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Results for “microscopy analysis”

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 361 records · Page 20
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Comparison of damage and ablation dynamics of multilayer dielectric films initiated by few-cycle pulses versus longer femtosecond pulses

The importance of high intensity few- to single-cycle laser pulses for applications such as intense isolated attosecond pulse generation is constantly growing, and with the breakdown of the monochromatic approximation in field ionization models, the few-cycle pulse (FCP) interaction with solids near the damage threshold has ushered a new paradigm of nonperturbative light–matter interaction. In this Letter, we systematically study and contrast how femtosecond laser-induced damage and ablation behaviors of SiO 2 /HfO 2 -based reflective multilayer dielectric thin film systems vary between FCP and 110 fs pulses. With time-resolved surface microscopy and ex situ analysis, we show that there are distinct differences in the interaction depending on the pulse duration, specifically in the “blister” morphology formation at lower fluences (damage) as well as in the dynamics of debris formation at higher fluences (ablation).

42 ENGINEERING↗
DOE OSTI2020

A natural mutation between SARS-CoV-2 and SARS-CoV determines neutralization by a cross-reactive antibody

Epitopes that are conserved among SARS-like coronaviruses are attractive targets for design of cross-reactive vaccines and therapeutics. CR3022 is a SARS-CoV neutralizing antibody to a highly conserved epitope on the receptor binding domain (RBD) on the spike protein that is able to cross-react with SARS-CoV-2, but with lower affinity. Using x-ray crystallography, mutagenesis, and binding experiments, we illustrate that of four amino acid differences in the CR3022 epitope between SARS-CoV-2 and SARS-CoV, a single mutation P384A fully determines the affinity difference. CR3022 does not neutralize SARS-CoV-2, but the increased affinity to SARS-CoV-2 P384A mutant now enables neutralization with a similar potency to SARS-CoV. We further investigated CR3022 interaction with the SARS-CoV spike protein by negative-stain EM and cryo-EM. Three CR3022 Fabs bind per trimer with the RBD observed in different up-conformations due to considerable flexibility of the RBD. In one of these conformations, quaternary interactions are made by CR3022 to the N-terminal domain (NTD) of an adjacent subunit. Overall, this study provides insights into antigenic variation and potential cross-neutralizing epitopes on SARS-like viruses.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Nucleation, growth, and superlattice formation of nanocrystals observed in liquid cell transmission electron microscopy

This work reviews the advancements and prospects of liquid cell transmission electron microscopy (TEM) imaging and analysis methods in understanding the nucleation, growth, etching, and assembly dynamics of nanocrystals. The bonding of atoms into nanoscale crystallites produces materials with nonadditive properties unique to their size and geometry. The recent application of in situ liquid cell TEM to nanocrystal development has initiated a paradigm shift, (1) from trial-and-error synthesis to a mechanistic understanding of the “synthetic reactions” responsible for the emergence of crystallites from a disordered soup of reactive species (e.g., ions, atoms, molecules) and shape-defined growth or etching; and (2) from post-processing characterization of the nanocrystals’ superlattice assemblies to in situ imaging and mapping of the fundamental interactions and energy landscape governing their collective phase behaviors. Imaging nanocrystal formation and assembly processes on the single-particle level in solution immediately impacts many existing fields, including materials science, nanochemistry, colloidal science, biology, environmental science, electrochemistry, mineralization, soft condensed-matter physics, and device fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Materials data science using CRADLE: A distributed, data-centric approach

Abstract There is a paradigm shift towards data-centric AI, where model efficacy relies on quality, unified data. The common research analytics and data lifecycle environment (CRADLE™) is an infrastructure and framework that supports a data-centric paradigm and materials data science at scale through heterogeneous data management, elastic scaling, and accessible interfaces. We demonstrate CRADLE’s capabilities through five materials science studies: phase identification in X-ray diffraction, defect segmentation in X-ray computed tomography, polymer crystallization analysis in atomic force microscopy, feature extraction from additive manufacturing, and geospatial data fusion. CRADLE catalyzes scalable, reproducible insights to transform how data is captured, stored, and analyzed. Graphical abstract

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2022

Irradiation of Sintered Mo Disks with Presence of Organic Impurities in He Gas Flow

