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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 1,621 records · Page 90
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Evaluating Stage Motion for Automated Electron Microscopy

Abstract Precise control is an essential and elusive quality of emerging self-driving transmission electron microscopes (TEMs). It is widely understood these instruments must be capable of performing rapid, high-volume, and arbitrary movements for practical self-driving operation. However, stage movements are difficult to automate at scale, owing to mechanical instability, hysteresis, and thermal drift. Such difficulties pose major barriers to artificial intelligence-directed microscope designs that require repeatable, precise movements. To guide design of emerging instruments, it is necessary to understand the behavior of existing mechanisms to identify rate limiting steps for full autonomy. Here, we describe a general framework to evaluate stage motion in any TEM. We define metrics to evaluate stage degrees of freedom, propose solutions to improve performance, and comment on fundamental limits to automated experimentation using present hardware.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Design of Electrostatic Aberration Correctors for Scanning Transmission Electron Microscopy

Abstract In a scanning transmission electron microscope (STEM), producing a high-resolution image generally requires an electron beam focused to the smallest point possible. However, the magnetic lenses used to focus the beam are unavoidably imperfect, introducing aberrations that limit resolution. Modern STEMs overcome this by using hardware aberration correctors comprised of many multipole elements, but these devices are complex, expensive, and can be difficult to tune. We demonstrate a design for an electrostatic phase plate that can act as an aberration corrector. The corrector is comprised of annular segments, each of which is an independent two-terminal device that can apply a constant or ramped phase shift to a portion of the electron beam. We show the improvement in image resolution using an electrostatic corrector. Engineering criteria impose that much of the beam within the probe-forming aperture be blocked by support bars, leading to large probe tails for the corrected probe that sample the specimen beyond the central lobe. We also show how this device can be used to create other STEM beam profiles such as vortex beams and probes with a high degree of phase diversity, which improve information transfer in ptychographic reconstructions.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2018

More are better, but the details matter: combinations of multiple Fresnel zone plates for improved resolution and efficiency in X-ray microscopy

Fresnel zone plates used for X-ray nanofocusing face high-aspect-ratio nanofabrication challenges in combining narrow transverse features (for high spatial resolution) along with extended optical modulation along the X-ray beam direction (to improve efficiency). The stacking of multiple Fresnel zone plates along the beam direction has already been shown to offer improved characteristics of resolution and efficiency when compared with thin single zone plates. Using multislice wave propagation simulation methods, here a number of new schemes for the stacking of multiple Fresnel zone plates are considered. These include consideration of optimal thickness and spacing in the axial direction, and methods to capture a fraction of the light otherwise diffracted into unwanted orders, and instead bring it into the desired first-order focus. In conclusion, the alignment tolerances for stacking multiple Fresnel zone plates are also considered.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

3D Nanotomography of calcium silicate hydrates by transmission electron microscopy

Calcium silicate hydrate (C-S-H), is the principal hydration product of Portland cement that mainly contributes to the physical and mechanical properties of concrete. This paper aims to investigate the three-dimensional structure of C-S-H with Ca/Si ratios of 1.0 and 1.6 at the nanoscale using electron tomography. The 3D reconstructions and selected region of interest analysis confirm that the morphology of both C-S-H materials are foil-like structures. Additionally, the difference between the two materials is the density of elongated structures. C-S-H with Ca/Si ratio 1.6 is clearly composed of denser particles compared to the other C-S-H material due to overlapping of the foil-like structure. Pore analysis shows that C-S-H 1.0 and C-S-H 1.6 have porosities 69.2% and 49.8% respectively. Pore size distribution also reveals that C-S-H 1.0 has pore size range between 0-250 nm and C-S-H 1.6 between 0-100 nm. The pore network's size of C-S-H 1.0 is significantly larger than 1.6. This study illustrates the capability of using electron tomography to determine the 3D nanoscale structure of cementitious products and to distinguish between C-S-H 1.0 and 1.6.

42 ENGINEERING↗
DOE OSTI2025

Orientation microscopy–assisted grain boundary analysis for protonic ceramic cell electrolytes

Abstract Grain boundaries in protonic ceramic cell (PCC) electrolytes hinder proton transport, reducing interfacial conductivity. In multicomponent PCC electrolytes, the inclusion of sintering aids further accentuates the complexity of grain boundaries. In this study, we synthesize nanocrystalline BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3− δ thin films via pulsed laser deposition and analyze their grain boundary character distributions using orientation data collected by precession electron diffraction technique. The results reveal an anisotropic distribution of grain boundary characters, with notably high populations of 180°‐tilt and twist grain boundaries. These findings provide critical insights into identifying the predominant grain boundaries in this PCC electrolyte material, assessing the vast five‐dimensional grain boundary space.

Patel, Sooraj [School of Aerospace and Mechanical ↗
DOE OSTI2020

Field emission microscopy of carbon nanotube fibers: Evaluating and interpreting spatial emission

In this work, the authors quantify field emission properties of cathodes made from carbon nanotube (CNT) fibers. The cathodes were arranged in different configurations to determine the effect of cathode geometry on the emission properties. Various geometries were investigated including (1) flat cut fiber tip, (2) folded fiber, (3) looped fiber, and (4) fibers wound around a cylinder. The authors employ a custom field emission microscope to quantify I-V characteristics in combination with laterally resolved field-dependent electron emission area. Additionally, they look at the very early emission stages, first when a CNT fiber is turned on for the first time, which is then followed by multiple ramp-up/down runs. Upon the first turn on, all fibers demonstrated limited and discrete emission area. During ramping runs, all CNT fibers underwent multiple (minor and/or major) breakdowns, which improved emission properties in that turn-on field decreased and field enhancement factor and emission area both increased. It is proposed that breakdowns are responsible for removing initially undesirable emission sites caused by stray fibers higher than average. This initial breakdown process gives way to a larger emission area that is created when the CNT fiber subcomponents unfold and align with the electric field. Overall, the authors' results form the basis for careful evaluation of CNT fiber cathodes for dc or low frequency pulsed power systems in which large uniform area emission is required or for narrow beam high frequency applications in which high brightness is a must.

