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At least 325 records · Page 18

Doping of Cr in Graphene Using Electron Beam Manipulation for Functional Defect Engineering

Chromium atoms in graphene have been proposed to exhibit magnetic moments and spin-selective conducting states depending on the local bonding geometry within the graphene structure, which could lead to interesting applications in spintronics. Despite this interest, there are few direct experimental reports of Cr dopants in graphene even though it is theorized to be stable. Here, we demonstrate the introduction of single Cr dopant atoms into the graphene lattice and onto graphene edges through the controlled use of a focused electron beam in a scanning transmission electron microscope. Here, we show local control of doping locations, and when coupled with targeted in situ milling during scanning of the e-beam, these strategies demonstrate an important component of the fabrication of tailored nanostructured devices in the electron microscope. The approach is validated with first-principles calculations to understand synthesis pathways during fabrication and reveal the energetics and local properties of Cr atoms embedded in graphene; for example, Cr doping can convert graphene into a magnetic and semiconducting material, which suggests Cr-doped graphene can be used as a building block for potential electronic devices and a means to construct them.

36 MATERIALS SCIENCE↗

Wide Dynamic Range, 10 kHz Framing Detector for 4D-STEM

Hybrid pixel array detectors (PADs) have expanded the fidelity, frame rate and dynamic range for diffractive imaging in electron microscopes. With their high detective quantum efficiencies (DQE), the noise performance limited is by counting statistics. Consequently, improving the precision and quality of high-speed images requires increasing the linear dynamic range and the maximum usable beam current. Here we describe a new prototype hybrid PAD, our next-generation electron microscope pixel array detector (NG-EMPAD) that expands both the framing speed and dynamic range of our earlier EMPAD design. Like the EMPAD, electrons are detected directly in a 500 μm thick silicon sensor bonded pixel-by-pixel to a custom signal processing integrated circuit (IC). Each pixel in the IC integrates charge carriers produced by the high-energy incident electrons. Here, in-pixel circuitry uses a combination of techniques to extend the dynamic range, including adaptive gain switching and the quantitative excess charge dumping similar to the EMPAD. In-pixel buffering of signals during readout allows acquiring a new image while reading out the previously collected image, yielding an image collection duty cycle of nearly 100%.

36 MATERIALS SCIENCE↗

A scanning electron microscopy study of the macro-crystalline structure of 2-(2,4-dinitrobenzyl) pyridine

The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.

Ware, Jacqueline↗

High framerate and high dynamic range electron microscopy

Methods and systems for acquiring transmission electron microscope video data on a rolling-shutter detector at an enhanced frame rate and without temporal distortions are described. Also described are methods to enhance the dynamic range of image and diffraction data acquired using a transmission electron microscope. The disclosed methods and systems may also be applicable to photon detection and imaging systems.

Bloom, Ruth↗

Particulate impacts on the UHCRE cosmic ray experiment teflon covers: The ESA programme

The optical scanning equipment at the University of Kent Unit for Space Science consists of a 102.5 by 42.5 cm computer controlled motorized stage which has a reproduction accuracy of 30 microns over the entire area. This is used with an optical microscope connected to two charge coupled device video cameras which can be used to obtain stereo color images of any features found. A coordinate system can be defined on each cover by means of two or more reference marks which allow a feature to be located using different equipment such as a scanning electron microscope, providing two known marks can be found. By using back illumination, penetrating features can be found automatically, and their sizes, circularity, and positions logged for later revisiting either on the optical system or using a scanning electron microscope.

