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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 613 records · Page 34

Hindlimb Suspension as a Model to Study Ophthalmic Complications in Microgravity Status Report: Optimization of Rat Retina Flat Mounts Staining to Study Vascular Remodeling

Preliminary data from a prior tissue‐sharing experiment has suggested that early growth response protein‐1 (Egr1), a transcription factor involved in various stress responses in the vasculature, is induced in the rat retina after 14 days of hindlimb suspension (HS) and may be evidence that mechanical stress is occurring secondary to the cephalad fluid shift. This mechanical stress could cause changes in oxygenation of the retina, and the subsequent ischemia‐ or inflammation‐driven hypoxia may lead to microvascular remodeling. This microvascular remodeling process can be studied using image analysis of retinal vessels and can be then be quantified by the VESsel GENeration Analysis (VESGEN) software, a computational tool that quantifies remodeling patterns of branching vascular trees and capillary or vasculogenic networks. Our project investigates whether rodent HS is a valid model to study the effects of simulated‐weightlessness on ocular structures and their relationship with intracranial pressure (ICP). One of the hypotheses to be tested is that HS‐induced cephalad fluid shift is accompanied by vascular engorgement that produces changes in retinal oxygenation, leading to oxidative stress, hypoxia, microvascular remodeling, and cellular degeneration. We have optimized the procedure to obtain flat mounts of rat retina, staining of the endothelial lining in vasculature and acquisition of high quality images suitable for VESGEN analysis. Briefly, eyes were fixed in 4% paraformaldehyde for 24 hours and retinas were detached and then mounted flat on microscope slides. The microvascular staining was done with endothelial cell‐specific isolectin binding, coupled to Alexa‐488 fluorophore. Image acquisition at low magnification and high resolution was performed using a new Leica SP8 confocal microscope in a tile pattern across the X,Y plane and multiple sections along the Z‐axis. This new confocal microscope has the added capability of dye separation using the Linear Unmixing method and allows us to remove the autofluorescence originating from the photoreceptor layer. In summary, we have an improved method for studying the retinal microvasculature that will provide an increase in the quality of images captured and will be applied throughout the various animal cohorts of the recentlyinitiated study that will evaluate rodent HS as a model to study ophthalmic complications in microgravity.

Theriot, Corey A.↗

Analysis of Defects in Metal Additive Manufacturing with Augmented Data Generation

Laser powder bed fusion (LPBF) is a method of additive manufacturing (AM) that selectively melts and fuses together microscopic metallic powder. LPBF offers the benefit of producing custom structures out of high strength metals that can be difficult to fabricate with conventional methods. The challenge of LPBF is that 3D printed structures often have internal pores due to process flaws. Pulsed thermal tomography (PTT) is a method for reconstructing the depth profile of materials, allowing the visualization internal voids in solids. In prior work, we developed a convolutional neural network (CNN) which, having been trained on simulated 2D PTT images of subsurface elliptical defects, was able to classify the semi-major radii, semi-minor radii, and angular orientation of the best-fit ellipses in previously unseen PTT images. The unseen PTT images contained subsurface irregular defect shapes imported from scanning electron microscopy (SEM) images of metallic LPBF-printed specimens. Training the CNN on irregular defect shapes instead of on elliptical shapes would make the resulting classifications more descriptive of actual defect shapes. However, this requires a much higher volume of SEM images of material defects, which are difficult to obtain because of random occurrence of defects in LPBF. To address this challenge, we developed a generative adversarial network (GAN) to augment the existing dataset of SEM defect images. The GAN model is demonstrated to create novel yet realistic defect shapes that can be used as input for simulated PTT images to train CNN.

36 MATERIALS SCIENCE↗

X ray analysis of balloon-collected particles erroneously considered as an October influx into the lower stratosphere

Individual particles were analyzed on the collection screens in a Jeolco scanning electron microscope using a Kevex Li-drifted silicon energy dispersive X ray detector. It was found that the bulk of the stratospheric samples studied comes from explosive squib devices. It is pointed out that this finding does not invalidate the extensive results obtained by Bigg et al. (1970, 1971) in previous sampling experiments.