Image processing↗
DOE OSTI2017

Scanning tunneling microscopy of the atomically smooth (001) surface of vanadium pentoxide V{sub 2}O{sub 5} crystals

The (001) cleavage surface of vanadium pentoxide (V{sub 2}O{sub 5}) crystal has been studied by scanning tunneling spectroscopy (STM). It is shown that the surface is not reconstructed; the STM image allows geometric lattice parameters to be determined with high accuracy. The nanostructure formed on the (001) cleavage surface of crystal consists of atomically smooth steps with a height multiple of unit-cell parameter c = 4.37 Å. The V{sub 2}O{sub 5} crystal cleavages can be used as references in calibration of a scanning tunneling microscope under atmospheric conditions both along the (Ñ…, y) surface and normally to the sample surface (along the z axis). It is found that the terrace surface is not perfectly atomically smooth; its roughness is estimated to be ~0.5 Å. This circumstance may introduce an additional error into the microscope calibration along the z coordinate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Atomic Force Microscopy Local Oxidation of GeO Thin Films

Metastable germanium monoxide (GeO) thin-insulating films have been investigated as a new promising material for atomic force microscope (AFM) oxidation lithography. The kinetics of GeO layer oxidation performed in the tapping mode of AFM was found to have a logarithmic relationship to oxide height versus pulse duration. Effect of humidity on oxidation of germanium monoxide thin films was studied at relative humidity 40, 60, 80%. When local anodic oxidation of GeO layer was carried out by AFM operating in the contact mode in high voltage (≥9 V) regime and at high relative humidity (RH = 80%), the size and shape of fabricated oxide was changed drastically.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Bi-Substituted Iron Garnet Films for Thermomagnetic Recording, Photonics, and Plasmonics: Optimization of Synthesis Conditions Using Scanning Probe Microscopy

We present the results of studies on the optimization of the synthesis of Bi-substituted iron garnet (Bi : IG) films by liquid-phase epitaxy and vacuum deposition followed by crystallization. The effect of the parameter of mismatch between the crystal lattices of the film and the substrate on the functional properties of thin single-crystal high-coercive Bi : IG films is demonstrated. The regime of high-temperature annealing of deposited films was optimized in order to form layers with a high bismuth concentration for magnetophotonic and magnetoplasmonic structures. It was established that annealing of the Bi : IG layer under a SiO{sub 2} layer deposited on top will reduce the roughness of interfaces in multilayer structures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Fast scanning in x-ray microscopy: the effects of offset in the central stop position

Scanning of lightweight circular diffractive optics, separate from central stops and apertures, is emerging as an approach to exploit advances in synchrotron x-ray sources. We consider the effects in a scanning microscope of offsets between the optic and its central stop and find that scan ranges of up to about half the diameter of the optic are possible with only about a 10% increase in the focal spot width. Finally, for large scanning ranges, we present criteria for the working distance between the last aperture and the specimen to be imaged.

47 OTHER INSTRUMENTATION↗
DOE OSTI2016

New insights on ion track morphology in pyrochlores by aberration corrected scanning transmission electron microscopy

Here we demonstrate the enhanced imaging capabilities of an aberration corrected scanning transmission electron microscope to advance the understanding of ion track structure in pyrochlore structured materials (i.e., Gd 2 Ti 2 O 7 and Gd 2 TiZrO 7 ). Track formation occurs due to the inelastic transfer of energy from incident ions to electrons, and atomic-level details of track morphology as a function of energy-loss are revealed in the present work. A comparison of imaging details obtained by varying collection angles of detectors is discussed in the present work. A quantitative analysis of phase identification using high-angle annular dark field imaging is performed on the ion tracks. Finally, a novel 3-dimensional track reconstruction method is provided that is based on depth dependent imaging of the ion tracks. The technique is used in extracting the atomic-level details of nanoscale features, such as the disordered ion tracks, which are embedded in relatively thicker matrix. Another relevance of the method is shown by measuring the tilt of the ion tracks relative to the electron beam incidence that helps in knowing the structure and geometry of ion tracks quantitatively.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

Reconstruction of simulated electrostatic potentials by automatic differentiation-based phase retrieval in electron microscopy imaging

Measuring interfacial electrostatic potentials is vital to understanding many fundamental materials properties. A variety of TEM methods exist for measuring electric potentials from the phase shift produced on an electron wave as it passes through a sample. However, most are either experimentally challenging or poorly suited to resolving nanoscale features. Here, we demonstrate the viability of a simple, automatic differentiation-based exit wave reconstruction from a focal series of images to accurately measure nanoscale electric potentials. Here, the analysis suggests that under optimal measurement conditions, electric potentials can be resolved to less than 0.06 V in magnitude and less than 1 nm in spatial extent.

36 MATERIALS SCIENCE↗