Mcdonnell, J. A. M.↗

An efficient instance segmentation approach for studying fission gas bubbles in irradiated metallic nuclear fuel

Abstract Gaseous fission products from nuclear fission reactions tend to form fission gas bubbles of various shapes and sizes inside nuclear fuel. The behavior of fission gas bubbles dictates nuclear fuel performances, such as fission gas release, grain growth, swelling, and fuel cladding mechanical interaction. Although mechanical understanding of the overall evolution behavior of fission gas bubbles is well known, lacking the quantitative data and high-level correlation between burnup/temperature and microstructure evolution blocks the development of predictive models and reduces the possibility of accelerating the qualification for new fuel forms. Historical characterization of fission gas bubbles in irradiated nuclear fuel relied on a simple threshold method working on low-resolution optical microscopy images. Advanced characterization of fission gas bubbles using scanning electron microscopic images reveals unprecedented details and extensive morphological data, which strains the effectiveness of conventional methods. This paper proposes a hybrid framework, based on digital image processing and deep learning models, to efficiently detect and classify fission gas bubbles from scanning electron microscopic images. The developed bubble annotation tool used a multitask deep learning network that integrates U-Net and ResNet to accomplish instance-level bubble segmentation. With limited annotated data, the model achieves a recall ratio of more than 90%, a leap forward compared to the threshold method. The model has the capability to identify fission gas bubbles with and without lanthanides to better understand the movement of lanthanide fission products and fuel cladding chemical interaction. Lastly, the deep learning model is versatile and applicable to the micro-structure segmentation of similar materials.

36 MATERIALS SCIENCE↗

Microscopic investigation of cavitation erosion damage in metals

The results of research to identify the cavitation erosion damage mechanisms at the microscopic level for three metals (aluminum, stainless steel, and titanium) representing a range of properties and microstructure are presented. The metals were exposed to cavitation generated in distilled water by a 20-kHz ultrasonic facility operating at a vibration amplitude of 2 mils. Representative properties of the metals and experimental details are summarized. Replicas of the eroded surfaces of the specimens obtained periodically during exposure were examined with a transmission electron microscope to follow progression of the erosion damage and identify dominant erosion mechanisms as a function of exposure time. Eroded surfaces of selected specimens were also examined with a scanning electron microscope to assist in the interpretation.

Hackworh, J. V.↗

A Transmission Electron Microscopy Study of a Refractory Metal Grain from a Calcium-Aluminum-Rich Inclusion in the Leoville CV3 Chondrite

