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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Preparing Lamellae from Vitreous Biological Samples using a Dual-Beam Scanning Electron Microscope for Cryo-Electron Tomography

Presented here is a protocol for preparing cryo-lamellae from plunge-frozen grids of Plasmodium falciparum-infected human erythrocytes, which could easily be adapted for other biological samples. The basic principles for preparing samples, milling, and viewing lamellae are common to all instruments and the protocol can be followed as a general guide to on-grid cryo-lamella preparation for cryo-electron microscopy (cryoEM) and cryo-electron tomography (cryoET). Electron microscopy grids supporting the cells are plunge-frozen into liquid nitrogen-cooled liquid ethane using a manual or automated plunge freezer, then screened on a light microscope equipped with a cryo-stage. Frozen grids are transferred into a cryo-scanning electron microscope equipped with a focused ion beam (cryoFIB-SEM). Grids are routinely sputter coated prior to milling, which aids dispersal of charge build-up during milling. Alternatively, an e-beam rotary coater can be used to apply a layer of carbon-platinum to the grids, the exact thickness of which can be more precisely controlled. Once inside the cryoFIB-SEM an additional coating of an organoplatinum compound is applied to the surface of the grid via a gas injection system (GIS). This layer protects the front edge of the lamella as it is milled, the integrity of which is critical for achieving uniformly thin lamellae. Regions of interest are identified via SEM and milling is carried out in a step-wise fashion, reducing the current of the ion beam as the lamella reaches electron transparency, in order to avoid excessive heat generation. A grid with multiple lamellae is then transferred to a transmission electron microscope (TEM) under cryogenic conditions for tilt-series acquisition. A robust and contamination-free workflow for lamella preparation is an essential step for downstream techniques, including cellular cryoEM, cryoET, and sub-tomogram averaging. Development of these techniques, especially for lift-out and milling of high-pressure frozen samples, is of high-priority in the field.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Resolving the Electron Plume within a Scanning Electron Microscope

Scanning electron microscopy (SEM), a century-old technique, is today a ubiquitous method of imaging the surface of nanostructures. However, most SEM detectors simply count the number of secondary electrons from a material of interest, and thereby overlook the rich material information contained within them. Here, by simple modifications to a standard SEM tool, we resolve the momentum and energy information on secondary electrons by directly imaging the electron plume generated by the electron beam of the SEM. Leveraging these spectroscopic imaging capabilities, our technique is able to image lateral electric fields across a prototypical silicon p–n junctions and to distinguish differently doped regions, even when buried beyond depths typically accessible by SEM. Intriguingly, the subsurface sensitivity of this technique reveals unexpectedly strong surface band bending within nominally passivated semiconductor structures, providing useful insights for complex layered component designs, in which interfacial dynamics dictate device operation. Further, these capabilities for noninvasive, multimodal probing of complicated electronic components are crucial in today’s electronic manufacturing but is largely inaccessible even with sophisticated techniques. These results show that seemingly simple SEM can be extended to probe complex and useful material properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Integrated transmission electron microscope

An integrated transmission electron microscope comprising multiple electron sources for tuned beams of ultrafast, scanning probe, and parallel illumination in varied beam energies can be alternated within sub-microseconds onto a sample with dynamic ‘transient state’ processes to acquire atomic-scale structural/chemical data with site specificity. The various electron sources and condenser optics enable high-resolution imaging, high-temporal resolution imaging, and chemical imaging, using fast-switching magnets to direct the different electron beams onto a single maneuverable objective pole piece where the sample resides. Such multimodal in situ characterization tools housed in a single microscope have the potential to revolutionize materials science.