Farlow, N. H.↗

Microscopic ejecta measurements from hypervelocity impacts on aluminum and powdered regolith targets

Meteoroids and space debris pose a two-fold threat to spacecraft due to the risk of both mechanical damage from the impact and electrical damage from the impact-generated plasma, which produces electromagnetic emissions. Analysis of impact products, however, has the potential to provide useful information about planetary rings and small solar system bodies, such as asteroids and comets. Understanding the plasma dynamics and radiation mechanism is essential to addressing the impact threat and extracting science data from impacts. Charge attachment to condensed-phase debris may lead to a dusty plasma under certain conditions, so interpreting hypervelocity impacts requires knowledge of both the nature of the plasma and of the ejecta. We address the latter with measurements of the microscopic ejecta distribution produced by light gas gun impacts on solid aluminum and powdered regolith simulant targets. We examine both the size and shape of the ejecta using thin-film witness plates and find that the size distributions of microscopic ejecta follow power laws. Observations from the powdered regolith simulant match well with disruption experiments of solid basalt, while measurements from the aluminum impacts diverge from extrapolations based on studies of macroscopic debris. Analysis of the ejecta shape shows a transition from smooth to irregularly shaped ejecta at the material grain size, and the shape of debris may provide insight on the phase of the ejected material. Finally, based on our results, we predict a significant number of secondary impacts on plasma sensors due to ejecta, even at considerable distance from the target, supporting the hypothesis that charged dust affects plasma measurements in the ejecta curtain.

42 ENGINEERING↗

A large interlaboratory electron diffraction study of monolayer graphene

Standardisation of data collection and analysis is essential to enable commercialisation of 2D materials in a wide range of technologies. Selected area electron diffraction (SAED) in the transmission electron microscope (TEM) is one of the key methods for distinguishing monolayer from bilayer and few-layer graphene by comparing the 1st and 2nd order diffraction spot intensities. Yet there are many factors that can affect the reliability of data collection and interpretation, causing the measurement of monolayer samples to deviate from the literature boundary condition of $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1 for monolayer graphene (1LG). Here we present the results of a large interlaboratory SAED comparison study, where 15 international laboratories measured and analysed nominally identical samples of chemical vapour deposited graphene. Large variations were observed in the measured ratios of diffraction spot intensities, with the largest variance associated with poor quality SAED data resulting from inadequate specimen handling and storage. To inform the reliable determination of monolayer thickness from SAED patterns we provide a description of best practice for specimen handling, TEM operation, data collection and analysis. This work was undertaken within VAMAS Technical Working Area 41: Graphene and related 2D materials—Project 9, the results of which have been directly incorporated into ISO/TS 21356–2 for the characterisation of graphene sheets. We find that when this methodology is followed, 1LG can be distinguished from bilayer or thicker material with high confidence where analysis of a single SAED pattern gives $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1.2, even in the absence of precise specimen tilting.

2D materials↗

Probing Electron Beam Induced Transformations on a Single-Defect Level via Automated Scanning Transmission Electron Microscopy

A robust approach for real-time analysis of the scanning transmission electron microscopy (STEM) data streams, based on ensemble learning and iterative training (ELIT) of deep convolutional neural networks, is implemented on an operational microscope, enabling the exploration of the dynamics of specific atomic configurations under electron beam irradiation via an automated experiment in STEM. Combined with beam control, this approach allows studying beam effects on selected atomic groups and chemical bonds in a fully automated mode. Here, in this study, we demonstrate atomically precise engineering of single vacancy lines in transition metal dichalcogenides and the creation and identification of topological defects in graphene. The ELIT-based approach facilitates direct on-the-fly analysis of the STEM data and engenders real-time feedback schemes for probing electron beam chemistry, atomic manipulation, and atom by atom assembly.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Neutron Activation Analysis of Single Grains Recovered by the Hayabusa Spacecraft

