SEARCH · Engineering Papers

Results for “TEM”

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.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 937 records · Page 52

All sources NASA NTRS DOE OSTI

DOE OSTI2013

TRANSMISSION ELECTRON MICROSCOPY OF Al-RICH SILICATE STARDUST FROM ASYMPTOTIC GIANT BRANCH STARS

We report on transmission electron microscopy (TEM) investigations of two mineralogically unusual stardust silicates to constrain their circumstellar condensation conditions. Both grains were identified by high spatial resolution nano secondary ion mass spectrometry (NanoSIMS) in the Acfer 094 meteorite, one of the most pristine carbonaceous chondrites available for study. One grain is a highly crystalline, highly refractory (Fe content < 0.5 at%), structurally undisturbed orthopyroxene (MgSiO{sub 3}) with an unusually high Al content (1.8 {+-} 0.5 at%). This is the first TEM documentation of a single crystal pyroxene within the complete stardust silicate data set. We interpret the microstructure and chemistry of this grain as being a direct condensate from a gas of locally non-solar composition (i.e., with a higher-than-solar Al content and most likely also a lower-than-solar Mg/Si ratio) at (near)-equilibrium conditions. From the overabundance of crystalline olivine (six reported grains to date) compared to crystalline pyroxene (only documented as a single crystal in this work) we infer that formation of olivine over pyroxene is favored in circumstellar environments, in agreement with expectations from condensation theory and experiments. The second stardust silicate consists of an amorphous Ca-Si rich material which lacks any crystallinity based on TEM observations in which tiny (<20 nm) hibonite nanocrystallites are embedded. This complex assemblage therefore attests to the fast cooling and rapidly changing chemical environments under which dust grains in circumstellar shells form.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Characterization of the state of nanoparticle aggregation in non-equilibrium plasma synthesis systems

Non-equilibrium plasmas offer a unique environment for nanoparticle synthesis. Particles are homogeneously nucleated and grow at near room temperature as a result of non-thermal decomposition of vapor precursors by electrons and other plasma-excited species. Despite their widespread use, several features regarding particle growth in these systems remain poorly understood. In particular, particle aggregation (the formation of non-spherical entities composed of primary particles) is assumed to be negligible because of unipolar particle charging and subsequent Coulombic repulsion, which would hinder collisional growth. Here, we apply ion mobility-mass spectrometry (IM-MS) to a non-thermal, atmospheric pressure DC microplasma to study the state of aggregation of as-synthesized nanoparticles. Under all examined synthesis conditions, we find the presence of highly branched, chain-like aggregates at the reactor outlet, with a primary particle radius below 10 nm that is relatively insensitive to synthesis conditions. The aggregates are polydisperse, with mean masses and mobility diameters increasing with both increasing precursor concentration and increasing flow residence time within the system. TEM structural characterization shows that the aggregates can be described by a quasifractal model, with a fractal dimensions in the 1.6–2.0 range. The mass-mobility relationship inferred from IM-MS and TEM agrees well with Langevin dynamics simulations where coulomb interactions are not considered. We suggest that particle aggregation occurs either in the plasma volume due to the scavenging of smaller neutral or positively charged particles by growing aggregates or outside the reactor where the plasma density is lower and electrons are not available to maintain high levels of unipolar charge. Furthermore, the methods applied here additionally demonstrate the potential of IM-MS and TEM structural characterization in analyzing gas-phase nanoparticle production processes.

