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At least 91 records · Page 5

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DOE OSTI2026

Structural and Mechanical Analysis of Individual Mineralized Collagen Fibrils Using In Situ Transmission Electron Microscopy

Bone serves as an example of nature’s architectured material with its characteristic blend of strength and toughness, all at a lightweight design. Given the hierarchical nature of these materials, it is essential to understand the governing mechanisms and organization of their constituents across length scales for bioinspired structural design. Despite recent advances in transmission electron microscopy (TEM) that have allowed us to witness the hierarchical arrangement of bone at micro-down to the nanoscale, we are still missing the details about the structural organization and mechanical properties of the main building blocks of bone─mineralized collagen fibrils (MCFs). Here, we present a method to extract individual MCFs from nature’s model material, mineralized turkey leg tendon, using a dropcasting procedure. By isolating the MCFs onto TEM supporting grids, we visualized the arrangement of organic and mineral phases within individual MCFs at the nanoscale. Using a four-dimensional scanning transmission electron microscopy (4D-STEM) approach, the orientation of individual mineral crystals within the MCFs was examined. Furthermore, we conducted in situ tensile experiments, revealing exceptional tensile strains of at least 8%, demonstrating the intricate relationship between structural organization and the mechanical behavior of MCFs. These insights into the ultrastructure of mineralized tissue building blocks, as well as the proposed sample-extraction method compatible with in situ mechanical testing, provide a strong basis for research into nature-inspired material design.

4D-STEM↗

DOE OSTI2024

Near-field imaging of optical resonances in silicon metasurfaces using photoelectron microscopy

Precise control of light–matter interactions at the nanoscale lies at the heart of nanophotonics. However, experimental examination at this length scale is challenging since the corresponding electromagnetic near-field is often confined within volumes below the resolution of conventional optical microscopy. In semiconductor nanophotonics, electromagnetic fields are further restricted within the confines of individual subwavelength resonators, limiting access to critical light–matter interactions in these structures. In this work, we demonstrate that photoelectron emission microscopy (PEEM) can be used for polarization-resolved near-field spectroscopy and imaging of electromagnetic resonances supported by broken-symmetry silicon metasurfaces. We find that the photoemission results, enabled through an in situ potassium surface layer, are consistent with full-wave simulations and far-field reflectance measurements across visible and near-infrared wavelengths. In addition, we uncover a polarization-dependent evolution of collective resonances near the metasurface array edge taking advantage of the far-field excitation and full-field imaging of PEEM. Here, we deduce that coupling between eight resonators or more establishes the collective excitations of this metasurface. All told, we demonstrate that the high-spatial resolution hyperspectral imaging and far-field illumination of PEEM can be leveraged for the metrology of collective, non-local, optical resonances in semiconductor nanophotonic structures.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2025

Morphological Characterization of Uranyl Fluoride Particles via Atomic Force Microscopy

Uranium hexafluoride (UF 6 ) undergoes a rapid hydrolysis reaction when exposed to atmospheric water. In addition to producing hazardous HF gas, the hydrolysis reaction produces uranyl fluoride (UO 2 F 2 ), a radioactive solid phase particulate material. Because of the technological utility of UF 6 in the nuclear fuel cycle, understanding the transport properties of UO 2 F 2 aerosol produced via UF 6 hydrolysis is important for accident scenarios. Moreover, the fundamental chemical and physical properties of the UF 6 hydrolysis reaction are not completely understood. Recently, several experiments on the aerosol phase properties of UO 2 F 2 produced in this way have shown that under most relevant conditions, the particle size distribution (PSD) of UO 2 F 2 can be extremely small, approximately 3 to 5 nm, which is well below the threshold that can be routinely observed via scanning electron microscopy (SEM). Although readily observable in the aerosol phase, observation of nanometer-sized particles in the condensed phase (i.e. deposited on surfaces) remains a challenge. Here, in this study, we have used atomic force microscopy (AFM) to study the PSD and morphological characteristics of UO 2 F 2 deposited at low and high concentrations under different humidity conditions, a primary variable in the hydrolysis reaction. Here, we find strong agreement between PSD measured in the aerosol phase via scanning mobility particle sizing and PSD measured via AFM, with particle sizes peaked below 4 nm for low-humidity conditions. At higher humidity, the distribution is centered around 5 to 10 nm but extends up to 20 nm. These results are in stark contrast to previous measurements using SEM that show PSD on the order of 300- to 1000-nm particle sizes; moreover, these are the first direct measurements of individual particles of UO 2 F 2 having been produced via UF 6 hydrolysis deposited on surfaces. These measurements, therefore, open a new avenue for collecting and detecting UO 2 F 2 in the condensed phase and further refine the PSD, which is critical for environmental transport determinations.

