beam and angular broadening effects that occur within thick biological samples and microchips. A precise understanding and mitigation of these constraints require detailed knowledge of beam emittance, aberrations in the STEM column optics, and energy-dependent elastic and inelastic critical angles of the materials being examined. This simulation study proposes a standardized experimental framework for comprehensively assessing beam intensity, divergence, and size at the sample exit. This framework aims to characterize electron-sample interactions, reconcile discrepancies among analytical models, and validate Monte Carlo (MC) simulations for enhanced predictive accuracy. Our numerical findings demonstrate that precise measurements of these parameters, especially angular broadening, are not only feasible but also essential for optimizing imaging resolution in thick biological samples and microchips. By utilizing an electron source with minimal emittance and tailored beam characteristics, along with amorphous ice and silicon samples as biological proxies and microchip materials, this research seeks to optimize electron beam energy by focusing on parameters to improve the resolution in MeV-STEM/TEM. This optimization is particularly crucial for in situ imaging of thick biological samples and for examining microchip defects with nanometer resolutions. Our ultimate goal is to develop a comprehensive mapping of the minimum electron energy required to achieve a nanoscale resolution, taking into account variations in sample thickness, composition, and imaging mode.

36 MATERIALS SCIENCE↗
NASA NTRS2005

High-Resolution Electron Energy-Loss Spectroscopy (HREELS) Using a Monochromated TEM/STEM

A 200 keV FEI TF20 XT monochromated (scanning) transmission electron microscope funded by NASA's SRLIDAP program is undergoing installation at Lawrence Livermore National Laboratory. Instrument specifications in STEM mode are Cs =1.0 mm, Cc =1.2 mm, image resolution =0.18 nm, and in TEM mode Cs =1.3 mm, Cc =1.3 mm, information limit =0.14 nm. Key features of the instrument are a voltage-stabilized high tension (HT) supply, a monochromator, a high-resolution electron energy-loss spectrometer/energy filter, a high-resolution annular darkfield detector, and a solid-state x-ray energy-dispersive spectrometer. The high-tension tank contains additional sections for 60Hz and high frequency filtering, resulting in an operating voltage of 200 kV plus or minus 0.005V, a greater than 10-fold improvement over earlier systems. The monochromator is a single Wien filter design. The energy filter is a Gatan model 866 Tridiem-ERS high resolution GIF spec d for less than or equal to 0.15 eV energy resolution with 29 pA of current in a 2 nm diameter probe. 0.13 eV has already been achieved during early installation. The x-ray detector (EDAX/Genesis 4000) has a take-off angle of 20 degrees, an active area of 30 square millimeters, and a solid angle of 0.3 steradians. The higher solid angle is possible because the objective pole-piece allows the detector to be positioned as close as 9.47 mm from the specimen. The voltage-stabilized HT supply, monochromator and GIF enable high-resolution electron energy-loss spectroscopy (HREELS) with energy resolution comparable to synchrotron XANES, but with approximately 100X better spatial resolution. The region between 0 and 100 eV is called the low-loss or valence electron energy-loss spectroscopy (VEELS) region where features due to collective plasma oscillations and single electron transitions of valence electrons are observed. Most of the low-loss VEELS features we are detecting are being observed for the first time in IDPs. A major focus of our research is to understand the origin and significance of these features and how they might be exploited to gain insight about IDPs and other meteoritic materials.