Introduction: Calcium-aluminum-rich inclusions (CAIs) are an important component of chondritic meteorites. They can contain materials that are thermodynamically predicted and isotopically age dated to be among the first-formed solids in our solar system [1-5]. Observed in some CAIs are micron to sub-micron sized inclusions rich in Fe, Ni, and high-Z elements such as Pt, Os, Ir and W, in the form of refractory metal nuggets (RMNs), fremdlinges, and ‘nugget like objects’ (NLOs) [1,6]. Refractory siderophile elements such as Os, Ir and Ru are thermodynamically predicted to condense at temperatures well in excess of the major CAI phases such as melilite, perovskite, spinel and hibonite [2,7-9]. These refractory metal inclusions in CAIs can therefore serve as probes into the thermodynamic landscape of the early solar protoplanetary disk. Here we report on a refractory grain identified in a CAI of the Leoville CV3 chondrite. This work is part of an ongoing effort to gain insight into the thermochemistry of the early solar system through systematic analyses of the structure and chemistry of various components in CAIs [10-13]. Sample and Analytical Techniques: A fluffy type A CAI (Fig. 1A) was identified in a section of the Leoville, CV3 chondrite (Center for Meteorite Studies, Arizona State University collection, #821_C_3) using a JOEL-JXA 8530F electron microprobe at Arizona State University. Backscattered electron (BSE) imaging and energy-dispersive X-ray spectroscopy (EDS) were used to identify refractory metal grains in the CAI using a Thermo Fisher (formerly FEI) Helios NanoLab 660 G3 focused-ion-beam scanning-electron microscope (FIBSEM) located at the Kuiper Materials Imaging and Characterization Facility (KMICF) at the Lunar and Planetary Laboratory, University of Arizona. The FIB is equipped with an EDAX EDS system. We selected one of the larger (micron-sized) refractory metal grains, designated as ‘Spud’ (Fig. 1B) for further analysis. ‘Spud’ was extracted and thinned to electron transparency (<100 nm) using the FIB-SEM located in KMICF, following methods described by [14- 15]. The FIB section was analyzed using a 200 keV Hitachi HF5000 scanning transmission electron microscope (S/TEM) located at KMICF. The HF5000 is equipped with cold-field emission gun, 3rd-order spherical aberration corrector for STEM imaging, and an Oxford Instruments X-Max N 100 TLE energydispersive spectroscopy (EDS) system with dual 100 mm2 windowless silicon-drift detectors (Ω = 2.0 sr). Selected-area electron-diffraction (SAED) patterns were acquired to aid in determination of crystallinity and phase. Results: The mineralogy, texture, and morphology of the CAI are consistent with that of a fluffy type A (FTA) CAI [16]. BSE imaging at high magnifications revealed grains with high contrast, indicative of compositions rich in elements of higher atomic number relative to surrounding material. These high-Z grains have sizes that range from ∼250 nm to 4 µm. EDS analyses confirm that the bright grains are metal-rich inclusions. A minor fraction of the grains are composed of only Fe and Ni, but the majority (∼60%) of the identified inclusions also contained various refractory siderophiles including Os, Ru, Zr, Ir and Mo. EDS analysis on the FIB-SEM of Spud shows that it contains Fe, Ni, Mo and Ru. High-angle annular dark-field (HAAFD) imaging and EDS mapping in the TEM (Fig. 2) show that Spud occurs in melilite (Ca1.9Al1.99Si1.06O7). Spud contains a subhedral to anhedral morphology and is compositionally heterogenous (polyphasic, Fig. 2). Local spatial correlation occurs among Fe, Ni, and Pt, and also among Os, Ru, and Mo. SAED patterns show that the Fe-Ni-Pt, Fe-Os-Mo-Ru and Fe-Pt regions are crystalline. Discussion: CAIs can contain various types of inclusions rich in Fe, Ni and refractory siderophiles such as Os, Ru, W and Pt [1]. RMNs are micron-sized, single phase alloy grains and can contain Os, Ir, Ru and Rh [1,7,17]. NLOs are also micron-sized inclusions, but contain two phases, a refractory metal, and an oxide [6]. Fremdlinge are the largest of such inclusions (tens of microns in size) and are complex aggregates of Fe-Ni alloy, silicates, oxides, and sulfides [1,17]. While the size of Spud matches previous descriptions of RMNs and NLOs, Spud is neither a single-phase alloy like RMNs, nor does it contain one metal phase and one oxide like NLOs. Spud does not match the above described categories of refractory metal inclusions. The presence of refractory siderophiles such as Mo, Os, Ru, and Pt suggests a high-temperature origin. Thermodynamic modelling by [7] indicates condensation temperatures of 1917 K, 1693 K, 1613 K and 1415 K for Os, Mo, Ru and Pt respectively. These models also show that following the initial condensation of a refractory metal, alloying of solutes such as Fe, Ni and W, occurs in levels proportional to their partial pressures in the surrounding gas. Such alloying occurs at temperatures above the condensation temperatures of common CAI phases such as melilite (1529 K), perovskite (1441 K), spinel (197 K) and forsterite (1354 K) [2]. The polyphasic nature of Spud could be the result of such high-temperature alloying, possibly shortly after the condensation of Mo and Ru at 1693 K and 1613 K respectively. That Spud occurs as an inclusion is consistent with it having formed prior to and at temperature above that of its host melilite in this FTA CAI, which is qualitatively consistent with such prior thermodynamic modeling. Further, the polyphasic nature of Spud is similar to refractory grains from a FTA CAI in the Northwest Africa (NWA) 8323, CV3 chondrite [11-13]. These data suggest that such refractory metal grains could have been widespread in the inner and early solar protoplanetary disk and represent some of the earliest formed solids to have condensed. Acknowledgments: Research and instrumentation supported by NASA grants #NNX12AL47G, #NNX15AJ22G and #80NSSC19K0509, and NSF grants #1531243 and #0619599. Fig 2. STEM data on ‘Spud’. HAADF Image (Top) False-color EDS Maps (Bottom) References: [1] MacPherson G. J. (2014) T. of Geochem. Vol I: Met. And Cosmochem. Processes, 139-179. [2] Lodders K. (2003) ApJ, 591, 1220-1247. [3] Ebel D. S. (2006) Met. & the Early S. Sys. II., 253- 277. [4] Amelin Y. (2002) Science, 297, 1678-1683. [5] Connelly J.N. et.al. (2012) Science, 338, 651-655. [6] Schwander D. et al. (2015) GCA, 18, 70-87. [7] Palme H. and Wlotzka F. (1976) EPSL, 33, 45-60. [8] Berg T. et al. (2009) ApJ, 702, 172-176. [9] Liffman K. et al. (2021) Icarus, 221, 89-105. [10] Zega T.J. et al. (2021) PSJ, 2, 115. [11] Ramprasad T. et al. (2020) LPSC LI, Abstract #2472. [12] Ramprasad T. et al. (2021) Microscopy & Microanalysis, S1, 2792-2794. [13] Ramprasad T. et al. (2021) 84th MetSoc, Abstract #6123. [14] Zega T.J. et al. (2007) MAPS, 42, 1373-1386. [15] Ramprasad T. et al. (2022) MAPS, in revision. [16] Grossman L. (1975), GCA, 39, 433-454. [17] El Goresy A. et al. (1978) LPSC IX, Abstract#1100