Uranium hexafluoride↗

DOE OSTI2025

Quantitative phase retrieval and characterization of magnetic nanostructures via Lorentz (scanning) transmission electron microscopy

Magnetic materials phase reconstruction using Lorentz transmission electron microscopy (LTEM) measurements have traditionally been achieved using longstanding methods such as off-axis holography (OAH) fast-Fourier transform technique and the transport-of-intensity equation (TIE). The increase in access to processing power alongside the development of advanced algorithms have allowed for phase retrieval of nanoscale magnetic materials with greater efficacy and resolution. Specifically, reverse-mode automatic differentiation (RMAD) and the extended electron ptychography iterative engine (ePIE) are two recent developments of phase retrieval that can be applied to analyzing micro-to-nano- scale magnetic materials. This work evaluates phase retrieval using TIE, RMAD, and ePIE in simulations of Permalloy (Ni 80 Fe 20 ) nanoscale islands, or nanomagnets. Extending beyond simulations, we demonstrate total phase retrieval and image reconstructions of a NiFe nanowire using OAH and RMAD in LTEM and ePIE in Lorentz-mode-4D scanning transmission electron microscopy experiments and determine the saturation magnetization through corroborations with micromagnetic modeling. Finally, we demonstrate the efficacy of these methods in retrieving the total phase and highlight its use in characterizing and analyzing the proximity effect of the magnetic nanostructures.

Lorentz transmission electron microscopy↗

DOE OSTI2024

Synergizing human expertise and AI efficiency with language model for microscopy operation and automated experiment design

With the advent of large language models (LLMs), in both the open source and proprietary domains, attention is turning to how to exploit such artificial intelligence (AI) systems in assisting complex scientific tasks, such as material synthesis, characterization, analysis and discovery. Here, we explore the utility of LLMs, particularly ChatGPT4, in combination with application program interfaces (APIs) in tasks of experimental design, programming workflows, and data analysis in scanning probe microscopy, using both in-house developed APIs and APIs given by a commercial vendor for instrument control. We find that the LLM can be especially useful in converting ideations of experimental workflows to executable code on microscope APIs. Beyond code generation, we find that the GPT4 is capable of analyzing microscopy images in a generic sense. At the same time, we find that GPT4 suffers from an inability to extend beyond basic analyses for more in-depth technical experimental design. We argue that an LLM specifically fine-tuned for individual scientific domains can potentially be a better language interface for converting scientific ideations from human experts to executable workflows. Such a synergy between human expertise and LLM efficiency in experimentation can open new doors for accelerating scientific research, enabling effective experimental protocols sharing in the scientific community.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2024

The 4D Camera: An 87 kHz Direct Electron Detector for Scanning/Transmission Electron Microscopy

We describe the development, operation, and application of the 4D Camera—a 576 by 576 pixel active pixel sensor for scanning/transmission electron microscopy which operates at 87,000 Hz. The detector generates data at ~480 Gbit/s which is captured by dedicated receiver computers with a parallelized software infrastructure that has been implemented to process the resulting 10–700 Gigabyte-sized raw datasets. The back illuminated detector provides the ability to detect single electron events at accelerating voltages from 30 to 300 kV. Through electron counting, the resulting sparse data sets are reduced in size by 10--300× compared to the raw data, and open-source sparsity-based processing algorithms offer rapid data analysis. The high frame rate allows for large and complex scanning diffraction experiments to be accomplished with typical scanning transmission electron microscopy scanning parameters.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

Do We Really Need All That Data: From Data to Agency in Automated Microscopy

Microscopy is entering an era of automated laboratories and AI-enabled instruments, often justified by a simple narrative of automating experiments to collect more data and train better models. In this work, we argue that, for microscopy, this framing is incomplete and can be counterproductive.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2026

Development of In-situ Digital Microscopy Capabilities for Electrochemical Testing

In-situ digital optical microscopy data was successfully collected during the potentiodynamic polarization of iron in corrosive NaCl solution. This report serves as a foundation for future, more comprehensive experiments that correlate electrochemical responses to near-real time surface morphology tracking. The development of in-situ microscopy and roughness collection will help realize increases in data acquisition of the surface morphology during electrochemical experiments.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Multiscale Cryo Electron Microscopy Reveals Interfacial Degradation and Stabilization in Battery Electrodes