Jungjohann, Katherine L.↗
DOE OSTI2023

Development of an in situ ion irradiation scanning electron microscope

An in situ ion irradiation scanning electron microscope (I 3 SEM) has been developed, installed, and integrated into the Ion Beam Laboratory at Sandia National Laboratories. The I 3 SEM facility combines a field emission, variable pressure, scanning electron microscope, a 6 MV tandem accelerator, high flux low energy ion source, an 808 nm-wavelength laser, and multiple stages to control the thermal and mechanical state of the sample observed. The facility advances real-time understanding of materials evolution under combined environments at the mesoscale. As highlighted in multiple examples, this unique combination of tools is optimized for studying mesoscale material response in overlapping extreme environments, allowing for simultaneous ion irradiation, implantation, laser bombardment, conductive heating, cooling, and mechanical deformation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
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 OSTI2021

Controlling hydrocarbon transport and electron beam induced deposition on single layer graphene: Toward atomic scale synthesis in the scanning transmission electron microscope

Abstract Focused electron beam induced deposition (FEBID) is a direct write technique for depositing materials on a support substrate akin to 3D printing with an electron beam (e‐beam). Opportunities exist for merging this existing technique with aberration‐corrected scanning transmission electron microscopy to achieve molecular‐ or atomic‐level spatial precision. Several demonstrations have been performed using graphene as the support substrate. A common challenge that arises during this process is e‐beam‐induced hydrocarbon deposition, suggesting greater control over the sample environment is needed. Various strategies exist for cleaning graphene in situ. One of the most effective methods is to rapidly heat to high temperatures, for example, 600℃ or higher. While this can produce large areas of what appears to be atomically clean graphene, mobile hydrocarbons can still be present on the surfaces. Here, we show that these hydrocarbons are primarily limited to surface migration and demonstrate an effective method for interrupting the flow using e‐beam deposition to form corralled hydrocarbon regions. This strategy is effective for maintaining atomically clean graphene at high temperatures where hydrocarbon mobility can lead to substantial accumulation of unwanted e‐beam deposition.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Reducing experimental uncertainty in the calculation of cavity swelling in a transmission electron microscope through crystallographically aided void volume tracking

Accurate measurement of cavity swelling in a transmission electron microscope is essential to define material performance under irradiation, and the conventionally applied spherical assumption for the calculation of cavity volumes in irradiated materials can result in errors ranging between a 25% underestimation and 72% overestimation of volume purely based on the assumption of shape. This assumption is undeniably expedient for calculation but does not sufficiently account for the 3D nature of polyhedral cavities and their shape projection in the transmission electron microscope, and therefore presents too large of an associated uncertainty in swelling determination for faceted cavities. This uncertainty has been defined for many common cavity shapes in FCC and BCC crystal systems, and has been tabulated across the cubic fundamental region. A revised methodology for crystallographically aided void volume tracking, or CAVV-T, is presented and demonstrated on a specimen of neutron irradiated Ni. In-depth discussion on the application of this technique is provided along with resources to allow for conversion between the spherical assumption and this revised method. This work seeks to increase experimental confidence in the characterization and quantification of critical aspects of irradiation damage in materials by applying a crystallographically-resolved approach for cavity swelling calculation.

Haag IV, James V. [Pacific Northwest National Labo↗
DOE OSTI2023

Gas delivery system for environmental transmission electron microscope

A portable, compact gas delivery system can support an environmental transmission electron microscope. Environment transmission electron microscopy provides researchers a unique capability of assessing a material's surface conditions at atomic resolution in a variety of reactive and oxidizing environments. The ability to precisely control the analysis chamber's environmental conditions over time is key to the success of a typical surface analysis. The gas delivery system provides the correct balance or pressure delivery precision, contamination control, and gas isolation.

Nogan, John Joseph↗
DOE OSTI2024

Single Electron Self-coherence and Its Wave/Particle Duality in the Electron Microscope

Intensities in high-resolution phase-contrast images from electron microscopes build up discretely in time by detecting single electrons. A wave description of pulse-like coherent-inelastic interaction of an electron with matter implies a time-dependent coexistence of coherent partial waves. Their superposition forms a wave package by phase decoherence of 0.5 - 1 radian with Heisenbergs energy uncertainty ΔE H = $\hbar$/2 Δt -1 matching the energy loss ΔE of a coherent-inelastic interaction and sets the interaction time Δt. In these circumstances, the product of Planck's constant and the speed of light hc is given by the product of the expression for temporal coherence λ 2 /Δλ and the energy loss ΔE. Experimentally, the self-coherence length was measured by detecting the energy-dependent localization of scattered, plane matter waves in surface proximity exploiting the Goos–Hänchen shift. Chromatic-aberration Cc-corrected electron microscopy on boron nitride (BN) proves that the coherent crystal illumination and phase contrast are lost if the self-coherence length shrinks below the size of the crystal unit cell at ΔE > 200 eV. Finally, in perspective, the interaction time of any matter wave compares with the lifetime of a virtual particle of any elemental interaction, suggesting the present concept of coherent-inelastic interactions of matter waves might be generalizable.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2024

