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DOE OSTI2022

Stroboscopic ultrafast imaging using RF strip-lines in a commercial transmission electron microscope

The development of ultrafast electron microscopy (UEM), specifically stroboscopic imaging, has brought the study of structural dynamics to a new level by overcoming the spatial limitations of ultrafast spectroscopy and the temporal restrictions of traditional TEM simultaneously. Combining the concepts governing both techniques has enabled direct visualization of dynamics with spatiotemporal resolutions in the picosecond-nanometer regime. Here, in this study, we push the limits of imaging using a pulsed electron beam via RF induced transverse deflection based on the newly developed 200 keV frequency-tunable strip-line pulser. We demonstrate 0.2 nm spatial resolution at high magnifications and elucidation of Lorentz imaging using the phase-microscopy method. We also present beam coherence measurements and expand our study using the breathing modes of a silicon interdigitated comb under RF excitation which achieves improved temporal synchronization between the electron pulse-train and electric field. A new RF holder has also been developed with impedance matching to the RF signal to minimize transmission power loss to samples and its performance is compared with a conventional sample holder.

47 OTHER INSTRUMENTATION↗

NASA NTRS1990

Digital compression algorithms for HDTV transmission

Digital compression of video images is a possible avenue for high definition television (HDTV) transmission. Compression needs to be optimized while picture quality remains high. Two techniques for compression the digital images are explained and comparisons are drawn between the human vision system and artificial compression techniques. Suggestions for improving compression algorithms through the use of neural and analog circuitry are given.

Adkins, Kenneth C.↗

DOE OSTI2021

Development of liquid cells for high resolution imaging and chemical analysis in situ with Transmission Electron Microscopy

The development of liquid cells for transmission electron microscopy (TEM) have enabled breakthroughs in the study of nanoscale structural, morphological, or chemical changes during materials growth and applications [1]. The challenges of achieving high resolution imaging and chemical analysis through liquids often arise from the liquid cells being too thick. Making ultra-thin freestanding membranes and controlling the liquid thickness are some of the key attributes to the recent liquid cell developments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

4D-STEM of Beam-Sensitive Materials

We report that a scanning electron nanobeam diffraction, or 4D-STEM (four-dimensional scanning transmission electron microscopy), is a flexible and powerful approach to elucidate structure from "soft" materials that are challenging to image in the transmission electron microscope because their structure is easily damaged by the electron beam. In a 4D-STEM experiment, a converged electron beam is scanned across the sample, and a pixelated camera records a diffraction pattern at each scan position. This four-dimensional data set can be mined for various analyses, producing maps of local crystal orientation, structural distortions, crystallinity, or different structural classes. Holding the sample at cryogenic temperatures minimizes diffusion of radicals and the resulting damage and disorder caused by the electron beam. The total fluence of incident electrons can easily be controlled during 4D-STEM experiments by careful use of the beam blanker, steering of the localized electron dose, and by minimizing the fluence in the convergent beam thus minimizing beam damage. This technique can be applied to both organic and inorganic materials that are known to be beam-sensitive; they can be highly crystalline, semicrystalline, mixed phase, or amorphous. One common example is the case for many organic materials that have a π-π stacking of polymer chains or rings on the order of 3.4-4.2 Å separation. If these chains or rings are aligned in some regions, they will produce distinct diffraction spots (as would other crystalline spacings in this range), though they may be weak or diffuse for disordered or weakly scattering materials. We can reconstruct the orientation of the π-π stacking, the degree of π-π stacking in the sample, and the domain size of the aligned regions. This Account summarizes illumination conditions and experimental parameters for 4D-STEM experiments with the goal of producing images of structural features for materials that are beam-sensitive. We will discuss experimental parameters including sample cooling, probe size and shape, fluence, and cameras. 4D-STEM has been applied to a variety of materials, not only as an advanced technique for model systems, but as a technique for the beginning microscopist to answer materials science questions. It is noteworthy that the experimental data acquisition does not require an aberration-corrected TEM but can be produced on a variety of instruments with the right attention to experimental parameters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1993

Laser-enhanced synthesis and processing of diamond films from liquid hydrocarbons

We report synthesis of diamond films by pulsed laser irradiation on copper substrate immersed into liquid benzene. It is envisaged that carbon released from benzene at the liquid-solid interface is converted into diamond as a result of rapid quenching from a high temperature. The diamond crystallites were characterized using high resolution transmission electron microscopy imaging and electron diffraction techniques. Growth of thicker diamond films by subsequent chemical vapor deposition has been investigated by transmission and scanning electron microscopy techniques. Thin diamond film deposited during liquid phase provided seed for diamond growth during subsequent chemical vapor deposition.