Electrochemical interfaces are dynamic systems, evolving based on their local environment and reactant surface structures. The electrode-electrolyte interface in Li-ion batteries can be protective, limiting parasitic reactions with the electrolyte to passivate the surface [1]. Additionally, this interphase has an impact on the Li-ion transport through that layer based on its composition, bonding environment, and thickness. These parameters are challenging to collect and may vary depending on the electrode surface site investigated relative to its spatial position in a coin cell. This study will detail a multiscale cryogenic electron microscopy approach where millimeter-scale cross-sections through the coin cell batteries were made using a cryogenic stage within a fs-laser plasma focused ion beam (laser PFIB) with complementary energy dispersive X-ray spectroscopy able to detect variations in the composition at electrode interfaces [2]. Microscale cross-sectioning and lamella sample preparation of battery electrodes was conducted at the Center for Integrated Nanotechnologies using a Ga-ion focused ion beam (FIB) with air-free and cryo-transfer [3], followed by nanoscale mapping of composition and bonding within the CEI through cryo-scanning transmission electron microscopy (cryo-STEM) electron energy loss spectroscopy [4]. This multiscale approach enabled identification of millimeter-scale features of a battery stack with visualization of degradation in electrodes such as cracks in cathode particles, gas evolution, and SEI evolution; microscale interfacial characteristics, such as heterogeneity in the SEI or barrier layer and identification of electrolyte networks to the electrode surfaces; and nanoscale measurement of the CEI thickness, mapping of transition metal bonding within the cathode particles to identify loss of active materials, and identification of beneficial electrolyte additives incorporated into the CEI structure. This multiscale approach allows for a statistical understanding of the primary mechanisms and parasitic degradation pathways that impact performance by limiting the ion transport pathways within Li+ batteries.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Quantitative Analysis of Rhodobacter sphaeroides Storage Organelles via Cryo-Electron Tomography and Light Microscopy

Bacterial cytoplasmic organelles are diverse and serve many varied purposes. Here, we employed Rhodobacter sphaeroides to investigate the accumulation of carbon and inorganic phosphate in the storage organelles, polyhydroxybutyrate (PHB) and polyphosphate (PP), respectively. Using cryo-electron tomography (cryo-ET), these organelles were observed to increase in size and abundance when growth was arrested by chloramphenicol treatment. The accumulation of PHB and PP was quantified from three-dimensional (3D) segmentations in cryo-tomograms and the analysis of these 3D models. The quantification of PHB using both segmentation analysis and liquid chromatography and mass spectrometry (LCMS) each demonstrated an over 10- to 20-fold accumulation of PHB. The cytoplasmic location of PHB in cells was assessed with fluorescence light microscopy using a PhaP-mNeonGreen fusion-protein construct. The subcellular location and enumeration of these organelles were correlated by comparing the cryo-ET and fluorescence microscopy data. A potential link between PHB and PP localization and possible explanations for co-localization are discussed. Finally, the study of PHB and PP granules, and their accumulation, is discussed in the context of advancing fundamental knowledge about bacterial stress response, the study of renewable sources of bioplastics, and highly energetic compounds.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

X-ray Fluorescence Microscopy to Develop Elemental Classifiers and Investigate Elemental Signatures in BALB/c Mouse Intestine a Week after Exposure to 8 Gy of Gamma Rays

Iron redistribution in the intestine after total body irradiation is an established phenomenon. However, in the literature, there are no reports about the use of X-ray fluorescence microscopy or equivalent techniques to generate semi-quantitative 2D maps of iron in sectioned intestine samples from irradiated mice. In this work, we used X-ray fluorescence microscopy (XFM) to map the elemental content of iron as well as phosphorus, sulfur, calcium, copper and zinc in tissue sections of the small intestine from eight-week-old BALB/c male mice that developed gastrointestinal acute radiation syndrome (GI-ARS) in response to exposure to 8 Gray of gamma rays. Seven days after irradiation, we found that the majority of the iron is localized as hot spots in the intercellular regions of the area surrounding crypts and stretching between the outer perimeter of the intestine and the surface cell layer of villi. In addition, this study represents our current efforts to develop elemental cell classifiers that could be used for the automated generation of regions of interest for analyses of X-ray fluorescence maps. Once developed, such a tool will be instrumental for studies of effects of radiation and other toxicants on the elemental content in cells and tissues. While XFM studies cannot be conducted on living organisms, it is possible to envision future scenarios where XFM imaging of single cells sloughed from the human (or rodent) intestine could be used to follow up on the progression of GI-ARS.