Quantification of grain boundary effects on the geometrically necessary dislocation density evolution and strain hardening of polycrystalline Mg 4Al using in situ tensile testing in scanning electron microscope and HR-EBSD

In situ tensile testing in a scanning electron microscope (SEM) in conjunction with high-resolution electron backscatter diffraction (HR-EBSD) under load was used to characterize the evolution of geometrically necessary dislocation (GND) densities at individual grain boundaries as a function of applied strain in a polycrystalline Mg—4Al alloy. The increase in GND density was investigated at plastic strains of 0 %, 0.6 %, 2.2 %, 3.3 % from the area including 76 grains and correlated with (i) geometric compatibility between slip systems across grain boundaries, and (ii) plastic incompatibility. We develop expressions for the grain boundary GND density evolution as a function of plastic strain and plastic incompatibility, from which uniaxial tensile stress-strain response of polycrystalline Mg—4Al are computed and compared with experimental measurement. The findings in this study contribute to understanding the mechanisms governing the strain hardening response of single-phase polycrystalline alloys and more reliable prediction of mechanical behaviors in diverse microstructures.

Geometrically necessary dislocations↗
DOE OSTI2024

Precision-controlled ultrafast electron microscope platforms. A case study: Multiple-order coherent phonon dynamics in 1T-TaSe2 probed at 50 fs–10 fm scales

We report on the first detailed beam tests attesting the fundamental principle behind the development of high-current-efficiency ultrafast electron microscope systems where a radio frequency (RF) cavity is incorporated as a condenser lens in the beam delivery system. To allow for the experiment to be carried out with a sufficient resolution to probe the performance at the emittance floor, a new cascade loop RF controller system is developed to reduce the RF noise floor. Temporal resolution at 50 fs in full-width-at-half-maximum and detection sensitivity better than 1% are demonstrated on exfoliated 1T-TaSe2 system under a moderate repetition rate. To benchmark the performance, multi-terahertz edge-mode coherent phonon excitation is employed as the standard candle. The high temporal resolution and the significant visibility to very low dynamical contrast in diffraction signals via high-precision phase-space manipulation give strong support to the working principle for the new high-brightness femtosecond electron microscope systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

A Platform for Atomic Fabrication and In Situ Synthesis in a Scanning Transmission Electron Microscope

Here, the engineering of quantum materials requires the development of tools able to address various synthesis and characterization challenges. These include the establishment and refinement of growth methods, material manipulation, and defect engineering. Atomic-scale modification will be a key enabling factor for engineering quantum materials where desired phenomena are critically determined by atomic structures. Successful use of scanning transmission electron microscopes (STEMs) for atomic scale material manipulation has opened the door for a transformed view of what can be accomplished using electron-beam-based strategies. However, serious obstacles exist on the pathway from possibility to practical reality. One such obstacle is the in situ delivery of atomized material in the STEM to the region of interest for further fabrication processes. Here, progress on this front is presented with a view toward performing synthesis (deposition and growth) processes in a scanning transmission electron microscope in combination with top-down control over the reaction region. An in situ thermal deposition platform is presented, tested, and deposition and growth processes are demonstrated. In particular, it is shown that isolated Sn atoms can be evaporated from a filament and caught on the nearby sample, demonstrating atomized material delivery. This platform is envisioned to facilitate real-time atomic resolution imaging of growth processes and open new pathways toward atomic fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Achieving sub-0.5-angstrom–resolution ptychography in an uncorrected electron microscope