42 ENGINEERING↗

DOE OSTI2025

Observation and characterisation of trapped electron modes in Wendelstein 7-X

In the past, quasi coherent (QC) modes were reported for nearly all tokamaks. The general definition describes modes as QC when the magnitude squared coherence is in the range of 0.3 to 0.6. QC modes are observed in the plasma core as well as in the plasma edge and can have quite different physical origins. The one in the core are observed in plasmas with low collisionality, where the electron temperature exceeds the ion temperature in the plasma core. This is the case for electron cyclotron heating in general. The origin of these modes are electrons trapped within a magnetic mirror, as reported in the past from various fusion devices. The so-called trapped-electron modes (TEMs) belong to drift wave instabilities and can be destabilized by electron-temperature gradients in the plasma core. From the diagnostic point of view, QC modes appear as fluctuations in electron density and temperature. Therefore, the microwave reflectometer is very well suited to monitor these modes. This paper describes experiments, conducted at the Wendelstein 7-X stellarator (W7-X), which aim at detecting QC modes at low wave numbers. A poloidal correlation reflectometer installed at W7-X, is able to measure low wave numbers ($k_\perp\unicode{x2A7D}{3.5}\,\textrm{cm}^{-1}$). For medium line-averaged densities ($\int n_\textrm{e}\unicode{x2A7D}{6 \times10^{19}}\,\textrm{m}^{-2}$) the plasma core is accessible for this diagnostic. For different magnetic configurations and plasma parameters, broad QC structures are observed in the coherence spectra. From the analysis of the rotation and the poloidal structure, these QC modes show the properties of electron-temperature-gradient driven TEMs. A linear relation between the mode velocity and the rotation frequency is found. The relation is uniform and confirms the nature of QC-mode observation as TEM in tokamaks, too.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2022

Global gyrokinetic simulations of electrostatic microturbulent transport using kinetic electrons in LHD stellarator

Global gyrokinetic simulations of ion temperature gradient (ITG) and trapped electron mode (TEM) in the LHD stellarator are carried out using the gyrokinetic toroidal code (GTC) with kinetic electrons. ITG simulations show that kinetic electron effects increase the growth rate by more than 50% and more than double the turbulent transport levels compared with simulations using adiabatic electrons. Zonal flow dominates the saturation mechanism in the ITG turbulence. Nonlinear simulations of the TEM turbulence show that the main saturation mechanism is not the zonal flow but the inverse cascade of high to low toroidal harmonics. Further nonlinear simulations with various pressure profiles indicate that the ITG turbulence is more effective in driving heat conductivity whereas the TEM turbulence is more effective for particle diffusivity.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2019

Determination of nanoparticle collision cross section distribution functions in low pressure plasma synthesis reactors via ion mobility spectrometry

Low pressure (< 20 Torr) non-thermal plasma flow tube reactors are often used for the synthesis of high purity nanoparticles (NPs) via nucleation and subsequent growth from vapor phase precursors. In spite of their utility, process monitoring (i.e. output NP size characterization) in such reactors is difficult, as there is a dearth of techniques available for online nanoparticle size distribution function measurement. In this study, we developed and applied an ion mobility spectrometry (IMS) system consisting of a low pressure differential mobility analyzer (LPDMA) and electrical detector to determine the collision cross section distribution functions of Si NPs synthesized in a radiofrequency non-thermal SiH4-Ar plasma operated at ~2 Torr (266 Pa). The collision cross section, roughly proportional to projected area, is a parameter quantifying the size and structure of nanometer scale species in the vapor phase. We introduce the collision cross section distribution function as a metric for potential use in online process monitoring in NP synthesis. Proper inversion of the collision cross section distribution function requires a priori knowledge of the LPDMA transfer function. We utilized a tandem differential mobility analyzer approach, coupled with a Twomey-Markwoski based scheme to determine LPDMA transfer functions. Subsequent application of these transfer functions in collision cross section distribution function determination showed that at the outlet of the non-thermal plasma flow tube reactor, both negatively and positively charged Si NPs persisted with nearly identical collision cross section distribution functions. NPs were found to have mode “mobility equivalent” diameters near 10 nm, and via TEM analysis were found to persist at the reactor outlet as small aggregates composed of ~5 nm diameter primary particles. Size distributions functions inferred from collision cross section measurements were compared to size distribution functions inferred from TEM images; excellent agreement was found between IMS and TEM for both mean mobility equivalent diameter and distribution function width. In total, this study shows that (1) IMS is a viable approach for process monitoring in non-thermal plasma NP flow tube synthesis systems, (2) although NPs are modestly aggregated at low-pressure plasma reactor outlets, the extent of aggregation is considerably less than observed in most atmospheric pressure and equilibrium NP synthesis systems (e.g. flames), and (3) after exiting the plasma reactor, the decharging of NPs from highly negatively charge states to a bipolar charge distribution likely drives aggregation on the plasma boundary.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Towards Autonomous Experiments by Connecting High Performance Microscopy with High Performance Computing