Argonne National Laboratory (Argonne) is assisting NorthStar Medical Technologies in the development of a domestic supply of 99 Mo. Specifically, the present study focuses on the production of 99 Mo-feed solution used by the RadioGenix™ 99m Tc generator. During the target-irradiation phase of production, impurities can potentially be introduced into the feed, and can lead to disturbance of ligand- 99m Tc complexation chemistry and contamination of the final radiopharmaceutical that directly interacts with the patient. To address this issue, Argonne performed irradiations and chemical processing to identify whether the potential contamination of He flow with hydrocarbon oil during irradiation affects the radiochemical purity of the final K 2 MoO 4 (K 2 TcO 4 ) in 5M KOH solution. To mimic the conditions of real irradiation at NorthStar, Argonne used its electron linear accelerator and Van de Graaff facilities, heated the target and oil source to >800°C, and controlled oxygen in the presence of He during irradiation. Following irradiation, scanning electron microscopy (SEM) and carbon analysis (CA) were used to detect carbon contamination on the solid targets. The radiochemical purity of the dissolved targets was studied via thin-layer paper chromatography (TLC). As a result of these experiments, small regions of the surface of some irradiated disks were found to be high in carbon, but the total carbon content was still negligible in comparison to the reference sample, which had experienced no irradiation or contact with oil. The summarized results from the SEM, CA, and TLC tests lead to the conclusion that even an excess of oil and heating during irradiation do not affect the radiochemical purity of the final product.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2023

Low-Power Nuclear Heating Tests of UN Fuel Particles in Hydrogen Environment for Nuclear Thermal Propulsion

Recently, there has been a reemergence of interest within the space-exploration community regarding nuclear thermal propulsion (NTP) for interplanetary travel. NTP, as conceptualized, is a compact propulsion source, is relatively light because there is no need for an oxidizing agent and has a very high specific impulse compared to traditional forms of propulsion. These factors would reduce first-leg orbital-rocketry costs (by the source’s low weight and volume) and decrease overall travel time for astronauts with higher transit speeds. Idaho National Laboratory was provided bare, uncoated, and tungsten-coated uranium nitride fuel particles as part of a preliminary investigation. The fuel was fabricated by BWX Technologies and irradiated at the Massachusetts Institute of Technology research reactor. X-ray computed tomography and scanning electron microscopy and associated chemical analysis techniques were performed on these particles at Idaho National Laboratory. Both coated and uncoated forms were examined in the as-fabricated and as-irradiated conditions. The tungsten coating was found to be intact following the irradiation, indicating positive attributes for performance under these low-power-irradiation conditions. The irradiation of uncoated particles resulted in nitrogen enrichment at the edge of the particle.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Rapid Oxidation of Uranium Steel Alloys: Combustion Synthesis

This project explored the use of combustion synthesis as a rapid, high-temperature method for oxidizing uranium-bearing steel alloys. Traditional laboratory-scale synthesis methods often fail to replicate the thermal and kinetic conditions experienced by real-world particulates, particularly those formed under rapid quenching or high-temperature scenarios. Combustion synthesis offers a promising alternative by enabling fast, localized heating and flexible precursor selection. A series of targeted experiments were conducted using a U 2 NiCrFe 4 alloy as the precursor. The alloy was oxidized using combustion synthesis reactions fueled by uranyl nitrate and glycine, achieving peak temperatures exceeding 1,200 °C. Postreaction analysis using scanning electron microscopy (SEM), elemental mapping, and Raman spectroscopy revealed the formation of iron-based oxides, with limited but detectable evidence of uranium oxide phases such as UO 2 . The results indicate that under the rapid reaction and cooling conditions of combustion synthesis, iron oxides form preferentially, but uranium oxide formation is kinetically limited. These findings validate combustion synthesis as a viable method for simulating the oxidation behavior of uranium steels in extreme environments and lay the groundwork for future studies aimed at enhancing uranium oxide formation through higher temperatures or modified precursor compositions.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Microstructure, Texture, and Strength Development during High-Pressure Torsion of CrMnFeCoNi High-Entropy Alloy