The Hayabusa spacecraft was launched on May 9, 2003 and reached an asteroid Itokawa (25143 Itokawa) in September 2005. After accomplishing several scientific observations, the spacecraft tried to collect the surface material of Itokawa by touching down to the asteroid in November. The spacecraft was then navigated for the earth. In encountering several difficulties, Hayabusa finally returned to the earth on June 12, 2010 and the entry capsule was successfully recovered. Initially, a g-scale of solid material was aimed to be captured into the entry capsule. Although the sample collection was not perfectly performed, it was hoped that some extraterrestrial material was stored into the capsule. After careful and extensive examination, more than 1500 particles were recognized visibly by microscopes, most of which were eventually judged to be extraterrestrial, highly probably originated from Itokawa [1]. Several years before the launching of the Hayabusa spacecraft, the initial analysis team was officially formed under the selection panel at ISAS. As a member of this team, we have been preparing for the initial inspection of the returned material from many scientific viewpoints [2]. Once the recovered material had been confirmed to be much less than 1 g, a scheme for the initial analysis was updated accordingly [3]. In this study, we aim to analyze tiny single grains by instrumental neutron activation analysis (INAA). As the initial analysis is to be started in mid-January, 2011, some progress for the initial analysis using INAA is described here. Analytical procedure

Ebihara, M.↗

Mechanical Performance and Mesostructure Analysis of Proton-Irradiated Fused Filament Fabrication Acrylonitrile Butadiene Styrene Material

The use of fused filament fabrication (FFF) acrylonitrile butadiene styrene (ABS) and other thermoplastics in radiation environments is beginning to be studied as possible replacements for traditionally manufactured parts and tools. Interlayer adhesion within the mesostructure has been shown in published literature to be an integral component in the strength of FFF ABS. Research of irradiated 3D printed polymers has primarily focused on the influence of gamma irradiation on the mechanical properties of FFF ABS samples, without evaluating its impact on the mesostructure of the samples. The purpose of this paper is to understand the mechanical damage caused by proton radiation on FFF ABS samples through the evaluation of the mesostructure of the ABS samples. To achieve this objective, proton radiation at 40 MeV was applied to FFF ABS samples at radiation doses up to 1.0 MGy at a dose rate of 1 MGy/hr. Following the irradiation, tensile testing was performed on the samples. Here, the fractured surfaces of the tested samples were subsequently observed using a scanning electron microscope. The mechanical test results show an increase in the ultimate tensile strength (UTS) and a decrease in the ductility of the irradiated samples. Statistical analysis on the results shows that there is a statistically significant difference in the UTS and the ductility of unirradiated and 1.0 MGy irradiated samples and between irradiated samples and 1.0 MGy samples. In addition, the percentage elongation at break has statistically significant differences in the means between irradiated samples and 1.0 MGy samples. The UTS has statistically significant differences in the means between 0.1 MGy and 1.0 MGy. The difference in the means between the unirradiated and the 1.0 MGy samples is the most significant for both the UTS and elongation at break. The scanning electron microscopy (SEM) results indicated that interlayer adhesion improved as a function of radiation dose corresponding to the increase in tensile strength. The SEM results also showed that crazing and plastic deformation were reduced; aligning with the loss in ductility observed in the tensile tests results. The proton radiation is causing these mechanical and physical changes through two mechanisms: (1) dose rate effects on ionizing radiation-induced oxidative degradation; and (2) radiation heating effects of high energy (>1 MeV) charged particles.