The digitization of controls, data, and analysis in microscopy is bringing the idea of autonomous microscopes closer to reality than ever before. Automated transmission electron microscopy (TEM) is already fairly routine for some experiments the only require simple repetitive tasks such as imaging biological macromolecules for single particle cryoEM [1], tilt series for electron tomography [2], and movies for crystallography [3]. The vast majority of TEM experiments are conducted completely by human operators who choose the regions of interest, optimize experimental parameters, and make decisions about data quality visually during an experiment. The field is still a long way from having completely autonomous TEMs that can adapt to sample difficulties and tune experimental parameters based on data quality and desired experimental outcomes. Part of the issue is the lack of capability for feeding information learned from on-line, live data analysis back into the on-going experiment [4]. Furthermore, this presentation will discuss current capabilities for large scale data reduction and analysis using high performance computing (i.e. supercomputing) and progress towards developing a true feed-back loop that places data analysis and theory in the experimental loop.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2024

Generalization Across Experimental Parameters in Neural Network Analysis of High-Resolution Transmission Electron Microscopy Datasets

Neural networks are promising tools for high-throughput and accurate transmission electron microscopy (TEM) analysis of nanomaterials, but are known to generalize poorly on data that is “out-of-distribution” from their training data. Given the limited set of image features typically seen in high-resolution TEM imaging, it is unclear which images are considered out-of-distribution from others. Here, we investigate how the choice of metadata features in the training dataset influences neural network performance, focusing on the example task of nanoparticle segmentation. We train and validate neural networks across curated, experimentally collected high-resolution TEM image datasets of nanoparticles under various imaging and material parameters, including magnification, dosage, nanoparticle diameter, and nanoparticle material. Overall, we find that our neural networks are not robust across microscope parameters, but do generalize across certain sample parameters. Additionally, data preprocessing can have unintended consequences on neural network generalization. Our results highlight the need to understand how dataset features affect deployment of data-driven algorithms.

42 ENGINEERING↗

DOE OSTI2024

Three-Dimensional Ultrastructure of Arabidopsis Cotyledons Infected with Colletotrichum higginsianum

We used serial block-face scanning electron microscopy (SBF-SEM) to study the host–pathogen interface between Arabidopsis cotyledons and the hemibiotrophic fungus Colletotrichum higginsianum. By combining high-pressure freezing and freeze-substitution with SBF-SEM, followed by segmentation and reconstruction of the imaging volume using the freely accessible software IMOD, we created 3D models of the series of cytological events that occur during the Colletotrichum–Arabidopsis susceptible interaction. We found that the host cell membranes underwent massive expansion to accommodate the rapidly growing intracellular hypha. As the fungal infection proceeded from the biotrophic to the necrotrophic stage, the host cell membranes went through increasing levels of disintegration culminating in host cell death. Intriguingly, we documented autophagosomes in proximity to biotrophic hyphae using transmission electron microscopy (TEM) and a concurrent increase in autophagic flux between early to mid/late biotrophic phase of the infection process. Occasionally, we observed osmiophilic bodies in the vicinity of biotrophic hyphae using TEM only and near necrotrophic hyphae under both TEM and SBF-SEM. Overall, we established a method for obtaining serial SBF-SEM images, each with a lateral ( x-y) pixel resolution of 10 nm and an axial ( z) resolution of 40 nm, that can be reconstructed into interactive 3D models using the IMOD. Application of this method to the Colletotrichum–Arabidopsis pathosystem allowed us to more fully understand the spatial arrangement and morphological architecture of the fungal hyphae after they penetrate epidermal cells of Arabidopsis cotyledons and the cytological changes the host cell undergoes as the infection progresses toward necrotrophy. [Formula: see text] Copyright © 2024 The Author(s). This is an open access article distributed under the CC BY 4.0 International license .

