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At least 1,423 records · Page 79

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NASA NTRS1992

Tensile strain measurements of ceramic fibers using scanning laser acoustic microscopy

A noncontacting technique using scanning laser acoustic microscopy for making in situ tensile strain measurements of small diameter fibers was implemented for the tensile strain analysis of individual Nicalon SiC fibers (nominal diameter 15 microns). Stress vs strain curves for the fibers were plotted from the experimental data. The mean elastic modulus of the fibers was determined to be 185.3 GPa. Similar measurements were made for Carborundum SiC fibers (nominal diameter 28 microns) and Saphikon sapphire fibers (nominal diameter 140 microns).

Kent, Renee M.↗

NASA NTRS1992

Sudbury project (University of Muenster-Ontario Geological Survey): Petrology, chemistry, and origin of breccia formations

Within the Sudbury Project of the University of Muenster and the Ontario Geological Survey special emphasis was put on the breccia formations exposed at the Sudbury structure (SS) because of their crucial role for the impact hypothesis. They were mapped and sampled in selected areas of the north, east, and south ranges of the SS. The relative stratigraphic positions of these units are summarized. Selected samples were analyzed by optical microscopy, SEM, microprobe, XRF and INAA, Rb-Sr and SM-Nd-isotope geochemistry, and carbon isotope analysis. The results of petrographic and chemical analysis for those stratigraphic units that were considered the main structural elements of a large impact basin are summarized.

Stoeffler, D.↗

NASA NTRS1994

Application of an alkylammonium method for characterization of phyllosilicates in CI chondrites

Many meteorites and interplanetary dust particles (IDP's) with primitive compositions contain significant amounts of phyllosilicates, which are generally interpreted as evidence of protoplanetary aqueous alteration at an early period in the solar system. These meteorites are chondrites of the carbonaceous and ordinary varieties. Characterization of phyllosilicates in these materials is important because of the important physico-chemical information they hold, e.g., from well characterized phyllosilicates, thermodynamic stability relations and hence the conditions of formation of phyllosilicates in the parent body of the meteorite can be predicted. Although we are at a rudimentary level of understanding of the minerals resulting from the aqueous alteration in the early solar nebula, we know that the most common phyllosilicates present in chondritic extraterrestrial materials are serpentines, smectites, chlorites, and micas. The characterization of fine grained minerals in meteorites and IDP's rely heavily on electron beam instruments, especially transmission electron microscopy (TEM). Typically, phyllosilicates are identified by a combination of high resolution imaging of basal spacings, electron diffraction analysis, and chemical analysis. Smectites can be difficult to differentiate from micas because the smectites loose their interlayer water and the interlayers collapse to the same basal spacing as mica in the high vacuum of the TEM. In high-resolution TEM (HRTEM) images, smectite basal spacings vary from 1 nm up to 1.5 nm, while micas show 1 or 2 nm basal spacings. Not only is it difficult to differentiate smectites from micas, but there is no way of identifying different classes of smectites in meteorites and IDP's. To differentiate smectites from micas and also to recognize the charge differences among smectites, an alkylammonium method can be employed because the basal spacings of alkylammonium saturated smectites expand as a function of alkylamine chain length and the layer-charge density of the 2:1 expanding phyllosilicate, and the final product is significantly more stable under electron beam examination. Such a method was tested on standard clays and several meteorite samples using four alkylammonium salts.

Golden, D. C.↗

NASA NTRS2001

The Role of Bearing and Scan Mechanism Life Testing in Flight Qualification of the MODIS Instrument

This paper describes the results of accelerated and operational life tests on bearings for the Moderate Resolution Imaging Spectroradiometer (MODIS). It also describes the post test analysis of the disassembled bearings. Analysis was performed using micro-Raman, micro-FTIR, X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Size Exclusion Chromatography (SEC). In general, the three sets of bearings in each of three test stations were in very good condition after accumulating 68, 144, and 209 million cycles, respectively. Some of the bearings exhibited lubricant degradation, indicated by viscous lubricant deposits on the cage and raceways.