electron microscopy↗

MPEX AI Digital Twins

All magnetically confined plasma fusion power plant concepts (Tokamak, Spherical Tokamak, Stellarator, Mirror, ...) must exhaust the heat and plasma from the core confinement region to the material walls. The primary channel for this exhaust is through a plasma divertor which directs plasma along open magnetic field lines to a material target. The Material Plasma Exposure eXperiment (MPEX) illustrated in Figure 1, is a high-power, steady-state linear plasma device designed to produce the plasma material interaction (PMI) conditions of the divertor of future magnetic confinement fusion power plants: energy flux 20MW/m 2 , ion fluence 1031/m 2 , pulse duration 106 sec. These goals of plasma exposure in MPEX are well beyond those achieved in magnetic fusion experimental devices. Successfully achieving these high power steady state conditions for long pulses requires operational control of the heating and particle sources and the plasma flux to the walls and target. The MPEX AI Hot Spot Controller, proposed in this project, will help achieve the operational milestones of MPEX. The MPEX device will begin commissioning at the end of FY26. A smaller proto-MPEX was operated for 14,666 plasma discharges and will resume operation in September of 2025 as proto-MPEX-lite, with reduced capability, to test a new window for the Helicon plasma source. The proto-MPEX data has undergone surrogate modeling with machine learning methods (R. Archibald, 2022 IEEE International Conference on Big Data). This proto-MPEX data will be used to begin development of the AI digital twins described in this white paper. The scientific mission of MPEX is to qualify materials of different composition for use in the high energy and plasma flux conditions of a fusion power plant. The materials exposed in MPEX will in some cases be exposed to high neutron fluxes at other ORNL facilities to measure the changes to their PMI properties. The targets exposed in MPEX will be transported under vacuum to a Surface Analysis Station (SAS). The SAS will be equipped with the following diagnostics: Focused Ion Beam (FIB) for trench milling, 100-400 angstrom resolution scanning electron microscope (SEM), surface mapping x-ray spectrometer, high resolution camera, and a future upgrade to a laser induced breakdown spectroscopy quadruple mass spectrometer (LIBS-QMS). The MPEX experiments will generate diverse pre- and post-exposure measurement data of detailed material properties down to the crystal grain level in 3D for post-exposure assessment of PMI damage (e.g. cracking, melting, erosion and redeposition of the material). Physics models for the PMI, and how the material composition and manufacturing impact its performance under high energy plasma exposure, need to be validated with MPEX data to guide the selection of new candidate materials. Our vision for the MPEX AI Digital Twins project is to supply experimental and physics model simulation data to train Artificial Intelligence (AI) models for data processing, analysis, operational control, PMI and materials simulation to maximize the scientific output of the MPEX device. Ultimately, an AI digital twin of MPEX material assessment metrics for tested and synthetic material types with simulated PMI will be trained by the AI Modeling Teams on the experimental and physics simulation data submitted to the American Science Cloud by this project. A purely empirical search for the best material is inefficient given the finite number of samples that can be tested on MPEX. In order to expand the material properties database for training the MPEX Material Assessment AI Digital Twin, and to gain physics understanding of the PMI processes, physics models of the material properties and PMI processes are required. The physics simulations provide detailed simulation data, like impact angles for plasma ions, sputtering yields, transport of the ionized sputtered target material in the plasma, and redeposition locations. This simulation data expands the measurement data for deeper physics understanding. The experimental data is essential to validate the PMI and material structure simulation models. The validated models can then be used to generate new simulation data of MPEX material assessments for synthetic material compositions that have not been exposed in MPEX. These predictive simulations, plus the whole experimental dataset, will be used to train the MPEX Material Assessment AI Digital Twin allowing a rapid generative AI search for new materials with reduced PMI damage by interpolating the domain of the training set. These new optimum materials can be simulated with the physics codes and/or tested in MPEX. The ability of AI neural networks to interpolate multi-dimensional parameter spaces and generate virtual data is exploited for a more efficient search for optimum materials. The advent of the Transformational AI Models Consortium (TAIMC) is an opportunity to engage with state of the art private and public AI developers to achieve the goals of the AI digital twins and AI accelerated physics models proposed in this project. Our partners at ORNL from the Advance Scientific Computing Research (ASCR) organization will collaborate in accelerating the integrated plasma material interaction simulation framework. This simulation framework will provide a platform for generating simulation data across a range of physical fidelities, including hybrid methods that produce multi-fidelity results. This data will be leveraged for AI model development, both for generation of surrogates and the automation of simulation campaigns. A part of the research below will include collaborative efforts with the TAIMC to (i) adapt data storage approaches to ensure AI-readiness, (ii) provide a protypical exemplar to inform and exercise constructed workflows, and (iii) generate and share data, using the TAIMC unified AI data standard, for foundational models that will be trained from multiple sources across the DOE complex. We will also collaborate with the TAIMC, as well as the planned AI modeling teams, to develop approaches for reducing the cost of data generation. These include tailored multi-fidelity approaches as well as fine-tuning strategies to augment general, large-scale foundational models.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Parameters, Properties, and Process: Conditional Neural Generation of Realistic SEM Imagery Toward ML-Assisted Advanced Manufacturing

