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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 109 records · Page 6

Scanning Electron Microscopy Analysis of Fuel/Matrix Interaction Layers in Highly-Irradiated U–Mo Dispersion Fuel Plates with Al and Al–Si Alloy Matrices

In order to investigate how the microstructure of fuel/matrix-interaction (FMI) layers change during irradiation, different U–7Mo dispersion fuel plates have been irradiated to high fission density and then characterized using scanning electron microscopy (SEM). Specifially, samples from irradiated U–7Mo dispersion fuel elements with pure Al, Al–2Si and AA4043 (~4.5 wt.%Si) matrices were SEM characterized using polished samples and samples that were prepared with a focused ion beam (FIB). Features not observable for the polished samples could be captured in SEM images taken of the FIB samples. For the Al matrix sample, a relatively large FMI layer develops, with enrichment of Xe at the FMI layer/Al matrix interface and evidence of debonding. Overall, a significant penetration of Si from the FMI layer into the U–7Mo fuel was observed for samples with Si in the Al matrix, which resulted in a change of the size (larger) and shape (round) of the fission-gas bubbles. Additionally, solid-fission-product phases were observed to nucleate and grow within these bubbles. These changes in the localized regions of the microstructure of the U–7Mo may contribute to changes observed in the macroscopic swelling of fuel plates with Al–Si matrices.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A comparison of carbon impurities in pre- and post-melt uranium Part 1: Scanning electron microscopy analysis

Although C impurities in U have been studied for decades, fundamental questions regarding their incorporation, migration, and overall transformation during metal processing still exist. In two written Parts, we compare the chemical speciation, distribution, crystallography, and morphologies (size, shape, etc.) of carbon-containing impurities in U metal both before and after melting using high resolution analytical electron microscopy (AEM). This first Part demonstrates the variability of carbide inclusions in depleted U (DU) metal with respect to their chemical phases and morphologies as observed by scanning electron microscopy (SEM). Here, a variety of inclusion types, such as the pill-shaped U monocarbide (UC), previously only hypothesized, are summarized. Additionally, delineation between hopper-shaped U carbonitride U(C,N) and dendritic UC inclusions is discussed in relationship to archived literature.

36 MATERIALS SCIENCE↗

Real-time 3D analysis during electron tomography using tomviz

The demand for high-throughput electron tomography is rapidly increasing in biological and material sciences. However, this 3D imaging technique is computationally bottlenecked by alignment and reconstruction which runs from hours to days. We demonstrate real-time tomography with dynamic 3D tomographic visualization to enable rapid interpretation of specimen structure immediately as data is collected on an electron microscope. Using geometrically complex chiral nanoparticles, we show volumetric interpretation can begin in less than 10 minutes and a high-quality tomogram is available within 30 minutes. Real-time tomography is integrated into tomviz, an open-source and cross-platform 3D data analysis tool that contains intuitive graphical user interfaces (GUI), to enable any scientist to characterize biological and material structure in 3D.

36 MATERIALS SCIENCE↗

Can molecular projected density of states (PDOS) be systematically used in electronic conductance analysis?

Using benzenediamine and benzenedithiol molecular junctions as benchmarks, we investigate the widespread analysis of the quantum transport conductance in terms of the projected density of states (PDOS) onto molecular orbitals (MOs). We first consider two different methods for identifying the relevant MOs: (1) diagonalization of the Hamiltonian of the isolated molecule and (2) diagonalization of a submatrix of the junction Hamiltonian constructed by considering only basis elements localized on the molecule. We find that these two methods can lead to substantially different MOs and hence PDOS. Furthermore, within Method 1, the PDOS can differ depending on the isolated molecule chosen to represent the molecular junction (e.g., with or without dangling bonds); within Method 2, the PDOS depends on the chosen basis set. We show that these differences can be critical when the PDOS is used to provide a physical interpretation of the conductance (especially when its value is small, as it happens typically at zero bias). In this work, we propose a new approach in an attempt to reconcile the two traditional methods. Although some improvements were achieved, the main problems remain unsolved. Our results raise more general questions and doubts on a PDOS-based analysis of the conductance.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

The use of analytical surface tools in the fundamental study of wear

Various techniques and surface tools available for the study of the atomic nature of the wear of materials are reviewed These include chemical etching, x-ray diffraction, electron diffraction, scanning electron microscopy, low-energy electron diffraction, Auger emission spectroscopy analysis, electron spectroscopy for chemical analysis, field ion microscopy, and the atom probe. Properties of the surface and wear surface regions which affect wear, such as surface energy, crystal structure, crystallographic orientation, mode of dislocation behavior, and cohesive binding, are discussed. A number of mechanisms involved in the generation of wear particles are identified with the aid of the aforementioned tools.