VanDyk, Steven G.↗

NASA NTRS2003

A Gravity-Responsive Time-Keeping Protein of the Plant and Animal Cell Surface

The hypothesis under investigation was that a ubiquinol (NADH) oxidase protein of the cell surface with protein disulfide-thiol interchange activity (= NOX protein) is a plant and animal time-keeping ultradian (period of less than 24 h) driver of both cell enlargement and the biological clock that responds to gravity. Despite considerable work in a large number of laboratories spanning several decades, this is, to my knowledge, our work is the first demonstration of a time-keeping biochemical reaction that is both gravity-responsive and growth-related and that has been shown to determine circadian periodicity. As such, the NOX protein may represent both the long-sought biological gravity receptor and the core oscillator of the cellular biological clock. Completed studies have resulted in 12 publications and two issued NASA-owned patents of the clock activity. The gravity response and autoentrainment were characterized in cultured mammalian cells and in two plant systems together with entrainment by light and small molecules (melatonin). The molecular basis of the oscillatory behavior was investigated using spectroscopic methods (Fourier transform infrared and circular dichroism) and high resolution electron microscopy. We have also applied these findings to an understanding of the response to hypergravity. Statistical methods for analysis of time series phenomena were developed (Foster et al., 2003).

Morre, D. James↗

DOE OSTI2023

Focused Interest Groups Propel Innovation in the Emerging Data-Driven Hardware Ecosystem

Over the past several decades, the science of electron microscopy (EM) has risen to become one of the cornerstone approaches to understanding material structure, chemistry, and defects at exceptional spatial resolution. This rise can be attributed to the hard work of researchers and companies who have pushed the bounds of instrumentation and analysis, but it is also the result of advocacy by members of professional societies. Furthermore, such advocacy is exemplified by the Aberration Corrected EM (ACEM) focused interest group (FIG) of the Microscopy Society of America (MSA), which has played an important role in facilitating new hardware developments, promoting the exchange of ideas to catalyze discovery, and building the next generation of leaders in electron microscopy. From the early 2000s to the present, aberration correction has moved from proof-of-concept instrumentation to an established technique, providing unprecedented improvements in spatial and chemical resolution for breakthroughs in chemistry, physics, and materials science.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

Illuminating the Material World: Autonomous Microscopy to Understand Order, Disorder, and Everything In Between

Artificial intelligence (AI) holds immense promise for revolutionizing microscopy, yet its widespread adoption has been hindered by challenges ranging from user inexperience to limited model transferability and difficulties in operationalizing machine learning. This presentation showcases our approach to developing practical autonomy for materials discovery, aiming to accelerate the integration of AI into everyday microscopy workflows. As shown in Fig. 1, I will focus on three key areas: understanding order-disorder transitions, quantifying point defects, and achieving truly device-scale microscopy. First, I will demonstrate the power of multi-modal knowledge graphs for integrating diverse microscopy data. By combining imaging, spectroscopy, and diffraction data, these graphs provide a holistic view of material behavior, capturing the intricate relationships between different modalities [1,2]. I will present a case study on how these models illuminate the structural and chemical changes associated with irradiation in oxide thin films, revealing critical insights for designing materials for extreme environments like spaceflight and nuclear energy. Specifically, I will show how multi-modal analysis clarifies the evolution of order-disorder transitions under irradiation, a key factor influencing material performance in these applications. Next, I will address the challenge of quantifying point defects in 2D materials. We demonstrate the application of computer vision and transfer learning to accurately identify and classify various defect types, such as vacancies and substitutional atoms, and to quantify their concentrations. This information is crucial for understanding and tailoring the properties of 2D materials for applications in electronics, optoelectronics, and catalysis. For example, I will show how our models can characterize the topological distribution of point defects in MXene transition metal carbides, providing valuable insights for optimizing their performance in energy storage and separation science. Finally, I will discuss our progress toward autonomous device-scale microscopy [3,4]. We are fundamentally redesigning electron microscopes around the principles of machine reasoning, enabling automation beyond basic tasks like sample navigation and data acquisition to include sophisticated experimental design. This approach paves the way for truly reproducible and massively scaled analysis campaigns. I will emphasize the importance of autonomous microscopy platforms for high-throughput materials discovery and characterization, facilitating the rapid screening of materials for a broad range of applications and accelerating the development of next-generation technologies.