Abstract The research and development cycle of advanced manufacturing processes traditionally requires a large investment of time and resources. Experiments can be expensive and are hence conducted on relatively small scales. This poses problems for typically data-hungry machine learning tools which could otherwise expedite the development cycle. We build upon prior work by applying conditional generative adversarial networks (GANs) to scanning electron microscope (SEM) imagery from an emerging advanced manufacturing process, shear-assisted processing and extrusion (ShAPE). We generate realistic images conditioned on temper and either experimental parameters or material properties. In doing so, we are able to integrate machine learning into the development cycle, by allowing a user to immediately visualize the microstructure that would arise from particular process parameters or properties. This work forms a technical backbone for a fundamentally new approach for understanding manufacturing processes in the absence of first-principle models. By characterizing microstructure from a topological perspective, we are able to evaluate our models’ ability to capture the breadth and diversity of experimental scanning electron microscope (SEM) samples. Our method is successful in capturing the visual and general microstructural features arising from the considered process, with analysis highlighting directions to further improve the topological realism of our synthetic imagery.

36 MATERIALS SCIENCE↗

Direct Air Capture of CO 2 via Reactive Crystallization

Atmospheric CO 2 removal using engineered chemical processes, aka direct air capture (DAC), has become an essential component of our available portfolio for mitigating climate change. Here we describe a promising approach to DAC based on reactive crystallization of atmospheric CO 2 (RC-DAC) with aqueous guanidine and amino acid. Compared to the previously studied phase-changing DAC processes involving initial CO 2 absorption by an aqueous alkaline solvent followed by carbonate crystallization in a second step, RC-DAC combines the CO 2 absorption and carbonate crystallization into a single step. Thus, as the insoluble carbonate salts are removed from solution by crystallization, more CO 2 is pulled from the air into solution, further driving the DAC process. The RC-DAC was performed in a household humidifier as the air–liquid contactor, which can handle solid–liquid slurries effectively. The crystallization was monitored in situ by pH measurements, real-time imaging with a microscope probe, and by Raman spectroscopy, and ex situ by NMR spectroscopy, powder X-ray diffraction, and total inorganic carbonate analysis. Further, the investigation provided a detailed mechanistic picture of the RC-DAC process, involving formation of carbamate and carbonate anions in solution, followed by sequential crystallization of different guanidinium carbonate phases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Collinear ferromagnetism with reduced moment length in kagome magnet Nd 3 ⁢Ru 4 ⁢Al 12

Here, we determine the magnetic ground state of the kagome lattice magnet Nd 3 ⁢Ru 4⁢ Al 12 by single-crystal neutron diffraction, supported by experiments with polarized neutrons. We identify this material as a collinear ferromagnet (“hex-FM”) with uniform moment length and ordering vector 𝑸 = 0, in contrast to a previous, seminal report that proposed unequal moment lengths on two Nd sites, here called the “ortho-FM” state. Our analysis of the flipping ratio in polarized neutron scattering is consistent with the hex-FM state. The results provide a microscopic basis for understanding the large fluctuation-induced Hall and Nernst responses near 𝑇 C ≈ 41K, as previously reported for Nd 3 ⁢Ru 4 ⁢Al 12 .

