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At least 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

In Situ Liquid Electron Microscope Cells Strongly Attenuate Electrochemical Behavior

In situ electrochemical Scanning Transmission Electron Microscopy (ec-S/TEM) probes the dynamics of electrochemical processes in real time and at high spatial resolution. This method utilizes microfabricated electrochemical cells, with enclosed dimensions of 800 μm wide, 800 μm long, and 1–2 μm tall, with electron-transparent silicon nitride windows. Working, counter, and reference electrodes in the configuration studied are deposited Pt with a planar surface area of about 1 μm 2 and a height of 50 nm. The cell confines the electrolyte within a 1 μm tall channel, and the microfabricated electrodes have a non-standard geometry, are coplanar, and are not front-facing. As such, standard assumptions of electrochemical experiments do not apply. COMSOL modeling was used to compare and contrast differences in electrochemical behavior between conventional experimental setups and the in situ ec-S/TEM cells. Cell height strongly affected voltammogram measurements: peak magnitudes and shifts correlate directly to cell height. Reactant concentration above the electrode quickly decreases during deposition, leading to a planar diffusion-dominated regime. The concentration gradient prioritizes particle growth along the thin edges of the electrode and not on the planar part of the electrode. Experiments done in the ec-S/TEM ex situ of a TEM verify the model’s accuracy.

Wittman, Reed M. [Oak Ridge National Laboratory (O↗
NASA NTRS1969

Flexible high-voltage supply for experimental electron microscope

Scanning microscope uses a field-emission tip for the electron source, an electron gun that simultaneously accelerates and focuses electrons from the source, and one auxiliary lens to produce a final probe size at the specimen on the order of angstroms.

Chapman, G. L.↗
NASA NTRS1980

The determination of transport parameters of minority carriers in n-p junctions by means of an electron microscope - Critique of recent developments

It has recently been shown that amplitude modulated electron beams provide a novel means for the determination of minority carrier lifetimes, diffusion lengths, etc., in n-p junctions. In this paper it is shown that: (1) a recently published analysis based on a cylindrically symmetric configuration is incorrect, (2) the correct approach leads to a system of dual integral equations for which the formal solution is given, (3) in general, the short circuit current can only be determined by means of extensive computer calculations except in the case of large front surface recombination velocities, and (4) the difficulties encountered with cylindrically symmetric configurations (circular ohmic contacts and the like) are completely avoided with a choice of a planar geometry since simple closed form expressions for the short circuit current are readily available in this case.

Von Roos, O.↗
NASA NTRS1992

X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be the development of new spectrometers and improvements in thin specimen preparation. The microanalysis technique needs to be simplified and software developed so that the EELS technique approaches the relative simplicity of the X-ray technique. Finally, one can expect major improvements in EELS imaging as data storage and processing improvements occur.

Goldstein, J. I.↗
NASA NTRS1998

Production of otoconia in the endolymphatic sac in the Japanese red-bellied newt, Cynops pyrrhogaster: light and transmission electron microscopic study

The formation of otoconia in the endolymphatic sac (ES) of the larval newt, Cynops pyrrhogaster, has been studied by light and transmission electron microscopy. Some of the epithelial cells of the ES contain an abundance of swollen vesicles, Golgi complexes, rough endoplasmic reticula and ribosomes at the late larval stages 50 and 51, approximately 26-30 days after eggs are laid. Five days later, at stage 52, crystals are present in the vacuoles between the epithelial cells. Serial sections indicate that these vacuoles actually form small canals which lie in the wall and join the lumen of the ES. Reconstruction of the ES shows that several canals are contained in the ES wall. At stage 56, about 72 days after eggs are laid, a large number of otoconia are present in the ES lumen, while the otoconia disappear from the canals. It appears that the otoconia are first produced in the canals and then released to the lumen. Some epithelial cells of the ES are thought to expel the organic and inorganic material to the canals to form the otoconia in situ. The process of formation of the otoconia in the ES is discussed.

Non-NASA Center↗
DOE OSTI2020

High-resolution analogue of time-domain phonon spectroscopy in the transmission electron microscope

