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At least 199 records · Page 11

Radiation-Induced Changes in Single Crystal Calcite and Dolomite: Mineral Analogues of Light Water Reactor, Nuclear Power Plant Concrete Aggregates

Two analogues of aggregates (calcite and dolomite) found in nuclear power plant (NPP) concrete have been neutron irradiated to fluences up to 2 × 10 20 n/cm 2 at 52 °C and 4 × 10 19 n/cm 2 at 95 °C (E > 0.1 MeV). X-ray diffraction studies showed that these aging conditions affected crystallography of both calcite and dolomite, with both showing a growth in their unit cells compared to that of the unirradiated samples. Only dolomite samples showed a continuous increase of its lattice parameters with the increase in irradiation. In calcites, the lattice growth with irradiation dissipated after a fluence of 5 × 10 18 n/cm 2 . Radiation-induced disordering of the crystal structure was observed in both materials, while a healing effect of irradiation temperature was mainly observed in calcites. Dislocation densities calculated by using XRD data also supported these observations. Insights made into the unit cells of both minerals by using Fourier synthesis showed that the Mg sites are more prone to the neutron irradiation than the Ca sites, resulting in larger radiation effects and higher disruption in the crystal structure of dolomite than that of calcite. Furthermore, other than the polycrystalline characteristics observed by using TEM, these minerals did not show complete amorphization or significant structural decomposition at the studied irradiation fluences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Elucidating the Role of Halides and Iron during Radiolysis-Driven Oxidative Etching of Gold Nanocrystals Using Liquid Cell Transmission Electron Microscopy and Pulse Radiolysis

Graphene liquid cell transmission electron microscopy (TEM) has enabled the observation of a variety of nanoscale transformations. Yet understanding the chemistry of the liquid cell solution and its impact on the observed transformations remains an important step toward translating insights from liquid cell TEM to benchtop chemistry. Gold nanocrystal etching can be used as a model system to probe the reactivity of the solution. FeCl 3 has been widely used to promote gold oxidation in bulk and liquid cell TEM studies, but the roles of the halide and iron species have not been fully elucidated. In this work, we observed the etching trajectories of gold nanocrystals in different iron halide solutions. We observed an increase in gold nanocrystal etch rate going from Cl - - to Br - - to I - -containing solutions. Furthermore, this is consistent with a mechanism in which the dominant role of halides is as complexation agents for oxidized gold species. Additionally, the mechanism through which FeCl 3 induces etching in liquid cell TEM remains unclear. Ground-state bleaching of the Fe(III) absorption band observed through pulse radiolysis indicates that iron may react with Cl 2 · - radicals to form an oxidized transient species under irradiation. Complete active space self-consistent field (CASSCF) calculations indicate that the FeCl 3 complex is oxidized to an Fe species with an OH radical ligand. Together our data indicate that an oxidized Fe species may be the active oxidant, while halides modulate the etch rate by tuning the reduction potential of gold nanocrystals.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deep learning-enabled probing of irradiation-induced defects in time-series micrographs

Modeling time-series data with convolutional neural networks (CNNs) requires building a model to learn in batches as opposed to training sequentially. Coupling CNNs with in situ or operando techniques opens the possibility of accurately segmenting dynamic reactions and mass transport phenomena to understand how materials behave under the conditions in which they are used. In this article, in situ ion irradiation transmission electron microscopy (TEM) images are used as inputs into the CNN to assess the defect generation rate, defect cluster density, and saturation of defects. We then use the output segmentation maps to correlate with conventional TEM micrographs to assess the model’s ability to detail nanoscale interactions. Next, we discuss the implications of preprocessing and hyperparameters on model variability, accuracy when expanded to other datasets, and the role of regularization when controlling model variance. Ultimately, we eliminate human bias when extrapolating physical metrics, speed up analysis time, decouple reactions that happen at 100 ms intervals, and deploy models that are both accurate and transferable to similar experiments.