Buckley, D. H.↗

The use of analytical surface tools in the fundamental study of wear

This paper reviews the various techniques and surface tools available for the study of the atomic nature of the wear of materials. These include chemical etching, X-ray diffraction, electron diffraction, scanning electron microscopy, low-energy electron diffraction, Auger emission spectroscopy analysis, electron spectroscopy for chemical analysis, field ion microscopy, and the atom probe. Properties of the surface and wear surface regions which effect wear such as surface energy, crystal structure, crystallographic orientation, mode of dislocation behavior, and cohesive binding are discussed. A number of mechanisms involved in the generation of wear particles are identified with the aid of the aforementioned tools.

Buckley, D. H.↗

Creating ground truth for nanocrystal morphology: a fully automated pipeline for unbiased transmission electron microscopy analysis

Control over colloidal nanocrystal morphology (size, size distribution, and shape) is important for tailoring the functionality of individual nanocrystals and their ensemble behavior. Despite this, traditional methods to quantify nanocrystal morphology are laborious. New developments in automated morphology classification will accelerate these analyses but the assessment of machine learning models is limited by human accuracy for ground truth, causing even unsupervised machine learning models to have inherent bias. Herein, we introduce synthetic image rendering to solve the ground truth problem of nanocrystal morphology classification. By simulating 2D images of nanocrystal shapes via a function of high-dimensional parameter space, we trained a convolutional neural network to link unique morphologies to their simulated parameters, defining nanocrystal morphology quantitatively rather than qualitatively. An automated pipeline then processes, quantitatively defines, and classifies nanocrystal morphology from experimental transmission electron microscopy (TEM) images. Using improved computer vision techniques, 42,650 nanocrystals were identified, assessed, and labeled with quantitative parameters, offering a 600-fold improvement in efficiency over best-practice manual measurements. Further, a classification algorithm was trained with a prediction accuracy of 99.5%, which can successfully analyze a range of concave, convex, and irregular nanocrystal shapes. The resulting pipeline was applied to differentiating two syntheses of nominally cuboidal CsPbBr 3 nanocrystals and uniquely classifying binary nickel sulfide nanocrystal phase based on morphology. This pipeline provides a simple, efficient, and unbiased method to quantify nanocrystal morphology and represents a practical route to construct large datasets with an absolute ground truth for training unbiased morphology-based machine learning algorithms.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Comprehensive Study of Hydrated IDPs: X-Ray Diffraction, IR Spectroscopy and Electron Microscopic Analysis

Chondritic hydrated interplanetary dust particles (IDPs) comprise up to 50% of all IDPs collected in the stratosphere(1). Although much is known about the mineralogy, chemistry and carbon abundance of hydrated IDPs (2-4) controversies still exist regarding their formation, history, and relationship to other primitive solar system materials. Hydrated IDPs are generally believed to be derived from asteroidal sources that have undergone some degree of aqueous alteration. However, the high C contents of hydrated IDPs (by 2 to 6X CI levels (3,4) indicate that they are probably not derived from the same parent bodies sampled by the known chondritic meteorites. We report the comprehensive study of individual hydrated IDPs. The strong depletion in Ca (I) has been used as a diagnostic feature of hydrated IDPs. The particles are embedded in elemental sulfur or low viscosity epoxy and ultramicrotomed thin sections are observed using a transmission electron microscope (TEM) equipped with an energy-dispersive X-ray detector (EDX) followed by other measurements including: 1) FTIR microspectroscopy to understand the significant constraints on the organic functionality and the nature of the C-bearing phases and 2) powder X-ray difiaction using a synchrotron X-ray source to understand the bulk mineralogy of the particles.