Femtosecond photoexcitation of semiconducting materials leads to the generation of coherent acoustic phonons (CAPs), the behaviours of which are linked to intrinsic and engineered electronic, optical and structural properties. While often studied with pump-probe spectroscopic techniques, the influence of nanoscale structure and morphology on CAP dynamics can be challenging to resolve with these all-optical methods. Here, we used ultrafast electron microscopy (UEM) to resolve variations in CAP dynamics caused by differences in the degree of crystallinity in as-prepared and annealed GaAs lamellae. Following in situ femtosecond photoexcitation, we directly imaged the generation and propagation dynamics of hypersonic CAPs in a mostly amorphous and, following an in situ photothermal anneal, a mostly crystalline lamella. Subtle differences in both the initial hypersonic velocities and the asymptotic relaxation behaviours were resolved via construction of space-time contour plots from phonon wavefronts. Comparison to bulk sound velocities in crystalline and amorphous GaAs reveals the influence of the mixed amorphous-crystalline morphology on CAP dispersion behaviours. Further, an increase in the asymptotic velocity following annealing establishes the sensitivity of quantitative UEM imaging to both structural and compositional variations through differences in bonding and elasticity. Lastly, implications of extending the methods and results reported here to elucidating correlated electronic, optical and structural behaviours in semiconducting materials are discussed.

42 ENGINEERING↗
NASA NTRS1992

Combined infrared and analytical electron microscope studies of interplanetary dust particles

Ultramicrotomed thin sections (less than 100 nm thick) of eight chondritic interplanetary dust particles (IDPs) were studied by analytical electron microscopy and IR microspectroscopy with the objective of identifying IDPs or their specific components with IR spectral transmission characteristics at 10 microns similar to those of comets. Two IDPs are identified whose silicate emission characteristics between 8 and 12 microns are similar to those of comets Halley and Bradfield. Implanted solar flare tracks and sputtered rims resulting from solar wind damage suggest that the minerology and petrography of these IDPs have not been significantly perturbed since ejection from their parent bodies.

Bradley, J. P.↗
DOE OSTI2021

Possibility of an integrated transmission electron microscope: enabling complex in-situ experiments

Abstract Multimodal in-situ experiments are the wave of the future, as this approach will permit multispectral data collection and analysis during real-time nanoscale observation. In contrast, the evolution of technique development in the electron microscopy field has generally trended toward specialization and subsequent bifurcation into more and more niche instruments, creating a challenge for reintegration and backward compatibility for in-situ experiments on state-of-the-art microscopes. We do not believe this to be a requirement in the field; therefore, we propose an adaptive instrument that is designed to allow nearly simultaneous collection of data from aberration-corrected transmission electron microscopy (TEM), probe-corrected scanning transmission electron microscopy, ultrafast TEM, and dynamic TEM with a flexible in-situ testing chamber, where the entire instrument can be modified as future technologies are developed. The value would be to obtain a holistic understanding of the underlying physics and chemistry of the process-structure–property relationships in materials exposed to controlled extreme environments. Such a tool would permit the ability to explore, in-situ, the active reaction mechanisms in a controlled manner emulating those of real-world applications with nanometer and nanosecond resolution. If such a powerful tool is developed, it has the potential to revolutionize our materials understanding of nanoscale mechanisms and transients. Graphical Abstract

36 MATERIALS SCIENCE↗
DOE OSTI2022

An Automated Scanning Transmission Electron Microscope Guided by Sparse Data Analytics

Abstract Artificial intelligence (AI) promises to reshape scientific inquiry and enable breakthrough discoveries in areas such as energy storage, quantum computing, and biomedicine. Scanning transmission electron microscopy (STEM), a cornerstone of the study of chemical and materials systems, stands to benefit greatly from AI-driven automation. However, present barriers to low-level instrument control, as well as generalizable and interpretable feature detection, make truly automated microscopy impractical. Here, we discuss the design of a closed-loop instrument control platform guided by emerging sparse data analytics. We hypothesize that a centralized controller, informed by machine learning combining limited a priori knowledge and task-based discrimination, could drive on-the-fly experimental decision-making. This platform may unlock practical, automated analysis of a variety of material features, enabling new high-throughput and statistical studies.

47 OTHER INSTRUMENTATION↗
DOE OSTI2025

Magnon spectroscopy in the electron microscope

Abstract The miniaturization of transistors is approaching its limits owing to challenges in heat management and information transfer speed 1 . To overcome these obstacles, emerging technologies such as spintronics 2 are being developed, which make use of the electron’s spin as well as its charge. Local phenomena at interfaces or structural defects will greatly influence the efficiency of spin-based devices, making the ability to study spin-wave propagation at the nanoscale and atomic scale a key challenge 3,4 . The development of high-spatial-resolution tools to investigate spin waves, also called magnons, at relevant length scales is thus essential to understand how their properties are affected by local features. Here we detect bulk THz magnons at the nanoscale using scanning transmission electron microscopy (STEM). By using high-resolution electron energy-loss spectroscopy with hybrid-pixel electron detectors, we overcome the challenges posed by weak signals to map THz magnon excitations in a thin NiO nanocrystal. Advanced inelastic electron scattering simulations corroborate our findings. These results open new avenues for detecting magnons and exploring their dispersions and their modifications arising from nanoscale structural or chemical defects. This marks a milestone in magnonics and presents exciting opportunities for the development of spintronic devices.