T. Ramprasad↗

Autophosphorylation-dependent inactivation of plant chimeric calcium/calmodulin-dependent protein kinase

Chimeric calcium/calmodulin dependent protein kinase (CCaMK) is characterized by the presence of a visinin-like Ca(2+)-binding domain unlike other known calmodulin- dependent kinases. Ca(2+)-Binding to the visinin-like domain leads to autophosphorylation and changes in the affinity for calmodulin [Sathyanarayanan P.V., Cremo C.R. & Poovaiah B.W. (2000) J. Biol. Chem. 275, 30417-30422]. Here, we report that the Ca(2+)-stimulated autophosphorylation of CCaMK results in time-dependent loss of enzyme activity. This time-dependent loss of activity or self-inactivation due to autophosphorylation is also dependent on reaction pH and ATP concentration. Inactivation of the enzyme resulted in the formation of a sedimentable enzyme due to self-association. Specifically, autophosphorylation in the presence of 200 microm ATP at pH 7.5 resulted in the formation of a sedimentable enzyme with a 33% loss in enzyme activity. Under similar conditions at pH 6.5, the enzyme lost 67% of its activity and at pH 8.5, 84% enzyme activity was lost. Furthermore, autophosphorylation at either acidic or alkaline reaction pH lead to the formation of a sedimentable enzyme. Transmission electron microscopic studies on autophosphorylated kinase revealed particles that clustered into branched complexes. The autophosphorylation of wild-type kinase in the presence of AMP-PNP (an unhydrolyzable ATP analog) or the autophosphorylation-site mutant, T267A, did not show formation of branched complexes under the electron microscope. Autophosphorylation- dependent self-inactivation may be a mechanism of modulating the signal transduction pathway mediated by CCaMK.