Sai, Z. R.↗
NASA NTRS2001

Cytoplasmic pH dynamics in maize pulvinal cells induced by gravity vector changes

In maize (Zea mays) and other grasses, changes in orientation of stems are perceived by pulvinal tissue, which responds to the stimulus by differential growth resulting in upward bending of the stem. The amyloplast-containing bundle sheath cells are the sites of gravity perception, although the initial steps of gravity perception and transmission remain unclear. In columella cells of Arabidopsis roots, we previously found that cytoplasmic pH (pH(c)) is a mediator in early gravitropic signaling (A.C. Scott, N.S. Allen [1999] Plant Physiol 121: 1291-1298). The question arises whether pH(c) has a more general role in signaling gravity vector changes. Using confocal ratiometric imaging and the fluorescent pH indicator carboxy seminaphtorhodafluor acetoxymethyl ester acetate, we measured pH(c) in the cells composing the maize pulvinus. When stem slices were gravistimulated and imaged on a horizontally mounted confocal microscope, pH(c) changes were only apparent within the bundle sheath cells, and not in the parenchyma cells. After turning, cytoplasmic acidification was observed at the sides of the cells, whereas the cytoplasm at the base of the cells where plastids slowly accumulated became more basic. These changes were most apparent in cells exhibiting net amyloplast sedimentation. Parenchyma cells and isolated bundle sheath cells did not show any gravity-induced pH(c) changes although all cell types responded to external stimuli in the predicted way: Propionic acid and auxin treatments induced acidification, whereas raising the external pH caused alkalinization. The results suggest that pH(c) has an important role in the early signaling pathways of maize stem gravitropism.

Non-NASA Center↗
DOE OSTI2025

Electron Microscopy Approaches to Unraveling the Structure of Amorphous Materials

Determining atomic structures in crystalline materials—where atoms are arranged in rigid, periodic lattices—has been highly successful using probes such as electrons, X-rays, and neutrons. In contrast, amorphous materials, despite their ubiquity and technological importance, remain far more challenging to characterize with comparable accuracy and precision. This review highlights existing, emerging, and potential (scanning) transmission electron microscopy ((S)TEM) techniques for probing short- and medium-range order in amorphous materials. Approaches ranging from high-resolution (S)TEM imaging and selected electron diffraction pattern to four-dimensional STEM (4D-STEM) based pair distribution function, fluctuation electron microscopy, tomography, ptychography, and spectroscopic methods are discussed, emphasizing their ability to provide complementary insights across multiple length scales—from sub-angstrom local environments to nanometer-scale correlations. Here, we further explore the promise of multimodal and correlative strategies, as well as the growing role of machine learning and physics-informed AI in enabling real-time, quantitative interpretation of complex structural signatures. Together, these advances point toward a future where electron microscopy not only reveals the hidden order in amorphous systems but also establishes robust structure–property relationships, paving the way for materials innovation in disordered matter.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS1994

Fluorescence imaging to quantify crop residue cover

Crop residues, the portion of the crop left in the field after harvest, can be an important management factor in controlling soil erosion. Methods to quantify residue cover are needed that are rapid, accurate, and objective. Scenes with known amounts of crop residue were illuminated with long wave ultraviolet (UV) radiation and fluorescence images were recorded with an intensified video camera fitted with a 453 to 488 nm band pass filter. A light colored soil and a dark colored soil were used as background for the weathered soybean stems. Residue cover was determined by counting the proportion of the pixels in the image with fluorescence values greater than a threshold. Soil pixels had the lowest gray levels in the images. The values of the soybean residue pixels spanned nearly the full range of the 8-bit video data. Classification accuracies typically were within 3(absolute units) of measured cover values. Video imaging can provide an intuitive understanding of the fraction of the soil covered by residue.

Daughtry, C. S. T.↗
DOE OSTI2025

Quantitative Modeling of High-Energy Electron Scattering in Thick Samples Using Monte Carlo Techniques