Subangstrom resolution has long been limited to aberration-corrected electron microscopy, where it is a powerful tool for understanding the atomic structure and properties of matter. Here, we demonstrate electron ptychography in an uncorrected scanning transmission electron microscope (STEM) with deep subangstrom spatial resolution down to 0.44 angstroms, exceeding the conventional resolution of aberration-corrected tools and rivaling their highest ptychographic resolutions​. Our approach, which we demonstrate on twisted two-dimensional materials in a widely available commercial microscope, far surpasses prior ptychographic resolutions (1 to 5 angstroms) of uncorrected STEMs. We further show how geometric aberrations can create optimized, structured beams for dose-efficient electron ptychography. Our results demonstrate that expensive aberration correctors are no longer required for deep subangstrom resolution.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Delineation of the impact on temporal behaviors of off-axis photoemission in an ultrafast electron microscope

Efforts to push the spatiotemporal imaging-resolution limits of femtosecond laser-driven ultrafast electron microscopes (UEMs) to the combined angstrom–fs range will benefit from stable sources capable of generating high bunch charges. Recent demonstrations of unconventional off-axis photoemitting geometries are promising, but connections to the observed onset of structural dynamics are yet to be established. Here we use the in-situ photoexcitation of coherent phonons to quantify the relative time-of-flight (r-TOF) of photoelectron packets generated from the Ni Wehnelt aperture and from a Ta cathode set-back from the aperture plane. We further support the UEM experiments with particle-tracing simulations of the precise electron-gun architecture and photoemitting geometries. In this way, we measure discernible shifts in electron-packet TOF of tens of picoseconds for the two photoemitting surfaces. Furthermore, these shifts arise from the impact that the Wehnelt-aperture off-axis orientation has on the electron-momentum distribution, which modifies both the collection efficiency and the temporal-packet distribution relative to on-axis emission. Future needs are identified; we expect this and other developments in UEM electron-gun configuration to expand the range of material phenomena that can be directly imaged on scales commensurate with fundamental structural dynamics.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Quantitative Assessment and Measurement of X-ray Detector Performance and Solid Angle in the Analytical Electron Microscope

A wide range of X-ray detectors and geometries are available today on transmission/scanning transmission analytical electron microscopes. While there have been numerous reports of their individual performance, no single experimentally reproducible metric has been proposed as a basis of comparison between the systems. In this paper, we detail modeling, experimental procedures, measurements, and specimens which can be used to provide a manufacturer-independent assessment of the performance of an analytical system. Using these protocols, the geometrical collection efficiency, system peaks, and minimum detection limits can be independently assessed and can be used to determine the best conditions to conduct modern hyperspectral and/or spectrally resolved tomographic analyses for an individual instrument. Here, a simple analytical formula and specimen is presented which after suitable system calibrations can be used to experimentally determine the X-ray detector solid angle.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Wehnelt photoemission in an ultrafast electron microscope: Stability and usability

We tested and compared the stability and usability of three different cathode materials and configurations in a thermionic-based ultrafast electron microscope: (1) on-axis thermionic and photoemission from a custom 100 μm diameter LaB 6 source with a graphite guard ring, (2) off-axis photoemission from the Ni aperture surface of the Wehnelt electrode, and (3) on-axis thermionic and photoemission from a custom 200 μm diameter polycrystalline Ta source. For each cathode type and configuration, including the Ni Wehnelt aperture, we illustrate how the photoelectron beam-current stability is deleteriously impacted by simultaneous cooling of the source following thermionic heating. Furthermore, we demonstrate usability via collection of parallel- and convergent-beam electron diffraction patterns and by formation of the optimum probe size. We find that usability of the off-axis Ni Wehnelt-aperture photoemission is at least comparable to on-axis LaB 6 thermionic emission, as well as to on-axis photoemission [the heretofore conventional approach to ultrafast electron microscopy (UEM) in thermionic-based instruments]. However, the stability and achievable beam currents for off-axis photoemission from the Wehnelt aperture were superior to that of the other cathode types and configurations, regardless of the electron-emission mechanism. Beam-current stability for this configuration was found to be ±1% (one standard deviation from the mean) for 70 min (longest duration tested), and steady-state beam current was reached within the sampling-time resolution used here (~1 s) for 15 pA beam currents (i.e., 460 electrons per packet for a 200 kHz repetition rate). Repeatability and robustness of the steady-state condition were also found to be within ±1% of the mean. We discuss the implications of these findings for UEM imaging and diffraction experiments, for pulsed-beam damage measurements, and for practical switching between optimum conventional TEM and UEM operation within the same instrument.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2025