Burns, Kory (ORCID:0000000158019909)↗

Solution-Based, Anion-Doping of Li 4 Ti 5 O 12 Nanoflowers for Lithium-Ion Battery Applications

Solution–based, anionic doping represents a convenient strategy with which to improve upon the conductivity of candidate anode materials such as Li 4 Ti 5 O 12 (LTO). As such, novel synthetic hydrothermally–inspired protocols have primarily been devised herein, aimed at the large–scale production of unique halogen–doped, micron–scale, three–dimensional, hierarchical LTO flower–like motifs. Although fluorine (F) doping has been explored, the use of chlorine (Cl) dopants is the primary focus here. Several experimental variables, such as dopant amount, lithium hydroxide concentration, and titanium butoxide purity, were probed and perfected. Furthermore, the Cl doping process did not damage the intrinsic LTO morphology. The analysis, based on interpreting a compilation of SEM, XRD, XPS, and TEM–EDS results, was used to determine an optimized dopant concentration of Cl. Electrochemical tests demonstrated an increased capacity via cycling of 12 % for a Cl–doped sample as compared with pristine LTO. Moreover, the Cl–doped LTO sample described in this study exhibited the highest discharge capacity yet reported at an observed rate of 2C for this material at 143mAh g –1 . Overall, these data suggest that the Cl dopant likely enhances not only the ion transport capabilities, but also the overall electrical conductivity of our as–prepared structures. Furthermore, to help explain these favorable findings, theoretical DFT calculations were used to postulate that the electronic conductivity and Li diffusion were likely improved by the presence of increased Ti 3+ ion concentration coupled with widening of the Li migration channel.

25 ENERGY STORAGE↗

Microstructural and chemical characterization of medium burnup fast reactor MOX using electron microscopy

A thorough post-irradiation examination campaign of medium burnup Sodium Fast Reactor (SFR) mixed oxide (MOX) fuel has been undertaken over the past two years to better understand the performance at intermediate burnup of this annular fuel design. Non-destructive examinations as well as destructive examinations of two pins have been recently published by the authors, providing data regarding the performance at macro-scale. The analyses of selected samples have continued to provide more details regarding the overall microstructure and, particularly, the fuel-cladding interaction.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A novel statistical methodology for quantifying the spatial arrangements of axons in peripheral nerves

A thorough understanding of the neuroanatomy of peripheral nerves is required for a better insight into their function and the development of neuromodulation tools and strategies. In biophysical modeling, it is commonly assumed that the complex spatial arrangement of myelinated and unmyelinated axons in peripheral nerves is random, however, in reality the axonal organization is inhomogeneous and anisotropic. Present quantitative neuroanatomy methods analyze peripheral nerves in terms of the number of axons and the morphometric characteristics of the axons, such as area and diameter. In this study, we employed spatial statistics and point process models to describe the spatial arrangement of axons and Sinkhorn distances to compute the similarities between these arrangements (in terms of first- and second-order statistics) in various vagus and pelvic nerve cross-sections. We utilized high-resolution transmission electron microscopy (TEM) images that have been segmented using a custom-built high-throughput deep learning system based on a highly modified U-Net architecture. Our findings show a novel and innovative approach to quantifying similarities between spatial point patterns using metrics derived from the solution to the optimal transport problem. We also present a generalizable pipeline for quantitative analysis of peripheral nerve architecture. Our data demonstrate differences between male- and female-originating samples and similarities between the pelvic and abdominal vagus nerves.

59 BASIC BIOLOGICAL SCIENCES↗

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↗

Reflecting on Planning Models: A Challenge for Verification and Validation of Planning Systems

We discuss the opportunities for autonomous sys- tems to perform reflection on their planners by adapting the models used to build plans. We first describe model-based planning systems, a form of automated planning system driven by declarative models of the planning domain. These models include descriptions of the conditions and effects of actions on the state of the world. When planning the activities of cyber-physical systems, the command and data representation of the system must be formally abstracted to the actions and states described in the planning system model. When the execution of a plan either fails or produces unexpected outcomes, the execution trace can be abstracted and compared to the predicted state according to the planning model, producing a list of discrepancies; these discrepancies can then be used to fix the model. This provides part of a reflection capability, namely, a set of well-formed problems with the domain model, the abstractions, or both. The challenge lies in the rest of the reflection capability, namely, a set of techniques for changing the models or the abstractions. We discuss these challenges and describe some of the options for addressing them

Mission Planning↗

Structural and magnetic properties of hard magnetic system Ce(Co 1 -Fe ) 4.4 Cu 0.6 (0 ≤ x ≤ 0.19)