NASA Discipline Plant Biology↗

Dust That's Worth Keeping

Images taken of interstellar space often display a colorful canvas of portions of the electromagnetic spectrum. Dispersed throughout the images are interstellar clouds of dust and gas--remnants ejected from stars and supernovae over billions and billions of years. For more than 40 years, astronomers have observed that interstellar dust exhibits a consistent effect at a spectral wavelength of 2,175 angstroms, the equivalent of 5.7 electronvolts in energy on the electromagnetic spectrum. At this wavelength, light from stars is absorbed by dust in the interstellar medium, blocking the stars light from reaching Earth. The 2,175-angstrom feature, which looks like a bump on spectra, is the strongest ultraviolet-visible light spectral signature of interstellar dust and is visible along nearly every observational line of sight. Scientists have sought to solve the mystery of what causes the 2,175-angstrom feature by reproducing the effect in the laboratory. They speculated a number of possibilities, including fullerenes (buckyballs), nanodiamonds, and even interstellar organisms. However, none of these materials fits the data for the unique spectral feature. Limitations in the energy and spatial resolution achievable with electron microscopes and ion microprobes--the two main instruments used to study samples of dust--have also prevented scientists from finding the answer. A collaborative effort led by Livermore physicist John Bradley and funded by the National Aeronautics and Space Administration (NASA) has used a new-generation transmission electron microscope (TEM) and nanoscale ion microprobe to unlock the mystery. The Livermore group includes physicists Zu Rong Dai, Ian Hutcheon, Peter Weber, and Sasa Bajt and postdoctoral researchers Hope Ishii, Giles Graham, and Julie Smith. They collaborated with the University of California at Davis (UCD), Lawrence Berkeley National Laboratory, Washington University's Laboratory for Space Sciences in St. Louis, and NASA's Ames Research Center for their discovery. The team analyzed micrometer-size interplanetary dust particles (IDPs), each about one-tenth the diameter of a human hair. Within the particles, they found carriers of the 2,175-angstrom feature: organic carbon mixed with amorphous silicates (glass with embedded metals and sulfides, GEMS), two of the most common materials in interstellar space. Ishii says, 'Organic carbon and amorphous silicates are abundant in interstellar dust clouds, and abundant carriers are needed to account for the frequent astronomical observation of the 2,175-angstrom feature. It makes sense that this ubiquitous feature would come from common materials in interstellar space'. The group's results increase scientific understanding of the starting materials for the formation of the Sun, solar system, and life on Earth.

Interstellar matter↗

Damage-free Analysis of Biological Materials by Vibrational Spectroscopy in the EM

In summary, vibrational spectroscopy in the electron microscope promises to probe biological materials in a way that is similar to infrared spectroscopy, at a spatial resolution of about 30-50 nm, while circumventing radiation damage. Herein we are now focused on developing this technique fully, using a side-entry cryotransfer holder in a Nion HERMES electron microscope equipped with a fast and efficient EELS direct detector [10], and capable of 5 meV (and better) energy resolution. The results of these investigations will be reported at the meeting.

59 BASIC BIOLOGICAL SCIENCES↗

Toward Å-fs-meV Resolution in Electron Microscopy: Systematic Simulation of the Temporal Spread of Single-Electron Packets

Though efforts to improve the temporal resolution of transmission electron microscopes (TEMs) have waxed and waned for decades, with relatively recent advances routinely reaching sub-picosecond scales, fundamental and practical challenges have hindered the advance of combined Å-fs-meV resolutions, particularly for core-loss spectroscopy and real-space imaging. This is due in no small part to the complexity of the approach required to access timescales upon which electrons, atoms, molecules, and materials first begin to respond and transform – attoseconds to picoseconds. Here we present part of a larger effort devoted to systematically mapping the instrument parameter space of a TEM modified to reach ultrafast timescales. With General Particle Tracer, we studied the statistical temporal distributions of single-electron packets as a function of various fs pulsed-laser parameters and electron-gun configurations and fields for the exact architecture and dimensions of a Thermo Fisher Tecnai Femto ultrafast electron microscope. We focused on easily-adjustable parameters, such as laser pulse duration, laser spot size, photon energy, Wehnelt aperture diameter, and photocathode size. In addition to establishing trends and dispersion behaviors, we identify regimes within which packet duration can be 100s of fs and approach the 300-fs laser limit employed here. Overall, the results provide a detailed picture of the temporal behavior of single-electron packets in the Tecnai Femto gun region, forming the initial contribution of a larger effort.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Results of examination of the returned Surveyor 3 samples for particulate impacts

The television housing and a section of the strut of the radar altimeter and Doppler velocity sensor were examined optically and with a scanning electron microscope for particulate impacts. The white surface of the camera was discolored during the months the Surveyor 3 was on the moon; however, most of the craters must have occurred as a result of lunar dust sandblasted by the LM exhaust. The polished section of the strut exhibits contamination which appears brown and seems to be partially composed of crystals. Electron microscopic analysis of the strut section indicated no craters of hypervelocity impact origin, confirmed pitting density results of the optical scans, and indicated that material in the craters is of lunar origin. No meteorite impacts larger than 25 microns were detected on the tubing section.