Surface deposition of nanometer scale carbon structures on Bi 2 Sr 2 CaCu 2 O 8+δ using a low-cost scanning electron microscope

In this work, we investigate optically active nanostructures on Bi 2 Sr 2 CaCu 2 O 8+δ (BSCCO). The nanostructures are constructed from carbon nanocrystals formed using the electron beam of a scanning electron microscope to locally decompose residual hydrocarbons at the BSCCO surface. Atomic force microscopy is used to characterize the dimensions of these structures as a function of beam exposure time. This technique has been used to induce localized intercalation to form carbon nanoparticles up to tens of nanometers into a variety of 2D materials. Cross-sectional scanning transmission electron microscopy in BSCCO shows the presence of these carbon deposits on the surface, but there is no evidence they penetrate into the BSCCO substrate. Therefore, this technique is not suitable for localized intercalation in BSCCO, and it does have promise as a cost-effective approach to pattern nanometer scale etch stops.

2D materials↗
DOE OSTI2024

First-Principles Simulation of Beam-Induced Processes Underlying Atomic Manipulation in Electron Microscopes

The development of experimental methods and apparatuses capable of promoting atomically precise material manipulations holds great promise for realizing the ultimate limit of feature miniaturization in materials and devices. The ability to modify materials atom by atom is anticipated to usher in new technologies in areas as diverse as separation science, medicine, and quantum information science. Historically, scanning probe-based techniques have been the most prominent approaches in this space. However, these methods are best suited for the manipulation of surface-exposed regions of materials, as the strong perturbations required for bond scission are delivered most effectively to atoms in the near-proximity to the scanning probe. In contrast, convergent electron beams with energies tuned slightly below the threshold for inducing irreversible knock-on damage have recently been employed (within scanning transmission electron microscopy) to promote atomic-scale bond rearrangements in various beam-stable solids. Currently, however, the efficiency and selectivity of beam-induced atomic manipulation processes with focused electron beams are such that long irradiation times are required to induce a desired atomic rearrangement. With a better understanding of the underlying physics dictating the outcome of a given irradiation event, methods can be devised to improve the efficiency of these techniques so that their promise can be fully realized through widespread adoption.To this end, this Account details our recent efforts to develop and apply tractable first-principles simulation approaches for studying the response of materials to electric beam-like external electric potentials applied in real space. We briefly review the concepts and capabilities in the area of atomically precise materials manipulation and review the early demonstrations of accomplishments in this area, focusing on studies using scanned convergent electron beam probes in particular. We expound upon the depth of the challenge and identify critical shortcomings of theoretical methods that have previously been employed in the simulation of beam-induced processes. We then describe the computational methods that we have generalized from the concepts and tools most commonly applied to the study of molecular photochemistry and how our adaptations of these methods can be employed to capture the relevant dynamical phenomena for beam-induced processes ranging from the initial electron scattering to the ensuing multistate reactions. Here, we contextualize these methods within the current state of the art in this area, which has historically focused primarily on the simulation of inelastic image formation in the electron microscope for the purpose of interpreting the results of quantitative electron microscopy experiments. We demonstrate that the spatial distribution of state-specific excitation rates due to the presence of an external (probe) electric charge is inhomogeneous, such that irradiation at particular locations in materials can favor specific electronic transitions (and disallow others). In addition to the potential for excited-state reaction pathways to be accessed through the initial inelastic scattering of the tightly focused electron beam from the targeted atoms, we also identify favorable conditions for the electronically nonadiabatic evolution of the highly vibrationally excited system to open complex multistate reaction pathways. Implications of the early results for understanding the mechanisms and potential routes to improved efficiency and selectivity in beam-induced reactions are discussed. We conclude with a summary of the current state of theory and modeling capabilities in this area and provide our perspective on future directions for theoretical and experimental developments that we view as crucial to advancing the use of convergent electron beams in mode-specific, atomically precise platforms for direct-write materials modifications.

36 MATERIALS SCIENCE↗