The Ce(Co 1 -Fe ) 4.4 Cu 0.6 (0 ≤ x ≤ 0.19) is a composite, hard magnetic system that is based on the CaCu 5 -type structure (1:5). It shows both, unique magnetic and microstructural features that are essential for permanent magnets, e.g., exceptional squareness of the 2nd. quadrant of the magnetization loops and microstructural features typically needed for pinning. Samples solidified in alumina crucibles are coarse-grained and often clearly faceted and readily align in a magnetic field. X-ray, SEM, and TEM analyses show a 1:5-type single-phase material when quenched from high temperature, which, after heat treatment, transforms into a laminar coherent nanostructure through the formation of a dense array of extended intercalated regions. Furthermore, these extended intercalated regions are comprised of segments of the Ce 2 Ni 7 –type structure (2:7) which segregate into various closely related precipitates forming a nanostructure similar to the SmCo 5 - Sm 2 Co 17 composites seen in Sm-Co permanent magnets. Based on TEM and Lorentz microscopy of well-aligned single grain particles, the magnetic domains’ reversal mechanism is regulated by anisotropy fluctuations occurring along the easy direction of magnetization and strong exchange interactions between the matrix and defects (e.g.: stacking faults). Lorentz microscopy suggests the domain wall is not physically pinned by the defect, but rather is offset/deflected when it interacts with the defect. The Lorentz and magnetization data suggest that defects cause a bending of the moment away from the c axis inside the grains.

36 MATERIALS SCIENCE↗

Carbon Nanotube Activities at NASA-Johnson Space Center

Research activities on carbon nanotubes at NASA-Johnson Space Center include production, purification, characterization and their applications for human space flight. In-situ diagnostics during nanotube production by laser oven process include collection of spatial and temporal data of passive emission and laser induced fluorescence from C2, C3 and Nickel atoms in the plume. Details of the results from the "parametric study" of the pulsed laser ablation process indicate the effect of production parameters including temperature, buffer gas, flow rate, pressure, and laser fluence. Improvement of the purity by a variety of steps in the purification process is monitored by characterization techniques including SEM, TEM, Raman, UV-VIS-NIR and TGA. A recently established NASA-JSC protocol for SWCNT characterization is undergoing revision with feedback from nanotube community. Efforts at JSC over the past five years in composites have centered on structural polymednanotube systems. Recent activities broadened this focus to multifunctional materials, supercapacitors, fuel cells, regenerable CO2 absorbers, electromagnetic shielding, radiation dosimetry and thermal management systems of interest for human space flight. Preliminary tests indicate improvement of performance in most of these applications because of the large surface area as well as high electrical and thermal conductivity exhibited by SWCNTs.

Arepalli, Sivaram↗

Mechanical properties and deformation mechanisms of single crystal Mg micropillars subjected to high-strain-rate C-axis compression

Here, the mechanical properties and deformation mechanisms of single crystal magnesium under c-axis quasi-static and high-strain rate compressions are investigated through in situ scanning electron microscope (SEM) experiments and post-mortem transmission electron microscope (TEM) characterization. The findings revealed that ductility and high rates of hardening are preserved for pillars as large as 15 μm. Furthermore, rate effects result in a mild increase in flow stress with plastic deformations controlled primarily by the slip of type dislocations. Importantly and in contrast to other literature reports, plastic deformation occurs in the absence of twining. As the strain increases and plastic deformation exceeds about 4%, crystal rotation activates basal slip, <$\mathrm{a}$> type dislocations, resulting in a more rate independent flow stress. TEM observation on micropillars compressed at a strain rate of 250/s, revealed the activation of {${11}$$\bar{2}$$\bar{2}$} < $\bar{1}$$\bar{1}23$ > slip systems and high mobility of screw dislocations as major contributors to plastic strains in excess of 10% without fracture. These findings are relevant to the design of lightweight materials used in transportation systems, e.g., selection of material grain size. Moreover, the experimental data here reported provides the materials science community with a unique opportunity to validate discrete dislocation dynamics (DDD) formulations employed in multiscale design of materials.