36 MATERIALS SCIENCE↗

NASA NTRS1997

Stereological analysis of gravitropism in protonemata of the moss Ceratodon

Apical cells of dark-grown protonemata of the moss Cerotodon purpureus are negatively gravitropic. Previous light microscopy has shown that reorientation to the horizontal induces amyloplast sedimentation and redistribution of microtubules. To determine whether other components become redistributed laterally or axially, the apical 35 micrometers of both vertical and horizontal apical cells were compared stereologically using transmission electron microscopy. Reorientation to the horizontal changed the longitudinal distributions of tubular ER, Golgi stacks, and vesicles but not cisternal ER, mitochondria, and plastids. Only plastids showed a statistically significant lateral redistribution after horizontal placement. Qualitative examination of the sedimentation zone showed plastids sedimented close to peripherally located ER with vacuoles displaced above plastids. These results argue against a model where differential tip growth results from a redistribution of Golgi stacks or exocytic vesicles.

Non-NASA Center↗

DOE OSTI2025

Nanometer Resolution Structure‐Emission Correlation of Individual Quantum Emitters via Enhanced Cathodoluminescence in Twisted Hexagonal Boron Nitride

Understanding the atomic structure of quantum emitters, often originating from point defects or impuritie, is essential for designing and optimizing materials for quantum technologies such as quantum computing, communication, and sensing. Despite the availability of atomic-resolution scanning transmission electron microscopy and nanoscale cathodoluminescence microscopy, experimentally determining the atomic structure of individual emitters is challenging due to the conflicting needs for thick samples to generate strong cathodoluminescence signals and thin samples for structural analysis. To overcome this challenge, significantly enhanced cathodoluminescence at twisted interfaces is leveraged to achieve sub-nanometer localization precision for the first time in mapping individual quantum emitters in carbon-implanted hexagonal boron nitride. This unprecedent spatial sensitivity, together with correlative electron energy loss spectroscopy quantitative scanning transmission electron microscopy imaging, and first principles density functional theory calculations, enables the identification of the atomic structure of the 440 nm blue emitter in hexagonal boron nitride as a substituted vertical carbon dimer. Building on the atomic structure insights, nanoscale spatially precise creation of blue emitters is demonstrated by electron beam irradiation of carbon-coated hexagonal boron nitride. This advancement in correlating atomic structures with optical properties lays the foundation for a deeper understanding and precise engineering of quantum emitters, significantly advancing the development of cutting-edge quantum information technologies.

2D material↗

DOE OSTI2022

Magnetic resonance force microscopy with matching frequencies of cantilever and spin

We have studied theoretically magnetic resonance force microscopy with a high-frequency nanomechanical cantilever when the cantilever frequency matches the resonant frequency of a single electron spin. Our analysis shows that in this situation, there is a small probability that the cantilever will oscillate with a large frequency shift. In conclusion, this can open new experimental opportunities for increasing the sensitivity in the detection of a single electron spin or even a single nuclear spin by using a high-frequency cantilever.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2020

Nanomechanical sampling of material for nanoscale mass spectrometry chemical analysis

The ability to spatially resolve the chemical distribution of compounds on a surface is important in many applications ranging from biological to material science. To this extent, we have recently introduced a hybrid atomic force microscopy (AFM)-mass spectrometry (MS) system for direct thermal desorption and pyrolysis of material with nanoscale chemical resolution. However, spatially resolved direct surface heating using local thermal desorption becomes challenging on material surfaces with low melting points, because the material will undergo a melting phase transition due to heat dissipation prior to onset of thermal desorption. Therefore, here we developed an approach using mechanical sampling and collection of surface materials on an AFM cantilever probe tip for real-time analysis directly from the AFM tip. This approach allows for material to be concentrated directly onto the probe for subsequent MS analysis. We evaluate the performance metrics of the technique and demonstrate localized MS sampling from a candelilla wax matrix containing UV stabilizers avobenzone and oxinoxate from areas down to 250 nm × 250 nm. Overall, this approach removes heat dissipation into the bulk material allowing for a faster desorption and concentration of the gas phase analyte from a single heating pulse enabling higher signal levels from a given amount of material in a single sampling spot.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Correlated 4D-STEM and EDS for the classification of fine Beta-precipitates in aluminum alloy AA 6063-T6