RKKY interaction↗

Crystal growth from the vapour phase (ASTP experiment MA-085)

The positive effects of microgravity on crystal quality and fundamental properties of the vapor transport reaction were established by analyzing the results of three transport experiments on multi-component systems performed during the Apollo Soyuz Test Project (ASTP) mission. The systems employed were GeSe(0.99)Te(0.01) - GeI4 (A), GeS(0.98)Se(0.02) - GeCl4 (B), and GeS - GeCl4-Ar (C). The crystallographic analysis is based on a direct comparison of space and ground-based (prototype) crystals, employing X-ray diffraction, microprobe, microscopic, and chemical etching techniques. The results demonstrate a considerable improvement of the space-grown crystals in terms of chemical and crystalline homogeneity, surface morphology, and bulk perfection relative to ground specimens. The confirmation of greater mass transport rates than predicted for micro-gravity by present vapor transport models is of basic scientific and practical importance for the improvement of transport models and techniques on earth and for the development of a transport model for space conditions. The internal consistency and agreement between ASTP and Skylab results obtained for different compounds, transport agents, and temperature gradients strongly support the validity of these observations. The combined findings of improved crystal quality and high mass transport rates are of technological significance for space-processing applications.

Wiedemeier, H.↗

Crystal growth from the vapor phase. Experiment MA-085

The positive effects of microgravity on crystal quality and the fundamental properties of the vapor transport reaction were established by analyzing the results of three transport experiments on multicomponent systems performed during the Apollo-Soyuz Test Project mission. The systems employed were GeSe0.99Te0.01-GeI4(A), GeS0.98Se0.02-GeCl4(B), and GeS-GeCl4-Ar (C). The crystallographic analysis is based on a direct comparison of space and ground-based (prototype) crystals employing X-ray diffraction, microprobe, microscopic, and chemical etching techniques. The results demonstrate a considerable improvement of the space-grown crystals in terms of chemical and crystalline homogeneity, surface morphology, and bulk perfection relative to ground specimens.

Wiedemeier, H.↗

Characterization of the adsorption of water vapor and chlorine on microcrystalline silica

The characterization of water adsorption on silica is necessary to an understanding of how hydrogen chloride interacts with silica. The adsorption as a function of outgas temperatures of silica and as a function of the isotherm temperature was studied. Characterization of the silica structure by infrared analysis, X-ray diffraction and differential scanning calorimetry, surface area determinations, characterization of the sample surface by electron spectroscopy for chemical analysis (ESCA), and determinations of the heat of immersion in water of silica were investigated. The silica with a scanning electron microscope was examined.

Skiles, J. A.↗

Integrated material-surface analyzer

These 10 surface-analysis tests can be run without breaking vacuum: secondary-ion mass spectroscopy, ion-scattering spectroscopy, electron-stimulated desorption, residual-gas analysis, auger electron spectroscopy, x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, characteristic-electron energy-loss spectroscopy, scanning electron microscope, scanning low-energy electron probe. Quadruple mass spectrometer, used in first 4 tests, serves as electron transfer lens in last 6 tests.

Grunthaner, F. J.↗

Lunar sample analysis

Recent results on the antarctic meteorite ALPHA 77003 which contribute to understanding the alteration processes which produced matrix in unequilibrated chondrites are presented. Also included are additional scanning electron microscope results confirming that the matrix in Allende was formed by in situ alteration.

Housley, R. M.↗

Meteoritic ablation and fusion spherules in Antarctic ice

In the course of two Antarctic expeditions in 1980/1981 and 1982/1983 approximately 4 metric tons of documented ice samples were collected from the Atka Bay Ice Shelf, Antarctica, and subsequently shipped for cosmic dust studies. After filtration of the melt water, approximately 700 Antarctic spherules (AAS) in the size range of 5 to 500 microns were handpicked from the filter residue under optical microscopes. For the chemical investigation of single dust grains the following techniques were applied: scanning electron microscopy (SEM), X-ray analysis (EDAX), instrumental neutron activation analysis (INAA), laser microprobe mass analysis (LAMMA), and accelerator mass spectroscopy (AMS). For more than 95% of the total mass the bulk and trace elements were determined in single grain analyses using EDAX, INAA, and LAMMA. The element pattern of the dust particles was compared with that of typical terrestrial material and meteoritic matter. The majority of the spherules exhibited elemental compositions compatible with meteoritic element patterns.

Thiel, K.↗