Nakamura, K.↗

Structural and Mechanistic Analysis through Electronic Spectra: Aqueous Hyponitrite Radical (N2O2-) and Nitrosyl Hyponitrite Anion (N3O3-)

Aqueous hyponitrite radical (N{sub 2}O{sub 2}{sup -}) and nitrosyl hyponitrite anion (N{sub 3}O{sub 3}{sup -}) species are important intermediates in the reductive chemistry of NO. The structures and absorption spectra of various hydrated isomers of these compounds were investigated in this work using high-level quantum mechanical calculations combined with the explicit classical description of the aqueous environment. For N{sub 2}O{sub 2}{sup -}, comparison of the calculated spectra and energetics with the experimental data reveals that: (1) upon the one-electron oxidation of trans-hyponitrite (ON=NO{sub 2}{sup -}), the trans configuration of the resulting ON=NO{sup -} radical is preserved; (2) although cis- and trans-ON=NO{sup -} are energetically nearly equivalent, the barrier for the trans-cis isomerization is prohibitively high due to the partial double character of the NN bond; (3) the UV spectrum of ON=NO{sup -} was misinterpreted in the earlier pulse radiolysis work and its more recent revision has been justified. For the N{sub 3}O{sub 3}{sup -} ion, the symmetric isomer is the dominant observable species, and the asymmetric isomer contributes little to the experimental spectrum. Coherent analysis of the calculated and experimental data suggests a re-interpretation of the N{sub 2}O{sub 2}{sup -} + NO reaction mechanism, according to which the reaction evenly bifurcates to yield both the symmetric and asymmetric isomers of N{sub 3}O{sub 3}{sup -}. While the latter isomer rapidly decomposes to the final NO{sub 2}{sup -} + N{sub 2}O products, the former isomer is stable toward this decomposition but its formation is reversible with the homolysis equilibrium constant Khom = 2.2 - 10{sup -7} M. Collectively, these results demonstrate that advanced theoretical modeling can be of significant benefit in structural and mechanistic analysis of UV spectra.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electron Beam Analysis of Micrometeoroids Captured in Aerogel as Stardust Analogues

In January 2004, NASA s Stardust spacecraft passed through the tail of Comet 81P/Wild-2. The on-board dust flux monitor instrument indicated that numerous micro- and nano-meter sized cometary dust particles were captured by the dedicated silica aerogel capture cell. The collected cometary particles will be returned to Earth in January 2006. Current Stardust analogues are: (i) Light-gas-gun accelerated individual mineral grains and carbonaceous meteoritic material in aerogels at the Stardust encounter velocity ca.approximately 6 kilometers per second. (ii) Aerogels exposed in low-Earth orbit (LEO) containing preserved cosmic dust grains. Studies of these impacts offer insight into the potential state of the captured cometary dust by Stardust and the suitability of various analytical techniques. A number of papers have discussed the application of sophisticated synchrotron analytical techniques to analyze Stardust particles. Yet much of the understanding gained on the composition and mineralogy of interplanetary dust particles (IDPs) has come from electron microscopy studies. Here we discuss the application of scanning electron microscopy (SEM) for Stardust during the preliminary phase of post-return investigations.

Graham, G. A.↗

Strain Field Analysis in Electronic Components by ESPI: Bad Thermal Contact and Damage Evaluation

Designing electronic components and devices is a complex task that must include also considerations about thermo-mechanical behavior of the component itself. This aspect, in fact, can affect the reliability of the device as a consequence of the thermal stresses that are introduced in the component while it is working. Stress concentration can arise, in fact, due to different thermal expansion coefficients of the materials involved. Determining the thermo-mechanical response by numerically methods is not simple and not always possible so that experimental methods are preferable. In this paper, specifically, the electronic speckle pattern interferometry technique was adopted to measure full-field strain of the component during exercise. By using an optical technique it is possible to get information about the behavior of the component without being in contact with the component itself so that the dissipation coefficient is not altered. The system was able to detect gradients of deformation in the component itself connected to the different distribution of internal current in the component. Moreover, it was observed, that the presence of bad thermal contact between the package and the heat sink can be revealed because it results in a different thermos-mechanical behavior of the component. Finally, a critical defect was introduced in the component and it was observed the way the presence of damage affects the in-plane displacement of the component. Very huge differences were observed leading to the consideration that this kind of approach could be conveniently adopted also as a damage detection tool.

42 ENGINEERING↗

Visualizing quantum phenomena at complex oxide interfaces: An atomic view from scanning transmission electron microscopy

Complex oxide interfaces have been one of the central focuses in condensed matter physics and material science. Over the past decade, aberration corrected scanning transmission electron microscopy and spectroscopy has proven to be invaluable to visualize and understand the emerging quantum phenomena at an interface. In this paper, we briefly review some recent progress in the utilization of electron microscopy to probe interfaces. Furthermore, we discuss several important challenges for electron microscopy to advance our understanding on interface phenomena, from the perspective of variable temperature, magnetism, electron energy loss spectroscopy analysis, electronic symmetry, and defects probing.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