Tuning the properties of aluminum alloys AA 6063-T6 involves artificial aging to induce precipitate formation, particularly β’’ and β’ phases. Previous characterization challenges due to their similar appearance are addressed here by correlating 4D scanning transmission electron microscopy (4DSTEM) and energy-dispersive spectroscopy (EDS) mapping. This approach allows us to analyze the structure and composition of precipitates individually, overcoming limitations of conventional imaging and structural analysis techniques when the precipitates appear simultaneously, as is often the case. We present detailed characterizations of needle-shaped Beta precipitates, revealing distinct diffraction patterns (DPs) and compositional differences. The method's applicability extends beyond aluminum alloys, offering a promising strategy for complex composite material characterization with multimodal scanning transmission electron microscopy (STEM) techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Paramagnetic Mn 8 Fe 4 -co-Polystyrene Nanobeads as a Potential T 1 –T 2 Multimodal Magnetic Resonance Imaging Contrast Agent with In Vivo Studies

In developing a cluster-nanocarrier design, as a magnetic resonance imaging contrast agent, we have investigated the enhanced relaxivity of a manganese and iron-oxo cluster grafted within a porous polystyrene nanobead with increased relaxivity due to a higher surface area. The synthesis of the cluster-nanocarrier for the cluster Mn 8 Fe 4 O 12 (O 2 CC 6 H 4 CH=CH 2 ) 16 (H 2 O) 4 , cross-linked with polystyrene (the nano-carrier), under miniemulsion conditions is described. By including a branched hydrophobe, iso-octane, the resulting nanobeads are porous and similar to 70 nm in diameter. The increased surface area of the nanobeads compared to nonporous nanobeads leads to an enhancement in relaxivity; r 1 increases from 3.8 to 5.2 ± 0.1 mM -1 s -1 , and r 2 increases from 11.9 to 50.1 ± 4.8 mM -1 s -1 , at 9.4 teslas, strengthening the potential for T 1 and T 2 imaging. Several metrics were used to assess stability, and the porosity produced no reduction in metal stability. Synchrotron X-ray fluorescence microscopy was used to demonstrate that the nanobeads remain intact in vivo . In depth, physicochemical characteristics were determined, including extensive pharmacokinetics, in vivo imaging, and systemic biodistribution analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

A Review and Perspective on Cathodoluminescence Analysis of Halide Perovskites

Halide perovskite solar cells have achieved a certified efficiency of 25.2%, surpassing CdTe and CuInGaSe 2 , which have long been regarded as the most-efficient thin-film photovoltaic materials. As this exciting class of materials continues to mature, researchers will require characterization techniques capable of exposing the interplay among structure, chemistry, and optoelectronic properties to inform processing strategies and increase both device efficiencies and long-term stability. Cathodoluminescence microscopy is an ideal technique to provide such information due to the high spatial resolution and robust optical information acquired. Here, the current body of work related to cathodoluminescence analysis of halide perovskite materials for optoelectronic applications is surveyed. This review demonstrates how cathodoluminescence can monitor degradation due to environmental stressors, phase segregation resulting from material processing, and other halide perovskite-centric material issues. A persistent concern associated with e-beam-based analysis of halide perovskites is what effect the electron beam has on the material properties being probed. Addressing this, a detailed discussion is provided on the origin of the cathodoluminescence signal and a review of studies focused on revealing changes in the properties of halide perovskites resulting from e-beam excitation. Finally, a perspective on future opportunities to expand the role of cathodoluminescence analysis for halide perovskites is provided.

14 SOLAR ENERGY↗

DOE OSTI2020

Cathode Electrolyte Diagnostics Based on Scanning Probe Microscopy

Various processes lead to degradation of cathodes in lithium-ion batteries. Questions remain regarding mechanisms of many of these processes. Probe microscopy methods including scanning electrochemical microscopy (SECM) are capable of directly probing processes at the cathode/electrolyte interface. SECM uses a small electrode to perform rapid electrochemical analysis of transient species generated at an active cathode/electrolyte interface. This paper discusses the background of the SECM instrument and its application to lithium-ion battery research. We also describe the application of SECM methods to the study of cathode degradation processes observed in lithium-ion batteries. Specifically, we focus on characterizing the dissolution of manganese from LiMn2O4 (LMO) based on recent debate in the literature. We describe experiments to observe and characterize the electrochemical properties of manganese complexes emerging from degrading LMO electrode materials.

cathode/electrolyte interface↗

DOE OSTI2025

Ultralow-temperature cryogenic transmission electron microscopy using a new helium flow cryostat stage