Biochemistry & Molecular Biology↗

DOE OSTI2025

Interface, bulk and surface structure of heteroepitaxial altermagnetic α-MnTe films grown on GaAs(111)

Epitaxial MnTe films have recently seen a surge in research into their altermagnetic semiconducting properties. However, those properties may be extremely sensitive to structural and chemical modifications. We report a detailed investigation of the synthesis of the altermagnet α-MnTe on GaAs(111), which reveals the bulk defect structure of this material, the mechanism by which it releases strain from the underlying substrate, and the impact of oxidation on its surface. X-ray diffraction measurements show that α-MnTe layers with thicknesses spanning 45 to 640 nm acquire lattice parameters different from bulk, mostly due to thermal strain caused by the substrate rather than strain from the lattice mismatch. Through high-resolution transmission electron microscopy (TEM) measurement, we then unveil a misfit dislocation array at the interface, revealing the mechanism by which lattice strain is relaxed. TEM also reveals a stacking fault in the bulk, occurring along a glide plane parallel to the interface. The combination of TEM with polarized neutron reflectometry measurements finally reveals the impact of oxidation on the chemistry of the surface of uncapped MnTe. Furthermore, or findings highlight the subtle role of epitaxy in altering the structure of α-MnTe, providing potential opportunities to tune the altermagnetic properties of this material.

Altermagnets↗

DOE OSTI2026

Quantitative analysis of zonal flow influence on turbulent plasmas driven by trapped electrons

The role of zonal flow (ZF) in the turbulence saturation of trapped electron modes (TEM) in magnetically confined plasmas is revisited. Here, in this study, we examine ZF excitation and saturation mechanisms in TEM turbulence using detailed free-energy transfer diagnostics from nonlinear gyrokinetic simulations. When the ion channel becomes subdominant, electrons shift to transferring energy to the zonal component, which results in zonal flows always playing a significant though subdominant role, in the case of the temperature gradient driven TEM. The velocity-space structure of energy transfer reveals that trapped electrons directly couple to ZF. Regarding the saturation physics, the zonal flow advection, drift-wave–drift-wave interactions, and stable modes at the pump waves are compared. When ZF saturation is weak, drift-wave–drift-wave interactions play a larger role in maintaining turbulence saturation. The findings elucidate the roles of nonzonal to zonal flow coupling, stable modes, and nonzonal wave-wave interactions, and provide a basis for improving reduced models of turbulent transport.

Song, Jiheon [Hanyang University, Seoul (Korea, Re↗

DOE OSTI2015

Low- Z polymer sample supports for fixed-target serial femtosecond X-ray crystallography

X-ray free-electron lasers (XFELs) offer a new avenue to the structural probing of complex materials, including biomolecules. Delivery of precious sample to the XFEL beam is a key consideration, as the sample of interest must be serially replaced after each destructive pulse. The fixed-target approach to sample delivery involves depositing samples on a thin-film support and subsequent serial introduction via a translating stage. Some classes of biological materials, including two-dimensional protein crystals, must be introduced on fixed-target supports, as they require a flat surface to prevent sample wrinkling. A series of wafer and transmission electron microscopy (TEM)-style grid supports constructed of low- Z plastic have been custom-designed and produced. Aluminium TEM grid holders were engineered, capable of delivering up to 20 different conventional or plastic TEM grids using fixed-target stages available at the Linac Coherent Light Source (LCLS). As proof-of-principle, X-ray diffraction has been demonstrated from two-dimensional crystals of bacteriorhodopsin and three-dimensional crystals of anthrax toxin protective antigen mounted on these supports at the LCLS. In conclusion, the benefits and limitations of these low- Z fixed-target supports are discussed; it is the authors' belief that they represent a viable and efficient alternative to previously reported fixed-target supports for conducting diffraction studies with XFELs.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Measuring the Burgers vector of dislocations with dark-field X-ray microscopy