Singh, Jogender↗

DOE OSTI2022

Multi-modal tomographic imaging system for poolside characterization of nuclear test fuels: Design considerations and studies

Testing and qualification of advanced nuclear fuels involves an iterative process of prototyping, in-pile irradiation testing, and in-situ or ex-situ examination. Fuel restructuring and fission product migration during burnup are among the most important aspects of fuel evolution that affect several important performance characteristics such as heat removal, accident tolerance, and fission product retention. Pool-side non-destructive characterization techniques provide fuel developers with tools to understand fuel evolution at different points of burnup. A design for a compact, submersible, and multi-modal gamma-ray tomography system for imaging irradiated nuclear fuel is presented here. Detector selection, collimator geometry and fabrication, mechanical design, imaging protocol and acquisition speed are discussed. Modeling calculations show that sub-millimeter resolution can be achieved in both transmission computed tomography images as well as in emission computed tomography images in a matter of hours. Several design compromises and fabrication challenges are discussed which should be taken into consideration for future submersible gamma-ray tomography instruments.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Direct imaging of electron density with a scanning transmission electron microscope

Abstract Recent studies of secondary electron (SE) emission in scanning transmission electron microscopes suggest that material’s properties such as electrical conductivity, connectivity, and work function can be probed with atomic scale resolution using a technique known as secondary electron e-beam-induced current (SEEBIC). Here, we apply the SEEBIC imaging technique to a stacked 2D heterostructure device to reveal the spatially resolved electron density of an encapsulated WSe 2 layer. We find that the double Se lattice site shows higher emission than the W site, which is at odds with first-principles modelling of valence ionization of an isolated WSe 2 cluster. These results illustrate that atomic level SEEBIC contrast within a single material is possible and that an enhanced understanding of atomic scale SE emission is required to account for the observed contrast. In turn, this suggests that, in the future, subtle information about interlayer bonding and the effect on electron orbitals could be directly revealed with this technique.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Characterization of Mn 5 Ge 3 Contacts on a Shallow Ge/SiGe Heterostructure

Mn 5 Ge 3 is a ferromagnetic phase of the Mn-Ge system that is a potential contact material for efficient spin injection and detection. Here, we investigate the creation of Mn 5 Ge 3 -based contacts on a Ge/SiGe quantum well heterostructure via solid-state synthesis. X-ray diffraction spectra fitting indicates the formation of Mn 5 Ge 3 -based contacts on bulk Ge and Ge/SiGe. High-resolution scanning transmission electron microscopy imaging and energy dispersive X-ray spectroscopy verify the correct Mn 5 Ge 3 -based phase formation. Schottky diode measurements, transmission line measurements, and Hall measurements reveal that Mn 5 Ge 3 -based contacts serve as good p-type contacts for Ge/SiGe quantum well heterostructures due to having a low Schottky barrier height of 0.10 eV (extracted from a Mn 5 Ge 3 /n-Ge analogue) and a contact resistance in the order of 1 kΩ. Furthermore, we show that these electrical characteristics have a gate-voltage dependence, thereby providing tunability.

36 MATERIALS SCIENCE↗

NASA NTRS1978

Potential end-to-end imaging information rate advantages of various alternative communication systems

Various communication systems were considered which are required to transmit both imaging and a typically error sensitive, class of data called general science/engineering (gse) over a Gaussian channel. The approach jointly treats the imaging and gse transmission problems, allowing comparisons of systems which include various channel coding and data compression alternatives. Actual system comparisons include an Advanced Imaging Communication System (AICS) which exhibits the rather significant potential advantages of sophisticated data compression coupled with powerful yet practical channel coding.