Cryo-electron microscopy (cryo-EM) is a powerful tool for imaging biological samples but is typically limited by sample thickness, which is restricted to a few hundred nanometers depending on the electron energy. However, there is a growing need for imaging techniques capable of studying biological samples up to 10 µm in thickness while maintaining nanoscale resolution. This need motivates the use of mega-electron-volt scanning transmission electron microscopy (MeV-STEM), which leverages the high penetration power of MeV electrons to generate high-resolution images of thicker samples. In this study, we employ Monte Carlo simulations to model electron–sample interactions and explore the signal decay of imaging electrons through thick specimens. By incorporating material properties, interaction cross-sections for energy loss, and experimental parameters, we investigate the relationship between the incident and transmitted beam intensities. Key factors such as detector collection angle, convergence semi-angle, and the material properties of samples were analyzed. Our results demonstrate that the relationship between incident and transmitted beam intensities follows the Beer–Lambert law over thicknesses ranging from a few microns to several tens of microns, depending on material composition, electron energy, and collection angles. The linear depth of silicon dioxide reaches 3.9 µm at 3 MeV, about 6 times higher than that at 300 keV. Meanwhile, the linear depth of amorphous ice reaches 17.9 µm at 3 MeV, approximately 11.5 times higher than that at 300 keV. These findings are crucial for advancing the study of thick biological and semiconductor samples using MeV-STEM.

36 MATERIALS SCIENCE↗
NASA NTRS2018

Water-Rock Interactions in Outer Solar System Bodies: Evidence from the Coordinated Analysis of Interplanetary Dust

NASA has an ongoing program of collecting interplanetary dust particles (IDPs) in the stratosphere using high altitude research aircraft. The collected IDPs are derived from asteroids and comets and here we report studies of a subset of hydrated IDPs rich in carbonaceous matter that are proposed to have a cometary origin. Our studies are aimed at understanding the evolution of oxygen reservoirs in the Solar System and their interaction with cometary minerals and organic matter. The small size (<20 μm) and fragility of these IDPs present a number of analytical challenges. We have pioneered techniques for performing chemical, mineralogical, isotopic, and spectroscopic measurements on the same sample in a carefully coordinated sequence. Coordinated analyses of nanogram-size samples is made possible by several delicate sample preparation techniques. To avoid organic contamination, we embed IDPs in elemental sulfur and use ultramicrotomy to partly section the particles (the first few micrometers). Multiple thin sections (50-70 nm thick) are placed on different substrates depending on the analysis technique. We use a JEOL 2500SE scanning, transmission electron microscope (STEM) to determine the mineralogy, microstructure, and elemental compositions of constituent minerals in the thin sections through a combination of high resolution imaging, electron diffraction, quantitative energy-dispersive x-ray mapping, and electron energy-loss spectroscopy. Following the STEM analyses, we use a NanoSIMS 50L for high spatial resolution isotopic measurements of H, C, N, and O to search for presolar grains and to understand the origin of the indigenous organic matter. The isotopic analyses are performed on the same sections analyzed in the STEM in order to correlate isotopic properties with the elemental and mineralogical data. We reserve other thin sections for non-destructive analyses utilizing synchrotron-based techniques including Fourier-transform infrared (FTIR) micro-spectroscopy and X-ray absorption near-edge structure (XANES) analyses, especially for functional group analysis of organic matter in the particles. The remainder of the IDP is extracted from the sulfur bead that was used for microtomy and is pressed into Au foil for quantitative analysis (including light elements) using a JEOL 8530F field emission electron probe microanalyzer (EPMA). After the EPMA measurements, high precision oxygen isotopic analyses are obtained using Cameca IMS1270/1290 instruments at UCLA. The hydrated IDPs in this study are dominated by saponitic clays, with minor magnetite, carbonate and abundant organic matter. The remarkable oxygen isotopic compositions, high carbon contents, and the abundance of isotopically anomalous organic matter, together suggest that the high carbon, hydrated IDPs are derived from primitive sources not yet represented in meteorite collections such as outer main belt P- and D-type asteroids or comets.