The subsurface dynamics of dislocations are essential to many properties of bulk crystalline materials. However, it is challenging to characterize a bulk crystal by conventional transmission electron microscopy (TEM) due to the limited penetration depth of electrons. A novel X-ray imaging technique – dark-field X-ray microscopy (DFXM) – was developed to image hierarchical dislocation structures in bulk crystals. While today's DFXM can effectively map the line structures of dislocations, it is still challenging to quantify the Burgers vectors, the key characterization governing the dislocation behaviors. Here, we extend the 'invisibility criterion' formalism from the TEM theory to the geometrical-optics model of DFXM and demonstrate the consistency between DFXM and dark-field TEM using multi-diffraction-peak imaging for a single edge dislocation. Due to the practical difficulty of multi-peak DFXM experiments, we further study how the Burgers vector effect is encoded for a single-peak DFXM experiment. Using the geometrical-optics DFXM simulation, we explore the asymmetry of rocking tilt scans at different rolling tilts and develop a new method to characterize the Burgers vector. The conclusions of this study advance our understanding of the use of DFXM in characterizing individual dislocations, enabling the connection from bulk DFXM imaging to dislocation mechanics.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Transmission electron microscopy for the evaluation and optimization of crystal growth

The crystallization of protein samples remains the most significant challenge in structure determination by X-ray crystallography. Here, the effectiveness of transmission electron microscopy (TEM) analysis to aid in the crystallization of biological macromolecules is demonstrated. It was found that the presence of well ordered lattices with higher order Bragg spots, revealed by Fourier analysis of TEM images, is a good predictor of diffraction-quality crystals. Moreover, the use of TEM allowed (i) comparison of lattice quality among crystals from different conditions in crystallization screens; (ii) the detection of crystal pathologies that could contribute to poor X-ray diffraction, including crystal lattice defects, anisotropic diffraction and crystal contamination by heavy protein aggregates and nanocrystal nuclei; (iii) the qualitative estimation of crystal solvent content to explore the effect of lattice dehydration on diffraction and (iv) the selection of high-quality crystal fragments for microseeding experiments to generate reproducibly larger sized crystals. Applications to X-ray free-electron laser (XFEL) and micro-electron diffraction (microED) experiments are also discussed.

Stevenson, Hilary P.↗

DOE OSTI2018

Transmission Electron Microscopy Studies of Transition Metal Oxides Employed as Carrier Selective Contacts in Silicon Solar Cells

The focus of this work is on the nano-scale characterization of transition metal oxides employed as carrier selective contacts in crystalline silicon (c-Si) solar cells using crosssectional transmission electron microscopy (TEM). Both electronselective (titanium dioxide, TiO 2 ) and hole-selective (molybdenum oxide, MoO x ; tungsten oxide, WO x ) contacts were investigated. High-resolution TEM (HRTEM) images were obtained with a FEI Tecnai F30 TEM.

Ali, H↗

DOE OSTI2022

Dislocation loop evolution in Kr-irradiated ThO 2

Here, the early stage of microstructural evolution of ThO 2 , under krypton irradiation at 600, 800, and 1000°C, was investigated using in situ transmission electron microscopy (TEM). Dislocation loops grew faster, whereas their number density decreased with increasing irradiation temperature. Loop density was found to decrease with ion dose. Interstitial dislocation loops, including Frank loops with Burgers vector of $\textit{a}/3\langle111\rangle$ and perfect loops with Burgers vector of $\textit{a}/2\langle110\rangle$, were determined by traditional TEM and atomic resolution–scanning TEM techniques. Atomistic and mesoscale level modeling are performed to interpret experimental observations. The migration energy barriers of defects in ThO 2 were calculated using density-functional theory. The energetics of different dislocation loop types were studied using molecular dynamics simulations. Loop density and diameter were analyzed using a kinetic rate theory model that considers stoichiometric loop evolution. This analysis reveals that loop growth is governed by the mobility of cation interstitials, whereas loop nucleation is determined by the mobility of anion defects. Lastly, a rate theory model was used to extract the diffusion coefficients of thorium interstitials, oxygen interstitials, and vacancies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Micro-CT scouting for transmission electron microscopy of human tissue specimens