Advances in cryogenic electron microscopy have opened new avenues for probing quantum phenomena in correlated materials. This study reports the installation and performance of a new side-entry condenZero cryogenic cooling system for JEOL (Scanning) Transmission Electron Microscopes (S/TEM), utilizing compressed liquid helium (LHe) and designed for imaging and spectroscopy at ultra-low temperatures. The system includes an external dewar mounted on a vibration-damping stage and a pressurized, low-noise helium transfer line with a remotely controllable needle valve, ensuring stable and efficient LHe flow with minimal thermal and mechanical noise. Performance evaluation demonstrates a stable base temperature of 4.37 K measured using a Cernox bare chip sensor on the holder with temperature fluctuations within ±0.004 K. Complementary in-situ electron energy-loss spectroscopy (EELS) via aluminum bulk plasmon analysis was used to measure the local specimen temperature and validate cryogenic operation during experiments. The integration of cryogenic cooling with other microscopy techniques, including electron diffraction and Lorentz TEM, was demonstrated by resolving charge density wave (CDW) transitions in NbSe2 using electron diffraction, and imaging nanometric magnetic skyrmions in MnSi via Lorentz TEM. In conclusion, this platform provides reliable cryogenic operation below 7 K, establishing a low-drift route for direct visualization of electronic and magnetic phase transformations in quantum materials.

Charge density wave↗

NASA NTRSDate not supplied

Carbon Tracers of Aqueous Processes: Isotopic Analysis of Cr Carbonate Grains With Implications for Bennu Samples

Carbonate grains in carbonaceous chondrites record aqueous alteration events on the asteroidal parent bodies, including evidence for episodic alteration, timing of alteration, and time and temperature evolution of volatiles. Spectral features in the 3.4 μm region at asteroid Bennu have been interpreted as coming from carbonate minerals. Coordinated analysis of carbonate grains will be a valuable tool for analysis of Bennu samples, and related analysis of analog materials provides important context for understanding aqueous alteration of carbonaceous asteroids more broadly. To that end, our team is analyzing carbonates in Bennu analog materials, using Raman spectroscopy to identify carbonates and assess the maturity of related organic materials, vacuum reflectance spectroscopy from the ultraviolet through thermal infrared range to constrain contributions from carbonates and organics, X-ray microtomography and electron probe microanalysis (EPMA) to assess the distribution of void space, transmission electron microscopy to characterize space weathering effects, and EPMA and secondary ion mass spectrometry (SIMS) to measure composition and isotopic ratios. Here, we describe in situ analysis of carbon and oxygen isotopes from carbonates in Grosvenor Mountains (GRO) 95577.

K E Miller↗

DOE OSTI2023

Coso Geothermal Spectral Library for Rocks and Minerals

An integrated open mineral spectral library designed to enhance the utility and precision of mineral spectral data for geothermal exploration, developed from a reliable and comprehensive digital dataset for seamless sharing by integrating field data, the USGS spectral library, and pertinent information obtained from Coso geothermal field (Coso) in California. The ASD FieldSpec portable spectrometer was utilized for collecting spectral data, which was subsequently analyzed using the THOR Material Identification tool in ENVI, The Spectral Geologist (TSG) software by CSIRO, and the Fully Constrained Linear Spectral Unmixing algorithm (FCLSU) in MATLAB. Scanning Electron Microscopy (SEM) with a mineralogy-analyzing function was employed to assess the mineral composition of samples, ensuring precise mineralogical analysis. A portable X-ray fluorescence (pXRF) spectrometer was also utilized to gather information on elemental enrichment. A framework for developing spectra data and establishing spectral libraries for various geological cases was proposed within this study. The characteristic spectra of six alteration minerals - alunite, chalcedony, epidote, hematite, kaolinite, and opal - were acquired from Coso samples. The spectral library for the Coso alteration minerals was introduced for further application in academic study or industrial exploration. To browse the Coso Geothermal Spectral data and related figures from spreadsheets: #1 Unzip and store the following items in the same folder. 'Contact Probe Data.zip', 'Sample Photos.zip', and 'Coso spectra of higher-certainity minerals.xlsx'. #2 Open 'Coso spectra of higher-certainity minerals.xlsx'. The hyperlinks in the spreadsheet lead to the folders or figures of: spectra .asd file, spectra ASC II file, spectra plots, and sample photos. The spectra data is raw data without splice correction. Spectra .asd files require particular software to open. (These cannot be opened in GIS software such as ArcGIS.) Spectra ASC II files can be opened in a text editor or spread sheet program.

15 GEOTHERMAL ENERGY↗