Keller, Lindsay P.↗
DOE OSTI2023

Multiscale electric-field imaging of polarization vortex structures in PbTiO 3 /SrTiO 3 superlattices

In ferroelectric heterostructures, the interaction between intrinsic polarization and the electric field generates a rich set of localized electrical properties. The local electric field is determined by several connected factors, including the charge distribution of individual unit cells, the interfacial electromechanical boundary conditions, and chemical composition of the interfaces. However, especially in ferroelectric perovskites, a complete description of the local electric field across micro-, nano-, and atomic-length scales is missing. Here, by applying four-dimensional scanning transmission electron microscopy (4D STEM) with multiple probe sizes matching the size of structural features, we directly image the electric field of polarization vortices in (PbTiO 3 ) 16 /(SrTiO 3 ) 16 superlattices and reveal different electric field configurations corresponding to the atomic scale electronic ordering and the nanoscale boundary conditions. The separability of two different fields probed by 4D STEM offers the possibility to reveal how each contributes to the electronic properties of the film.

36 MATERIALS SCIENCE↗
NASA NTRS2012

Coordinated STEM/FIB/NanoSIMS Analyses of Presolar Silicates in Comet Dust and Primitive Meteorites

Silicate grains were among the most abundant mineralogical building blocks of our Solar System. These grains were the detritus from earlier generations of stars that have been recycled in the early solar nebula. Rare sub-micrometer survivors of this processing have been identified in meteorites, micrometeorites and interplanetary dust particles (IDPs). These silicate grains are recognized as presolar in origin because of their extremely anomalous isotopic compositions that reflect nucleosynthetic processes in their stellar sources (evolved stars, novae and supernovae). We perform coordinated chemical, mineralogical and isotopic studies of these grains to determine their origins and histories. We examine the complex mineralogy and petrography of presolar silicates using imaging, diffraction and chemical data obtained from thin sections with the JSC JEOL 2500 field-emission STEM equipped with a Noran thin window energy dispersive x-ray (EDX) spectrometer and a Gatan Tridiem GIF. Quantitative element x-ray maps (spectrum images) are acquired by rastering a 4 nm incident probe whose dwell time is minimized to avoid beam damage and element diffusion during mapping. Successive image layers are acquired and combined in order to achieve approx 1% counting statistics for major elements. The IDP samples are prepared by ultramicrotomy of particles embedded in epoxy or elemental sulfur. After EDX mapping, the sections are subjected to C, N, and O isotopic imaging with the JSC NanoSIMS 50L ion microprobe. We prepare sections of some meteorite grains using the JSC FEI Quanta 3D focused ion beam (FIB) instrument. The specimen surface is protected from the FIB milling process by layers of electron beam-deposited C and Pt followed by an ion-deposited Pt layer. We also use the FIB to preferentially remove surrounding grains to reduce the background in subsequent NanoSIMS measurements. For mineralogical studies, we again employ the FIB instrument to deposit a protective cap over the grain of interest and then extract the grain and thin it to electron transparency for TEM analysis.

Keller, Lindsay↗
DOE OSTI2020

Electron tomography imaging methods with diffraction contrast for materials research

Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) enable the visualization of three-dimensional (3D) microstructures ranging from atomic to micrometer scales using 3D reconstruction techniques based on computed tomography algorithms. This 3D microscopy method is called electron tomography (ET) and has been utilized in the fields of materials science and engineering for more than two decades. Although atomic resolution is one of the current topics in ET research, the development and deployment of intermediate-resolution (non-atomic-resolution) ET imaging methods have garnered considerable attention from researchers. This research trend is probably not irrelevant due to the fact that the spatial resolution and functionality of 3D imaging methods of scanning electron microscopy (SEM) and X-ray microscopy have come to overlap with those of ET. In other words, there may be multiple ways to carry out 3D visualization using different microscopy methods for nanometer-scale objects in materials. From the above standpoint, this review paper aims to (i) describe the current status and issues of intermediate-resolution ET with regard to enhancing the effectiveness of TEM/STEM imaging and (ii) discuss promising applications of state-of-the-art intermediate-resolution ET for materials research with a particular focus on diffraction contrast ET for crystalline microstructures (superlattice domains and dislocations) including a demonstration of in situ dislocation tomography.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Apparatus and method for agricultural data collection and agricultural operations

Aspects of the subject disclosure may include, for example, obtaining video data from a single monocular camera, wherein the video data comprises a plurality of frames, wherein the camera is attached to a mobile robot that is travelling along a lane defined by a row of crops, wherein the row of crops comprises a first plant stem, and wherein the plurality of frames include a depiction of the first plant stem; obtaining robot velocity data from encoder(s), wherein the encoder(s) are attached to the robot; performing foreground extraction on each of the plurality of frames of the video data, wherein the foreground extraction results in a plurality of foreground images; and determining, based upon the plurality of foreground images and based upon the robot velocity data, an estimated width of the first plant stem. Additional embodiments are disclosed.