Science & Technology - Other Topics↗
NASA NTRS1975

Scanning electron microscope investigation of the structural growth in thick sputtered coatings

Sputtered S-Monel, silver, and 304 stainless steel coatings and molybdenum disulfide coatings were deposited on mica and metal substrates with various surface finishes to investigate the structural growth of the coating by scanning electron microscopy. The geometry and the surface morphology of the nodules are characterized. Compositional changes within the coating were analyzed by energy dispersive X-ray analysis. Defects in the surface finish act as preferential nucleation sites and form isolated overlapping and complex nodules and various unusual surface overgrowths on the coating. The nodule boundaries are very vulnerable to chemical etching and these nodules do not disappear after full annealing. Further, they have undesirable effects on mechanical properties; cracks are initiated at the nodules when the coating is stressed by mechanical forces.

Spalvins, T.↗
DOE OSTI2021

X-ray diffraction and scanning electron microscope characterizations of the salt waste processing facility tank 101 and tank 104 solid samples

The “as-received” Salt Waste Processing Facility (SWPF) Tank 101 and two Tank 104 samples (pre-wash and washed solids) have been characterized using x-ray diffraction (XRD) and scanning electron microscope/energy dispersive x-ray (SEM/EDX) techniques to address the concerns for the existence of solids, which may interfere with the operational performance of the SWPF crossflow filtration process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS2002

Scanning Electron Microscope Mapping System Developed for Detecting Surface Defects in Fatigue Specimens

An automated two-degree-of-freedom specimen positioning stage has been developed at the NASA Glenn Research Center to map and monitor defects in fatigue specimens. This system expedites the examination of the entire gauge section of fatigue specimens so that defects can be found using scanning electron microscopy (SEM). Translation and rotation stages are driven by microprocessor-based controllers that are, in turn, interfaced to a computer running custom-designed software. This system is currently being used to find and record the location of ceramic inclusions in powder metallurgy materials. The mapped inclusions are periodically examined during interrupted fatigue experiments. The number of cycles to initiate cracks from these inclusions and the rate of growth of initiated cracks can then be quantified. This information is necessary to quantify the effect of this type of defect on the durability of powder metallurgy materials. This system was developed with support of the Ultra Safe program.

Bonacuse, Peter J.↗
DOE OSTI2024

Optimal Geometry for Focused Ion Beam-Milled Samples for Direct-Pull Micro-Tensile Testing Performed In Situ in a Scanning Electron Microscope

A thorough procedure was developed to efficiently manufacture dogbone samples using focused ion beam (FIB) milling for micro-tensile testing. A Bruker PI 89 PicoIndenter, Billerica, MA, USA, was used as a case study, although the analysis and results are applicable to other micro-mechanical testing systems capable of mounting a standard, Ø12.7 mm × Ø3.2 mm pin, scanning electron microscopy (SEM) pin stub (Ted Pella, Redding, CA, USA). Nine dogbones were made from an Fe-45Cu alloy additively manufactured using powder-fed laser-directed energy deposition (DED-LB). Testing showed that fracture was confined to the gauge section for all dogbones and that the fracture mode, ductile vs. brittle, was entirely dependent on the grain orientation relative to the loading direction. The analysis showed that the measured plastic strain to failure can vary from >11% (optimal geometry) to <1% (non-optimal geometry) in micro-tensile testing of high-tensile-strength (>1 GPa) metallic materials. Subsequently, a finite element analysis (FEA) was conducted to identify the improved dogbone geometries. A total of ten thousand dogbone geometries were tested, and their dimensions were defined by a set of four adjustable parameters (corner radius, load surface angle, load surface length, and dogbone head length). The gauge width and gauge length were fixed to 4 µm and 10 µm, respectively. Three-dimensional surface plots of the stress concentration as a function of two parameters were used to identify the optimal ranges of parameter values. The addition of maximum width and length constraints, measuring 25 µm and 30 µm, respectively, allowed us to identify an optimal geometry at load surface angles of 30° and 45°. Their respective dimensions (corner radius, load surface length, and dogbone head length) are, in µm, 12, 6, and 7 and 10, 7, and 7. Testing these two optimal geometries with a range of gauge lengths from 4 to 20 µm showed that smaller gauge lengths only slightly reduced the detrimental stress concentration outside the gauge section. However, smaller gauge lengths will notably improve the FIB surface polishing step as tapering is reduced with smaller dogbone lengths.

Chemistry↗