The equiatomic face-centered cubic high-entropy alloy CrMnFeCoNi was severely deformed at room and liquid nitrogen temperature by high-pressure torsion up to shear strains of about 170. Its microstructure was analyzed by X-ray line profile analysis and transmission electron microscopy and its texture by X-ray microdiffraction. Microhardness measurements, after severe plastic deformation, were done at room temperature. It is shown that at a shear strain of about 20, a steady state grain size of 24 nm, and a dislocation density of the order of 1016 m−2 is reached. The dislocations are mainly screw-type with low dipole character. Mechanical twinning at room temperature is replaced by a martensitic phase transformation at 77 K. The texture developed at room temperature is typical for sheared face-centered cubic nanocrystalline metals, but it is extremely weak and becomes almost random after high-pressure torsion at 77 K. The strength of the nanocrystalline material produced by high-pressure torsion at 77 K is lower than that produced at room temperature. The results are discussed in terms of different mechanisms of deformation, including dislocation generation and propagation, twinning, grain boundary sliding, and phase transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

An Experimental and Numerical Analysis of the Compression of Bimetallic Cylinders

This paper investigates the upsetting of bimetallic cylinders with an aluminum alloy center and a brass ring. The influence of the center-ring shape factor and type of assembly fit (interference and clearance), and the effect of friction on the compression force and ductile damage are comprehensively analyzed by means of a combined numerical-experimental approach. Results showed that the higher the shape factor, the lower the forces required, whereas the effect of friction is especially important for cylinders with the lowest shape factors. The type of assembly fit does not influence the compression force. The accumulated ductile damage in the compression of bimetallic cylinders is higher than in single-material cylinders, and the higher the shape factor, the lower the damage for the same amount of stroke. The highest values of damaged were found to occur at the middle plane, and typically in the ring. Results also showed that an interference fit was more favorable for preventing fracture of the ring than a clearance fit. Microstructural analysis by scanning electron microscopy revealed a good agreement with the finite element predicted distribution of ductile damage.

36 MATERIALS SCIENCE↗
DOE OSTI2021

ZrN Phase Formation, Hardening and Nitrogen Diffusion Kinetics in Plasma Nitrided Zircaloy-4

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Cost-Effective Thermomechanical Processing of Nanostructured Ferritic Alloys: Microstructure and Mechanical Properties Investigation

Nanostructured ferritic alloys (NFAs), such as oxide-dispersion strengthened (ODS) alloys, play a vital role in advanced fission and fusion reactors, offering superior properties when incorporating nanoparticles under irradiation. Despite their importance, the high cost of mass-producing NFAs through mechanical milling presents a challenge. This study delves into the microstructure-mechanical property correlations of three NFAs produced using a novel, cost-effective approach combining severe plastic deformation (SPD) with the continuous thermomechanical processing (CTMP) method. Analysis using scanning electron microscopy (SEM)-electron backscatter diffraction (EBSD) revealed nano-grain structures and phases, while scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectroscopy (EDS) quantified the size and density of Ti-N, Y-O, and Cr-O fine particles. Atom probe tomography (APT) further confirmed the absence of finer Y-O particles and characterized the chemical composition of the particles, suggesting possible nitride dispersion strengthening. Correlation of microstructure and mechanical testing results revealed that CTMP alloys, despite having lower nanoparticle densities, exhibit strength and ductility comparable to mechanically milled ODS alloys, likely due to their fine grain structure. However, higher nanoparticle densities may be necessary to prevent cavity swelling under high-temperature irradiation and helium gas production. Further enhancements in uniform nanoparticle distribution and increased sink strength are recommended to mitigate cavity swelling, advancing their suitability for nuclear applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In Situ and Post-Mortem Characterizations of Ultrasonic Spot Welded AZ31B and Coated Dual Phase 590 Steel Joints

Ultrasonic spot welding using different welding conditions was applied to join dissimilar metals of galvanized DP590 steel and AZ31B magnesium sheets. In situ high-speed imaging, digital image correlation, and infrared thermography were utilized to quantitatively study the interfacial relative motion, surface indentation, and heat generation across the joint faying interface and the sheet/sonotrode interfaces under the welding condition of moderate welding power and short welding time. For welds made with high power and long welding time, lap shear tensile tests as well as fatigue tests were carried out. Different fracture modes were observed after the lap shear tensile tests and fatigue tests performed under different peak loads. Post-weld cross-sectional analysis with scanning electron microscopy coupled with energy dispersive X-Ray spectroscopy revealed the variation of morphology and chemical composition at the joint interface for welds made with different welding conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Effect of Preparation Conditions of Fe@SiO2 Catalyst on Its Structure Using High-Pressure Activity Studies in a 3D-Printed SS Microreactor