Chowdhary, Girish↗
DOE OSTI2022

Single atoms and small clusters of atoms may accompany Au and Pd dendrimer-encapsulated nanoparticles

Here we report the presence of small clusters of atoms (<1 nm) (SCs) and single atoms (SAs) in solutions containing 1–2 nm dendrimer-encapsulated nanoparticles (DENs). Au and Pd DENs were imaged using aberration-corrected scanning transmission electron microscopy (ac-STEM), and energy dispersive spectroscopy (EDS) was used to identify and quantify the SAs/SCs. Two main findings have emerged from this work. First, the presence or absence of SAs/SCs depends on both the terminal functional group of the dendrimer (–NH 2 or –OH) and the elemental composition of the DENs (Au or Pd). Second, dialysis can be used to remove the majority of SAs/SCs in cases where a high density of SAs/SCs are present. The foregoing conclusions provide insights into the mechanisms for Au and Pd DEN synthesis and stability. Ultimately, these results demonstrate the need for careful characterization of systems containing nanoparticles to ensure that SAs/SCs, which may be below the detection limit of most analytical methods, are taken into consideration (especially for catalysis experiments).

74 ATOMIC AND MOLECULAR PHYSICS↗
NASA NTRS2013

Coordinated in Situ Analyses of Organic Nanoglobules in the Sutter's Mill Meteorite

The Sutter's Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Here we report in-situ analyses of organic nanoglobules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).

Nakamura-Messenger, K.↗
NASA NTRS2013

Coordinated In Situ Analyses of Organic Nanoglobules in the Sutter's Mill Meteorite

The Sutter s Mill meteorite is a newly fallen carbonaceous chondrite that was collected and curated quickly after its fall [1]. Preliminary petrographic and isotopic investigations suggest affinities to the CM2 carbonaceous chondrites. The primitive nature of this meteorite and its rapid recovery provide an opportunity to investigate primordial solar system organic matter in a unique new sample. Organic matter in primitive meteorites and chondritic porous interplanetary dust particles (CP IDPs) is commonly enriched in D/H and N-15/N-14 relative to terrestrial values [2-4]. These anomalies are ascribed to the partial preservation of presolar cold molecular cloud material [2]. Some meteorites and IDPs contain gm-size inclusions with extreme H and N isotopic anomalies [3-5], possibly due to preserved primordial organic grains. The abundance and isotopic composition of C in Sutter's Mill were found to be similar to the Tagish Lake meteorite [6]. In the Tagish Lake meteorite, the principle carriers of large H and N isotopic anomalies are sub-micron hollow organic spherules known as organic nanoglobules [7]. Organic nanoglobules are commonly distributed among primitive meteorites [8, 9] and cometary samples [10]. Here we report in-situ analyses of organic nano-globules in the Sutter's Mill meteorite using UV fluorescence imaging, Fourier-transform infrared spectroscopy (FTIR), scanning transmission electron microscopy (STEM), NanoSIMS, and ultrafast two-step laser mass spectrometry (ultra-L2MS).