36 MATERIALS SCIENCE↗

Creep fatigue life prediction for engine hot section materials (isotropic)

A series of high temperature strain controlled fatigue tests have been completed to study the effects of thermomechanical fatigue, multiaxial loading, reactive environments, and imposed mean stresses. The baseline alloy used in these tests was cast B1900+Hf (with and without coatings); a small number of tests of wrought INCO 718 are also included. A strong path dependence was demonstrated during the thermomechanical fatigue testing, using in-phase, out-phase, and non-proportional (elliptical and 'dogleg') strain-temperature cycles. The multiaxial tests also demonstrated cycle path to be a significant variable, using both proportional and non-proportional tension-torsion loading. Environmental screening tests were conducted in moderate pressure oxygen and purified argon; the oxygen reduced the specimen lives by two, while the argon testing produced ambiguous data. Both NiCoCrAlY overlay and diffusion aluminide coatings were evaluated under isothermal and TMF conditions; in general, the lives of the coated specimens were higher that those of uncoated specimens. Controlled mean stress TMF tests showed that small mean stress changes could change initiation lives by orders of magnitude; these results are not conservatively predicted using traditional linear damage summation rules. Microstructures were evaluated using optical, SEM and TEM methods.

Nelson, R. S.↗

Speciation mapping of the oxidation layer on aged uranium dioxide using scanning transmission x-ray spectromicroscopy

In this study, UO 2 was aged in humid air and prepared as a thin section using a focused ion beam (FIB) instrument. The specimen was measured using synchrotron radiation spectromicroscopy techniques at the Beamline 11.0.2 STXM end station of the Advanced Light Source (ALS). Non-negative matrix factorization (NMF) methods were used to identify and map three component x-ray absorption near-edge structure (XANES) spectra in the oxygen K-edge data, revealing a surface layer of U 4 O 9 with a thickness of 206 ± 21 nm, and the bulk of the sample remaining as UO 2 . Uranium N 4,5 -edge XANES spectromicroscopy supports these results. The diffusion-controlled parabolic rate constant for UO 2 oxidation to U 4 O 9 was calculated from the observed layer thickness and compared to literature values. Complementary transmission electron microscopy (TEM) was used to image the sample and identify the phases present in various regions, confirming the STXM results.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Surface interfacial analysis of simulant high level nuclear waste glass dissolved in synthetic cement solutions

Abstract The corrosion mechanisms and kinetics of a Mg-rich alkali aluminoborosilicate glass simulating UK high-level waste (CaZn28) were investigated upon dissolution in synthetic cement solutions. Dissolution varied as a function the different pH and alkali/alkaline earth content of each cement solution. High resolution microscopy and spectroscopy techniques ascertained the nature of the interface between the glass and the cement solutions. TEM-EDS revealed alkali- and alkaline earth-rich silica gels, into which K, Ca and Mg were incorporated. TEM-SAED, combined with synchrotron micro-focus XRD, identified the ubiquitous precipitation of the Mg-aluminate layered double hydroxide phase, meixnerite (Mg 6 Al 2 (OH) 18 ·4H 2 O), in addition to goethite (FeOOH) and crystalline silica. The C-S-H phase, tobermorite (Ca 5 Si 6 O 16 (OH) 2 ·4H 2 O), was identified in the most Ca-rich solution only. These data give insight to the role of alkali/alkaline earth-rich solutions in the dissolution or radioactive waste glasses, of importance to the final disposition in a geological disposal facility.

Corkhill, Claire L. (ORCID:0000000274883219)↗

SAMS Acceleration Measurements on Mir (NASA Increment 4)

During NASA Increment 4 (January to May 1997), about 5 gigabytes of acceleration data were collected by the Space Acceleration Measurements System (SAMS) onboard the Russian Space Station, Mir. The data were recorded on 28 optical disks which were returned to Earth on STS-84. During this increment, SAMS data were collected in the Priroda module to support the Mir Structural Dynamics Experiment (MiSDE), the Binary Colloidal Alloy Tests (BCAT), Angular Liquid Bridge (ALB), Candle Flames in Microgravity (CFM), Diffusion Controlled Apparatus Module (DCAM), Enhanced Dynamic Load Sensors (EDLS), Forced Flow Flame Spreading Test (FFFr), Liquid Metal Diffusion (LMD), Protein Crystal Growth in Dewar (PCG/Dewar), Queen's University Experiments in Liquid Diffusion (QUELD), and Technical Evaluation of MIM (TEM). This report points out some of the salient features of the microgravity environment to which these experiments were exposed. Also documented are mission events of interest such as the docked phase of STS-84 operations, a Progress engine bum, Soyuz vehicle docking and undocking, and Progress vehicle docking. This report presents an overview of the SAMS acceleration measurements recorded by 10 Hz and 100 Hz sensor heads. The analyses included herein complement those presented in previous summary reports prepared by the Principal Investigator Microgravity Services (PIMS) group.