Cour-Palais, B. G.↗

Investigation of the relations between neat resin and advanced composite mechanical properties. Volume 1: Results

A detailed evaluation of one untoughened epoxy baseline resin and three toughened epoxy resin systems was performed. The Hercules 3502, 2220-1, and 2220-3, and Ciba-Geigy Fibredux 914 resin systems were supplied in the uncured state by NASA-Langley and cast into thin flat specimens and round dogbone specimens. Tensile and torsional shear measurements were performed at three temperatures and two moisture conditions. Coefficients of thermal expansion and moisture expansion were also measured. Extensive scanning electron microscopic examination of fracture surfaces was performed, to permit the correlation of observed failure modes with the environmental conditions under which the various specimens were tested. A micromechanics analysis was used to predict the unidirectional composite response under the various test conditions, using the neat resin experimental results as the required input data. Mechanical and physical test results, the scanning electron microscope observations, and the analytical predictions were then correlated.

Zimmerman, R. S.↗

The origin of amorphous rims on lunar plagioclase grains: Solar wind damage or vapor condensates

A distinctive feature of micron sized plagioclase grains from mature lunar soils is a thin (20 to 100 nm) amorphous rim surrounding the grains. These rims were originally described from high voltage electron microscope observations of lunar plagioclase grains by Dran et al., who observed rims up to 100 nm thick on plagioclase grains from Apollo 11 and 12 soils. These rims are believed to be the product of solar wind damage. The amorphous rims were studied on micron sized plagioclase grains from a mature Apollo 16 soil using a JEOL 200FX transmission electron microscope equipped with an energy dispersive x ray spectrometer. It was found that the amorphous rims are compositionally distinct from the interior plagioclase and it is proposed that a major component of vapor condensates is present in the rims.

Keller, Lindsay P.↗

Investigation of the relations between resin and advanced composite mechanical properties. Volume 2: Appendices

One untoughened epoxy baseline resin and three toughened epoxy resin systems were evaluated. The Hercules 3502, 2220-1, and 2220-3, and Ciba-Geigy Fibredux 914 resin systems were supplied in the uncured state by NASA-Langley and cast into thin flat specimens and round dogbone specimens. Tensile and torsional shear measurements were performed at three temperatures and two moisture conditions. Coefficients of thermal expansion and moisture expansion were also measured. Extensive scanning electron microscopic examination of fracture surfaces was performed to permit the correlation of observed failure modes with the environmental conditions under which the various specimens were tested. A micromechanics analysis was used to predict the unidirectional composite response under the various test conditions, incorporating the neat resin experimental results as the required input data. The mechanical and physical test results, the scanning electron microscope observations, and the analytical predictions were then correlated.

Zimmerman, R. S.↗

Effect of grinding on the fatigue life of titanium alloy (5 Al-2.5 Sn) under dry and wet conditions

The principal factors in the performance of aerospace materials are strength-to-weight ratio, fatigue life, fracture toughness, survivability and, of course, reliability. Machining processes and, in particular, grinding under adverse conditions have been found to cause damage to surface integrity and affect the residual stress distribution in the surface and subsurface region. These effects have a direct bearing on the fatigue life. In this investigation the effects of grinding conditions on the fatigue life of Titanium 5 Al-2.5Sn were studied. This alloy is used in ground form in the manufacturing of some critical components in the space shuttle's main engine. It is essential that materials for such applications be properly characterized for use in severe service conditions. Flat sub-size specimens 0.1 inch thick were ground on a surface grinding machine equipped with a variable speed motor at speeds of 2000 to 6000 rpm using SiC wheels of grit sizes 60 and 120. The grinding parameters used in this investigation were chosen from a separate study. The ground specimens were then fatigued at a selected stress and the resulting lives were compared with that of the virgin material. The surfaces of the specimens were examined under a scanning electron microscope, and the roughness and hardness were measured using a standard profilometer and microhardness tester, respectively. The fatigue life of the ground specimens was found to decrease with the increase in speed for both dry and wet conditions. The fatigue life of specimens ground under wet conditions showed a significant increase at the wheel speed of 2000 rpm for both the grit sizes and thereafter decreased with increase profilometry, microhardness measurements and scanning electron microscopic examination.

Rangaswamy, Partha↗