X-ray fluorescence microscopy↗

NASA NTRS1996

Free-living spirochetes from Cape Cod microbial mats detected by electron microscopy

Spirochetes from microbial mats and anaerobic mud samples collected in salt marshes were studied by light microscopy, whole mount and thin section transmission electron microscopy. Enriched in cellobiose-rifampin medium, selective for Spirochaeta bajacaliforniensis, seven distinguishable spirochete morphotypes were observed. Their diameters ranged from 0.17 micron to > 0.45 micron. Six of these morphotypes came from southwest Cape Cod, Massachusetts: five from Microcoleus-dominated mat samples collected at Sippewissett salt marsh and one from anoxic mud collected at School Street salt marsh (on the east side of Eel Pond). The seventh morphotype was enriched from anoxic mud sampled from the north central Cape Cod, at the Sandy Neck salt marsh. Five of these morphotypes are similar or identical to previously described spirochetes (Leptospira, Spirochaeta halophila, Spirochaeta bajacaliforniensis, Spirosymplokos deltaeiberi and Treponema), whereas the other two have unique features that suggest they have not been previously described. One of the morphotypes resembles Spirosymplokos deltaeiberi (the largest free-living spirochete described), in its large variable diameter (0.4-3.0 microns), cytoplasmic granules, and spherical (round) bodies with composite structure. This resemblance permits its tentative identification as a Sippewissett strain of Spirosymplokos deltaeiberi. Microbial mats samples collected in sterile Petri dishes and stored dry for more than four years yielded many organisms upon rewetting, including small unidentified spirochetes in at least 4 out of 100 enrichments.

NASA Program Exobiology↗

NASA NTRS1992

Effects of spaceflight in the adductor longus muscle of rats flown in the Soviet Biosatellite COSMOS 2044. A study employing neural cell adhesion molecule (N-CAM) immunocytochemistry and conventional morphological techniques (light and electron microscopy)

The effects of spaceflight upon the "slow" muscle adductor longus were examined in rats flown in the Soviet Biosatellite COSMOS 2044. The techniques employed included standard methods for light microscopy, neural cell adhesion molecule (N-CAM) immunocytochemistry and electron microscopy. Light microscopic observations revealed myofiber atrophy and segmental necrosis accompanied by cellular infiltrates composed of macrophages, leukocytes and mononuclear cells. Neural cell adhesion molecule immunoreactivity (N-CAM-IR) was seen on the myofiber surface and in regenerating myofibers. Ultrastructural alterations included Z band streaming, disorganization of myofibrillar architecture, sarcoplasmic degradation, extensive segmental necrosis with apparent preservation of the basement membrane, degenerative phenomena of the capillary endothelium and cellular invasion of necrotic areas. Regenerating myofibers were identified by the presence of increased amounts of ribosomal aggregates and chains of polyribosomes associated with myofilaments. The principal electron microscopic changes of the neuromuscular junctions showed axon terminals with a decrease or absence of synaptic vesicles replaced by microtubules and neurofilaments, degeneration of axon terminals, vacant axonal spaces and changes suggestive of axonal sprouting. The present observations suggest that alterations such as myofibrillar disruption and necrosis, muscle regeneration and denervation and synaptic remodeling at the level of the neuromuscular junction may take place during spaceflight.

NASA Experiment Number COS 2044-10↗

NASA NTRS2005

Three-dimensional characterization of tethered microspheres by total internal reflection fluorescence microscopy

Tethered particle microscopy is a powerful tool to study the dynamics of DNA molecules and DNA-protein complexes in single-molecule experiments. We demonstrate that stroboscopic total internal reflection microscopy can be used to characterize the three-dimensional spatiotemporal motion of DNA-tethered particles. By calculating characteristic measures such as symmetry and time constants of the motion, well-formed tethers can be distinguished from defective ones for which the motion is dominated by aberrant surface effects. This improves the reliability of measurements on tether dynamics. For instance, in observations of protein-mediated DNA looping, loop formation is distinguished from adsorption and other nonspecific events.

Non-NASA Center↗

DOE OSTI2024

Advances in Spectro‐Microscopy Methods and their Applications in the Characterization of Perovskite Materials

Perovskite materials are promising contenders as the active layer in light-harvesting and light-emitting applications if their long-term stability can be sufficiently increased. Chemical and structural engineering are shown to enhance long-term stability, but the increased complexity of the material system also leads to inhomogeneous functional properties across various length scales. Thus, scanning probe and high-resolution microscopy characterization techniques are needed to reveal the role of local defects and the results promise to act as the foundation for future device improvements. Here, a look at the parameter space: technique-specific sample penetration depth versus probe size highlights a gap in current methods. High spatial resolution combined with a deep penetration depth is not yet achievable. However, multimodal measurement technique may be the key to covering this parameter space. In this perspective, current advanced spectro-microscopy methods which have been applied to perovskite materials are highlighted.