Rice, R. F.↗

NASA NTRS1982

End-to-end imaging information rate advantages of various alternative communication systems

The efficiency of various deep space communication systems which are required to transmit both imaging and a typically error sensitive class of data called general science and engineering (gse) are compared. The approach jointly treats the imaging and gse transmission problems, allowing comparisons of systems which include various channel coding and data compression alternatives. Actual system comparisons include an advanced imaging communication system (AICS) which exhibits the rather significant advantages of sophisticated data compression coupled with powerful yet practical channel coding. For example, under certain conditions the improved AICS efficiency could provide as much as two orders of magnitude increase in imaging information rate compared to a single channel uncoded, uncompressed system while maintaining the same gse data rate in both systems. Additional details describing AICS compression and coding concepts as well as efforts to apply them are provided in support of the system analysis.

Rice, R. F.↗

NASA NTRS2000

Real-time transmission of full-motion echocardiography over a high-speed data network: impact of data rate and network quality of service

With high-resolution network transmission required for telemedicine, education, and guided-image acquisition, the impact of errors and transmission rates on image quality needs evaluation. METHODS: We transmitted clinical echocardiograms from 2 National Aeronautics and Space Administration (NASA) research centers with the use of Motion Picture Expert Group-2 (MPEG-2) encoding and asynchronous transmission mode (ATM) network protocol over the NASA Research and Education Network. Data rates and network quality (cell losses [CLR], errors [CER], and delay variability [CVD]) were altered and image quality was judged. RESULTS: At speeds of 3 to 5 megabits per second (Mbps), digital images were superior to those on videotape; at 2 Mbps, images were equivalent. Increasing CLR caused occasional, brief pauses. Extreme CER and CDV increases still yielded high-quality images. CONCLUSIONS: Real-time echocardiographic acquisition, guidance, and transmission is feasible with the use of MPEG-2 and ATM with broadcast quality seen above 3 Mbps, even with severe network quality degradation. These techniques can be applied to telemedicine and used for planned echocardiography aboard the International Space Station.

NASA Discipline Cardiopulmonary↗

DOE OSTI2023

Plasmonic nanorod probes’ journey inside plant cells for in vivo SERS sensing and multimodal imaging

Nanoparticle-based platforms are gaining strong interest in plant biology and bioenergy research to monitor and control biological processes in whole plants. However, in vivo monitoring of biomolecules using nanoparticles inside plant cells remains challenging due to the impenetrability of the plant cell wall to nanoparticles beyond the exclusion limits (5-20 nm). To overcome this physical barrier, we have designed unique bimetallic silver-coated gold nanorods (AuNR@Ag) capable of entering plant cells, while conserving key plasmonic properties in the near-infrared (NIR). To demonstrate cellular internalization and tracking of the nanorods inside plant tissue, we used a comprehensive multimodal imaging approach that included transmission electron microscopy (TEM), confocal fluorescence microscopy, two-photon luminescence (TPL), X-ray fluorescence microscopy (XRF), and photoacoustics imaging (PAI). We successfully acquired SERS signals of nanorods in vivo inside plant cells of tobacco leaves. On the same leaf samples, we applied orthogonal imaging methods, TPL and PAI techniques for in vivo imaging of the nanorods. This study first demonstrates the intracellular internalization of AuNR@Ag inside whole plant systems for in vivo SERS analysis in tobacco cells. This work demonstrates the potential of this nanoplatform as a new nanotool for intracellular in vivo biosensing for plant biology.

Cupil-Garcia, Vanessa↗

NASA NTRS1985

Optical performance of synthetic aperture telescope configurations

The diffraction-limited performances of synthetic aperture configuration arrays of four telescopes, used for coherent imaging or beam transmission, are calculated and compared. The optical performance of phased telescope arrays was found to be more sensitive to rms piston errors than to rms tilt errors. Image degradation due to pupil mapping errors imposes tight tolerances upon the structural integrity of the telescope. One part in 10,000 pupil mapping error limits the field-of-view to approximately 30 arcsec. Field curvature of the independent telescopes provides a fundamental limit to the field-of-view for phased arrays made up of two-mirror telescopes. These field-of-view limitations may profoundly affect target acquisition, tracking, or imaging applications.

Harvey, J. E.↗

NASA NTRS1972

The synchronous meteorological satellite /SMS/ system.