DeLombard, Richard↗

SAMS Acceleration Measurements on Mir From January to May 1997 (NASA Increment 4)

During NASA Increment 4 (January to May 1997), about 5 gigabytes of acceleration data were collected by the Space Acceleration Measurements System (SAMS) onboard the Russian Space Station, Mir. The data were recorded on 28 optical disks which were returned to Earth on STS-84. During this increment, SAMS data were collected in the Priroda module to support the Mir Structural Dynamics Experiment (MiSDE), the Binary Colloidal Alloy Tests (BCAT), Angular Liquid Bridge (ALB), Candle Flames in Microgravity (CFM), Diffusion Controlled Apparatus Module (DCAM), Enhanced Dynamic Load Sensors (EDLS), Forced Flow Flame Spreading Test (FFFT), Liquid Metal Diffusion (LMD), Protein Crystal Growth in Dewar (PCG/Dewar), Queen's University Experiments in Liquid Diffusion (QUELD), and Technical Evaluation of MIM (TEM). This report points out some of the salient features of the microgravity environment to which these experiments were exposed. Also documented are mission events of interest such as the docked phase of STS-84 operations, a Progress engine burn, Soyuz vehicle docking and undocking, and Progress vehicle docking. This report presents an overview of the SAMS acceleration measurements recorded by 10 Hz and 100 Hz sensor heads. The analyses included herein complement those presented in previous summary reports prepared by the Principal Investigator Microgravity Services (PIMS) group.

DeLombard, Richard↗

Nanophase Iron Globules in Lunar Soil

Micrometeoritic impacts on lunar soils produce melt and vapor. A patina of condensed vapor is deposited on lunar grains, the melt forms agglutinitic glass. In lunar soils, agglutinitic glass and rinds of grains host submicron-sized globules of pure Fe0 (Fe-rich globules larger than 1 micron usually contain other elements such as Ni, P, and S). Observation and measurement of such small size requires either back scattered electron (BSE) imaging with a high-resolution SEM or transmitted electron imaging with a TEM. The two techniques impose different limitations on the size-range of measurements. Resolution of BSE imaging of polished thin sections or grain mounts of lunar soils is at best around 4-5nm (JEOL 6340F field-emission (FE)-SEM at JSC). Therefore, Fe0 globules below 10nm in cross-sectional diameter are not truly measured. The upper limit of a millimeter or so is not a hindrance. In fact, it is an advantage because whole grains can be observed and mapped at varying magnifications. Angstrom-scale resolution of TEM images is more than sufficient to observe and measure the smallest of Fe0 globules that are about 1nm in cross-section. Microtoming edges of lunar grains; however, puts an upper size limitation of 50nm, at best, on the wafer, which more or less limits measuring Fe0 globules up to 30nm or so. Clearly, SEM and TEM techniques complement each other in obtaining the complete range of size distribution of Fe0 globules in lunar soils. Below we describe, in brief, our method of determining the size distribution of Fe0 globules in agglutinitic glass using BSE-SEM imaging and size measurement. Although our work is incomplete, we also include a table of results obtained so far, which understandably would be refined as we collect more data.

C. L. James↗

Beyond the eutectic paradigm: nanolamellar patterns in a rapidly solidified peritectic alloy

Peritectic transformations are central to many structural alloys, yet pattern formation remains poorly understood due to complex growth dynamics and limited three-dimensional data. Here, we report an unusual two-phase microstructure in a Zn–Ag peritectic alloy subjected to rapid solidification by laser surface remelting. Synchrotron X-ray nanotomography reveals a lamellar structure of primary 𝜀-AgZn 3 and peritectic Zn with ∼700 nm spacing. Although resembling a eutectic morphology, this pattern forms without a eutectic reaction through non-steady coupled growth from the liquid. SEM and TEM-EDS confirm interface shapes and phase compositions. These findings expand the design space of peritectics for refined microstructural control.

36 MATERIALS SCIENCE↗