Fischer–Tropsch synthesis (FTS) in a 3D-printed stainless steel (SS) microchannel microreactor was investigated using Fe@SiO2 catalysts. The catalysts were prepared by two different techniques: one pot (OP) and autoclave (AC). The mesoporous structure of the two catalysts, Fe@SiO2 (OP) and Fe@SiO2 (AC), ensured a large contact area between the reactants and the catalyst. They were characterized by N2 physisorption, H2 temperature-programmed reduction (H2-TPR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron microscopy (XPS), and thermogravimetric analysis–differential scanning calorimetry (TGA-DSC) techniques. The AC catalyst had a clear core–shell structure and showed a much greater surface area than that prepared by the OP method. The activities of the catalysts in terms of FTS were studied in the 200–350 °C temperature range at 20-bar pressure with a H2/CO molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher selectivity and higher CO conversion to olefins than Fe@SiO2 (OP). Stability studies of both catalysts were carried out for 30 h at 320 °C at 20 bar with a feed gas molar ratio of 2:1. The Fe@SiO2 (AC) catalyst showed higher stability and yielded consistent CO conversion compared to the Fe@SiO2 (OP) catalyst.

Biochemistry & Molecular Biology↗
DOE OSTI2025

Impact of Hydrogen Combustion on the Oxidation-induced Degradation of Heavy-duty Diesel Engine Piston Materials

High temperature ferritic-martensitic steels are candidate materials for heavy-duty diesel engine pistons. The envisioned transition to hydrogen blended fuels is expected to alter the post-combustion atmosphere in the engines, primarily resulting in a higher water vapor content (> 20 vol%) and potentially higher exhaust gas temperatures. The oxidation resistance of existing and newly developed alloys will be a critical life-limiting mechanism under these conditions. In the present work, the oxidation behavior of candidate piston alloys was evaluated in air+10 vol.% H2O and air+30 vol.% H2O at 700°C. Thermal cyclic (1h cycle) exposures were conducted for two variants of commercial UNSS42200 ferritic-martensitic steel and two developmental alloy steels for up to 300h. The developmental alloys each have similar compositions but with one containing elevated Cu levels of 3 wt.%, A significant reduction in resistance to breakaway oxidation was observed for the commercial alloys in the higher water vapor atmosphere. Microstructural characterization (optical metallography, scanning electron microscopy and electron microprobe analysis) revealed the formation of thick Fe-rich oxides even for the high Cr (~12 wt.%) steels after an initial stage of protective oxidation with MnCr-rich spinels. The impact of the evaporation-induced loss of Cr on the time and temperature dependent compositional changes in the alloys was correlated with experimental findings. For the developmental alloys, Cu additions appear to play a role in significantly reducing oxidation kinetics in air+30 vol.% H2O at 700°C.

Pillai, Rishi [ORNL] (ORCID:0000000243688197)↗
DOE OSTI2022

Micro-spectroscopic and freezing characterization of ice-nucleating particles collected in the marine boundary layer in the eastern North Atlantic

Abstract. Formation of atmospheric ice plays a crucial role in the microphysical evolution of mixed-phase and cirrus clouds and thus climate. How aerosol particles impact ice crystal formation by acting as ice-nucleating particles (INPs) is a subject of intense research activities. To improve understanding of atmospheric INPs, we examined daytime and nighttime particles collected during the Aerosol and Cloud Experiments in the Eastern North Atlantic (ACE-ENA) field campaign conducted in summer 2017. Collected particles, representative of a remote marine environment, were investigated for their propensity to serve as INPs in the immersion freezing (IMF) and deposition ice nucleation (DIN) modes. The particle population was characterized by chemical imaging techniques such as computer-controlled scanning electron microscopy with energy-dispersive X-ray analysis (CCSEM/EDX) and scanning transmission X-ray microscopy with near-edge X-ray absorption fine-structure spectroscopy (STXM/NEXAFS). Four major particle-type classes were identified where internally mixed inorganic–organic particles make up the majority of the analyzed particles. Following ice nucleation experiments, individual INPs were identified and characterized by SEM/EDX. The identified INP types belong to the major particle-type classes consisting of fresh sea salt with organics or processed sea salt containing dust and sulfur with organics. Ice nucleation experiments show IMF events at temperatures as low as 231 K, including the subsaturated regime. DIN events were observed at lower temperatures of 210 to 231 K. IMF and DIN observations were analyzed with regard to activated INP fraction, ice-nucleation active site (INAS) densities, and a water activity-based immersion freezing model (ABIFM) yielding heterogeneous ice nucleation rate coefficients. Observed IMF and DIN events of ice formation and corresponding derived freezing rates demonstrate that the marine boundary layer aerosol particles can serve as INPs under typical mixed-phase and cirrus cloud conditions. The derived IMF and DIN parameterizations allow for implementation in cloud and climate models to evaluate predictive effects of atmospheric ice crystal formation.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