Transmission electron microscopy (TEM) provides sub-nanometre-scale details in volumetric samples. Samples such as pathology tissue specimens are often stained with a metal element to enhance contrast, which makes them opaque to optical microscopes. As a result, it can be a lengthy procedure to find the region of interest inside a sample through sectioning. Here, we describe micro-CT scouting for TEM that allows noninvasive identification of regions of interest within a block sample to guide the sectioning step. In a tissue pathology study, a bench-top micro-CT scanner with 10 m resolution was used to determine the location of patches of the mucous membrane in osmium-stained human nasal scraping samples. Furthermore, once the regions of interest were located, the sample block was sectioned to expose that location, followed by ultra-thin sectioning and TEM to inspect the internal structure of the cilia of the membrane epithelial cells with nanometre resolution. This method substantially reduced the time and labour of the search process from typically 20 sections for light microscopy to three sections with no added sample preparation. Lay description Electron microscopy provides very high levels of detail in a small area, and thus the question of where to look in an opaque sample, such as a stained tissue specimen, needs to be answered by sectioning the sample in small steps and examining the sections under a light microscope, until the region of interest is found. The search process can be lengthy and labor intensive, especially for a study involving a large number of samples. Small areas of interest can be missed in the process if not enough regions are examined. We also describe a method to directly locate the region of interest within a whole sample using micro-CT imaging, bypassing the need of blindly sectioning. Micro-CT enables locating the region within 3D space; this information provides a guide for sectioning the sample to expose that precise location for high resolution electron microscopy imaging. In a human tissue specimen study, this method considerably reduced the time and labor of the search process.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2013

X-ray photoelectron spectroscopy study on the chemistry involved in tin oxide film growth during chemical vapor deposition processes

The chemistry of atmospheric pressure chemical vapor deposition (APCVD) processes is believed to be complex, and detailed reports on reaction mechanisms are scarce. Here, the authors investigated the reaction mechanism of monobutyl tinchloride (MBTC) and water during SnO{sub 2} thin film growth using x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). XPS results indicate an acid-base hydrolysis reaction mechanism, which is tested with multilayer experiments, demonstrating self-terminating growth. In-house developed TEM wafers are used to visualize nucleation during these multilayer experiments, and results are compared with TEM results of APCVD samples. Results show almost identical nucleation behavior implying that their growth mechanism is identical. Our experiments suggest that in APCVD, when using MBTC and water, SnO{sub 2} film growth occurs via a heterolytic bond splitting of the Sn-Cl bonds without the need to invoke gas-phase radical or coordination chemistry of the MBTC precursor.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Spatially resolved structural order in low-temperature liquid electrolyte

Determining the degree and the spatial extent of structural order in liquids is a grand challenge. Here, we are able to resolve the structural order in a model organic electrolyte of 1 M lithium hexafluorophosphate (LiP 6 ) dissolved in 1:1 (v/v) ethylene carbonate:diethylcarbonate by developing an integrated method of liquid-phase transmission electron microscopy (TEM), cryo-TEM operated at -30°C, four-dimensional scanning TEM, and data analysis based on deep learning. This study reveals the presence of short-range order (SRO) in the high–salt concentration domains of the liquid electrolyte from liquid phase separation at the low temperature. Molecular dynamics simulations suggest the SRO originates from the Li + - (PF 6 - ) n (n > 2) local structural order induced by high LiP 6 salt concentration.

42 ENGINEERING↗