The responsibilities of the National Aeronautics and Space Administration (NASA) and Department of Commerce (DOC) pertaining to SMS are described in this paper. A description of the program objectives, payload, and spacecraft subsystems, is included along with an abbreviated description of the SMS ground system. Particular interest is directed towards the visible and infrared spin-scan radiometer (VISSR) as it will be the prime sensor and its performance directly effect the mission objectives. Also, of significant importance is the description of the communications subsystem since transmission and retransmission of image data, data relay, and data collection platform (DCP) transmissions play such a major role in the system. The conclusion is established that the current plans form a workable system for providing timely, high-quality day and night imaging of the earth's weather.

Burr, P. T.↗

DOE OSTI2020

In situ high-temperature X-ray diffraction study of Sc-doped titanium oxide nanocrystallites

Titanium dioxide is an inexpensive wide-gap highly ionic semiconductor with striking photocatalytic capabilities in several heterogeneous photoredox reactions. A small crystal size is desirable to maximize the surface area, since photocatalytic reactions occur at the surface of a photocatalyst. Presented in this work are the synthesis and microstructural characterization of 4 at.% Sc-doped TiO 2 (4SDT) prepared by water-based co-precipitation. The crystal structure of 4SDT was examined via in situ high-temperature powder X-ray diffraction experiments from 25 to 1200°C. Rietveld analysis revealed single-phase anatase up to 875°C, while at 900°C the anatase-to-rutile phase transformation occurred and at higher temperatures additional reflections of Sc-rich phases (Sc 2 TiO 5 from 975°C and Ti 3 Sc 4 O 12 or Sc 2 O 3 at 1200°C) were observed. Debye function analysis (DFA) was applied to model the total scattering pattern directly in reciprocal space, allowing the reconstruction of Ti vacancies. Both Rietveld and DFA methods were applied to estimate the nanocrystallite size and shape with consistent growth in crystallite size with temperature: an ellipsoid shape with equatorial ~4.7 nm / axial (001) ~6.9 nm at 25°C to equatorial ~27.9 nm / axial (001) ~39.6 nm at 900°C refined by Rietveld analysis, versus a cylinder shape with D a , b = 4.3 nm and size dispersion σ ab = 1.5 nm, L c = 4.9 nm and σ c = 2.3 nm at 25°C to D a , b = 21.4 nm, σ ab = 8.3 nm, L c = 23.9 and σ c = 10.9 nm at 900°C estimated by DFA. The microstructural changes obtained by Rietveld and DFA methods were supported by high-resolution transmission electron microscopy image analysis, as well as by the less direct nitrogen sorption techniques that provide information on the size of non-agglomerated and dense particles. The Ti site-occupancy factor showed a linear increase from 0.6–0.8 at 25°C to unity at 900°C for anatase, and from ~0.7 at 900°C to unity at 1200°C for rutile, via Rietveld analysis and DFA.

36 MATERIALS SCIENCE↗

NASA NTRS1996

Active-Pixel Image Sensors With Programmable Resolution

Active-pixel image sensors with programmable resolution proposed for use in applications in which speed and efficiency of processing of image data enhanced by providing those data at varying resolutions. Such applications include modeling of biological vision, stereoscopic range-finding, recognition of patterns, tracking targets, and progressive transmission of compressed images. In target-tracking application, sensor initially forms low-resolution image from which area of interest identified, then sensor set at high resolution for examination of identified area. Outputs of contiguous pixels combined. Sensor of this type made to act as though it comprised fewer and larger pixels.

Kemeny, Sabrina E.↗

NASA NTRS2003

Cable and Line Inspection Mechanism

An automated cable and line inspection mechanism visually scans the entire surface of a cable as the mechanism travels along the cable=s length. The mechanism includes a drive system, a video camera, a mirror assembly for providing the camera with a 360 degree view of the cable, and a laser micrometer for measuring the cable=s diameter. The drive system includes an electric motor and a plurality of drive wheels and tension wheels for engaging the cable or line to be inspected, and driving the mechanism along the cable. The mirror assembly includes mirrors that are positioned to project multiple images of the cable on the camera lens, each of which is of a different portion of the cable. A data transceiver and a video transmitter are preferably employed for transmission of video images, data and commands between the mechanism and a remote control station.

Terence J Ross↗

NASA NTRS2003

Cable and line inspection mechanism

Ross, Terence J.↗