UN-SiC TRISO Post Irradiation Examination Developmental Work

As part of efforts to strengthen INL?s post irradiation analysis capabilities with non-Advanced Gas Reactor (AGR) tristructural isotropic (TRISO) fuels, two developmental activities were conducted. The first activity was to determine how best to analyze uranium nitride TRISO fuel kernels using electron probe microanalysis, while the second activity focused on developing a method to deconsolidate TRISO fuel particles that have been encased in a silicon carbide matrix. Because these two activities were unrelated, they have been presented separately in this report. Initial EPMA analyses showed nitrogen contents that far exceeded the concentration expected for UN--a line compound. Further examination showed that current literature values for the mass absorption coefficient (MAC) for the N ka X-ray absorbed by U ranged from approximately 1600 to 9500, with most values tending toward 9500. Measuring UN with five different progressively increasing accelerating voltages followed by using the modeling program xMAC suggests the actual MAC is approximately 2115. Additional MAC modifications were required to produce reasonable analytical results. Because of the inaccuracies of necessary MAC coefficients, UN analysis via scanning electron microscopy (SEM) is likely to produce inaccurate results. This is because SEM software does not typically allow the user to alter MACs. Tests have been performed to examine the feasibility of an electrochemical technique to liberate irradiated TRISO fuel from a SiC matrix without damaging the outer pyrolytic carbon layer of the fuel particle. The method is performed by electrochemically exposing the SiC to magnesium metal forming Mg2Si and C. Following exposure, the small SiC samples showed slight mass increases with no evidence of conversion to Mg2Si and C nor obvious degradation of the SiC samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Machine learning-based multidomain processing for texture-based image segmentation and analysis

Atomic and molecular resolved atomic force microscopy (AFM) images offer unique insights into materials' properties such as local ordering, molecular orientation, and topological defects, which can be used to pinpoint physical and chemical interactions occurring at the surface. Utilizing machine learning for extracting underlying physical parameters increases the throughput of AFM data processing and eliminates inconsistencies intrinsic to manual image analysis, thus enabling the creation of reliable frameworks for qualitative and quantitative evaluation of experimental data. Here, we present a robust and scalable approach to the segmentation of AFM images based on flexible pre-selected classification criteria. The usage of supervised learning and feature extraction allows us to retain the consideration of specific problem-dependent features (such as types of periodical structures observed in the images and the associated numerical parameters: spacing, orientation, etc.). We highlight the applicability of this approach for the segmentation of molecular resolved AFM images based on the crystal orientation of the observed domains, automated selection of boundaries, and collection of relevant statistics. Finally, we outline a general strategy for machine learning-enabled analysis of nanoscale systems exhibiting periodic order that could be applied to any analytical imaging technique

36 MATERIALS SCIENCE↗
DOE OSTI2021

Combined effect of NaAlO2 and NaOH on the early age hydration of Portland cement with a high concentration of borate solution

The early age hydration of ordinary Portland cement in 5 M borate solution, with or without the addition of NaAlO{sub 2} and/or NaOH, was investigated. Hydration was measured using calorimetry, X-ray diffraction, thermogravimetric analysis, {sup 11}B and {sup 27}Al magic angle spinning NMR analysis, and scanning transmission electron microscopy. The purpose of this study was to reveal the mechanisms behind the retardation caused by a high concentration borate solution and the restoration of hydration through the combined addition of NaOH and NaAlO{sub 2}. Amorphous ulexite, which formed on the surface of the cement particles and prevented the further dissolution of anhydrous phases, was identified as the retardation product. The mechanism of the combined addition of NaAlO{sub 2} and NaOH in overcoming retardation was to transform amorphous ulexite into B-AFt and gowerite (CaB{sub 6}O{sub 10}·5H{sub 2}O). Formation of gowerite is favorable because of the much higher boron immobilization capacity in weight percentage, comparing to usual boron-containing phases reported previously.

36 MATERIALS SCIENCE↗