Luo, Yanqi↗

DOE OSTI2025

Informed unsupervised machine learning analysis of dislocation microstructure from high-resolution differential aperture X-ray structural microscopy data

This study leverages high-resolution differential-aperture X-ray structural microscopy (DAXM) to probe the local dislocation structure in deformed 304L-stainless steel at small strain, by measuring the lattice rotation and deviatoric elastic strain with a sub-micron resolution. For a single grain in a polycrystalline specimen, the measured lattice rotation field over the measured volume exhibited a multimodal distribution while the deviatoric elastic strain showed a single-mode distribution. An unsupervised Cauchy mixture machine learning model was developed to resolve the multimodal distribution of the lattice rotation. By mapping the lattice rotation data associated with each Cauchy peak in the model back onto the measured volume, we identify contiguous regions of the crystal rotated near the average values corresponding to the peaks of the overall rotation distribution. These regions represent the grain subdivision in the microstructure. Finally, the dislocation density tensor was also computed and its norm was laid over the rotation field to detect the subgrain boundaries. This step provided a validation of the Cauchy mixture model for the analysis of the lattice rotation distribution. The current study highlights the integration of advanced X-ray microscopy techniques with data-driven analysis methods to uncover detailed microstructure scales in deformed crystals.

Machine learning; Lattice rotation; High-energy X-↗

DOE OSTI2026

Visualization of the surface distribution of photocatalytic activity at the anatase/rutile TiO2 interface using X-ray photoelectron emission microscopy

We applied X-ray photoelectron emission microscopy (XPEEM) to visualize the surface distribution of photocatalytic activity at the anatase/rutile (A/R) interface of titanium dioxide. Acetic acid was adsorbed on the surface, and its decomposition and desorption reactions under ultraviolet light irradiation were monitored by observing C 1s spectra, enabling direct observation of the spatial distribution of photocatalytic activity. Complementary crystal structure information was obtained using spatially resolved low-energy electron diffraction, low-energy electron microscopy, X-ray absorption spectroscopy, and micro-focused Raman spectroscopy. Comparison with these structural data allowed for the evaluation of the photocatalytic activity as a function of the distance from the A/R interface. The activity is enhanced in the vicinity of the interface and gradually decreases toward both the anatase and rutile regions. These results demonstrate that XPEEM is an effective technique for spatially resolved mapping of photocatalytic activity, which has\\r\\npreviously been inaccessible using conventional characterization techniques.

25 ENERGY STORAGE↗

DOE OSTI2026

Elucidating microstructural evolution and hardness variation across friction self-piercing riveted Al-7055 using synchrotron X-ray scattering and advanced microscopy techniques

Friction self-piercing riveting (FSPR) is a unique hybrid joining technique that combines the advantages of mechanical interlocking, frictional heat, and solid-state joining (if metallurgically compatible) to produce crack free joints in high strength and/or low-ductility alloys at room temperature. Here, in the current study, Al-7055 sheets were joined using FSPR for lightweight automotive applications and significant microhardness variations were observed across the joint cross-section. A detailed microstructural characterization at multiple length scales was carried out using advanced electron microscopy and X-ray scattering techniques to provide a fundamental understanding of the process-structure-property relationships. The relative contributions of microstructural characteristics at various length scales (i.e., grain size, dislocation density, solute concentration, precipitate nature) to strengthening were estimated using existent formulations (i.e., Hall-Petch, Taylor, precipitate bypass/shear equations) and correlated to the observed microhardness values across different regions. Small-angle X-ray scattering and scanning transmission electron microscopy revealed significant changes in the size and volume fraction of precipitate species, i.e., GP-I Zones, η′, and Mg/Zn solute co-clusters, depending on the process region. It was observed that the dissolution of the small η′/GP-I zones (T ∼ 150–200 °C) in the heat-affected zone were the key reason for the hardness drop. Further, it was shown that solid-solution, dislocation, grain size and solute co-cluster strengthening played a key role in the thermo-mechanically affected zone and grain-refined zone (GRZ). Finally, these observations were leveraged along with the Zener-Holloman relationship and grain size in the GRZ to estimate the peak joining temperature of the GRZ (∼ 350 °C) near the steel rivet.

aluminum 7xxx alloy↗