Nakamura--Messenger, K.↗
NASA NTRS2017

Evidence from IRIS that Sunspot Large Penumbral Jets Spin

Recent observations from Hinode (SOT/FG) revealed the presence of large penumbral jets (widths ≥ 500 km, larger than normal penumbral microjets, which have widths < 400 km) repeatedly occurring at the same locations in a sunspot penumbra, at the tail of a filament or where the tails of several penumbral filaments apparently converge (Tiwari et al. 2016, ApJ). These locations were observed to have mixed-polarity flux in Stokes-V images from SOT/FG. Large penumbral jets displayed direct signatures in AIA 1600, 304, 171, and 193 channels; thus they were heated to at least transition region temperatures. Because large jets could not be detected in AIA 94 Å, whether they had any coronal-temperature plasma remains unclear. In the present work, for another sunspot, we use IRIS Mg II k 2796 Å slit jaw images and spectra and magnetograms from Hinode SOT/FG and SOT/SP to examine: whether penumbral jets spin, similar to spicules and coronal jets in the quiet Sun and coronal holes; whether they stem from mixed-polarity flux; and whether they produce discernible coronal emission, especially in AIA 94 Å images. The few large penumbral jets for which we have IRIS spectra show evidence of spin. If these have mixed-polarity at their base, then they might be driven the same way as coronal jets and CMEs.

Tiwari, Sanjiv K.↗
DOE OSTI2021

Correlative analysis of structure and chemistry of Li x FePO 4 platelets using 4D-STEM and X-ray ptychography

Lithium iron phosphate (Li x FePO 4 ), a cathode material used in rechargeable Li-ion batteries, phase separates upon de/lithiation under equilibrium. The interfacial structure and chemistry within these cathode materials affects Li-ion transport, and therefore battery performance. Here, correlative imaging of Li x FePO 4 was performed using four-dimensional scanning transmission electron microscopy (4D-STEM), scanning transmission X-ray microscopy (STXM), and X-ray ptychography in order to analyze the local structure and chemistry of the same particle set. Over 50,000 diffraction patterns from 10 particles provided measurements of both structure and chemistry at a nanoscale spatial resolution (16.6–49.5 nm) over wide (several micron) fields-of-view with statistical robustness. Li x FePO 4 particles at varying stages of delithiation were measured to examine the evolution of structure and chemistry as a function of delithiation. In lithiated and delithiated particles, local variations were observed in the degree of lithiation even while local lattice structures remained comparatively constant, and calculation of linear coefficients of chemical expansion suggest pinning of the lattice structures in these populations. Partially delithiated particles displayed broadly core–shell-like structures, however, with highly variable behavior both locally and per individual particle that exhibited distinctive intermediate regions at the interface between phases, and pockets within the lithiated core that correspond to FePO 4 in structure and chemistry. The results provide insight into the Li x FePO 4 system, subtleties in the scope and applicability of Vegard’s law (linear lattice parameter-composition behavior) under local versus global measurements, and demonstrate a powerful new combination of experimental and analytical modalities for bridging the crucial gap between local and statistical characterization.

25 ENERGY STORAGE↗
DOE OSTI2021

Wide Dynamic Range, 10 kHz Framing Detector for 4D-STEM

Hybrid pixel array detectors (PADs) have expanded the fidelity, frame rate and dynamic range for diffractive imaging in electron microscopes. With their high detective quantum efficiencies (DQE), the noise performance limited is by counting statistics. Consequently, improving the precision and quality of high-speed images requires increasing the linear dynamic range and the maximum usable beam current. Here we describe a new prototype hybrid PAD, our next-generation electron microscope pixel array detector (NG-EMPAD) that expands both the framing speed and dynamic range of our earlier EMPAD design. Like the EMPAD, electrons are detected directly in a 500 μm thick silicon sensor bonded pixel-by-pixel to a custom signal processing integrated circuit (IC). Each pixel in the IC integrates charge carriers produced by the high-energy incident electrons. Here, in-pixel circuitry uses a combination of techniques to extend the dynamic range, including adaptive gain switching and the quantitative excess charge dumping similar to the EMPAD. In-pixel buffering of signals during readout allows acquiring a new image while reading out the previously collected image, yielding an image collection duty cycle of nearly 100%.

36 MATERIALS SCIENCE↗