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At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
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 Characterization of the Effect of Twin-Microstructure Interactions on {$1 0 \bar{1} 2$} Tension and {$1 0\bar {1} 1$} Contraction Twin Nucleation, Growth and Damage in Magnesium

Through in situ electron backscatter diffraction (EBSD) experiments, this paper uncovers dominant damage mechanisms in traditional magnesium alloys exhibiting deformation twinning. The findings emphasize the level of deleterious strain incompatibility induced by twin interaction with other deformation modes and microstructural defects. A double fiber obtained by plane-strain extrusion as a starting texture of AM30 magnesium alloy offered the opportunity to track deformation by EBSD in neighboring grains where some undergo profuse {$1 0\bar {1} 2$} twinning and others do not. For a tensile loading applied along extrusion transverse (ET) direction, those experiencing profuse twinning reveal a major effect of grain boundaries on non-Schmid behavior affecting twin variant selection and growth. Similarly, a neighboring grain, with its $\langle$c$\rangle$-axis oriented nearly perpendicular to tensile loading, showed an abnormally early nucleation of {$1 0\bar {1} 1$} contraction twins (2% strain) while the same {$1 0\bar {1} 1$} twin mode triggering under $\langle$c$\rangle$-axis uniaxial compression have higher value of critical resolved shear stress exceeding the values for pyramidal $\langle$c + a$\rangle$ dislocations. The difference in nucleation behavior of contraction vs. compression {$1 0\bar {1} 1$} twins is attributed to the hydrostatic stresses that promote the required atomic shuffles at the core of twinning disconnections.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanoindentation Investigation of Chloride-Induced Stress Corrosion Crack Propagation in an Austenitic Stainless Steel Weld

Transgranular chloride-induced stress corrosion cracking (TGCISCC) is a mounting concern for the safety and longevity of arc welds on austenitic stainless steel (AuSS) nuclear waste storage canisters. Recent studies have shown the key role of crystallography in the susceptibility and propagation of TGCISCC in SS weldments. Given that crystallography underlies mechanical heterogeneities, the mechanical-crystallographic relationship during TGCISCC growth must be understood. In this study, welded SS 304L coupons are loaded in four-point bend fixtures and then boiled in magnesium chloride to initiate TGCISCC. Nanoindentation mapping is paired with scanning electron microscopy (SEM) electron backscatter diffraction (EBSD) to understand the correlation between grain orientation, grain boundaries, and hardening from TGCISCC propagation. The nanoindentation hardness of individual grains is found to not be a controlling factor for TGCISCC propagation. However, intragranular hardness is generally highest immediately around the crack due to localized strain hardening at the crack tip. This work shows that nanoindentation techniques can be useful in understanding CISCC behaviors when paired with electron microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Transformation of TiN to TiNO Films via In-Situ Temperature-Dependent Oxygen Diffusion Process and Their Electrochemical Behavior

Titanium oxynitride (TiNO) thin films represent a multifaceted material system applicable in diverse fields, including energy storage, solar cells, sensors, protective coatings, and electrocatalysis. This study reports the synthesis of TiNO thin films grown at different substrate temperatures using pulsed laser deposition. A comprehensive structural investigation was conducted by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Non-Rutherford backscattering spectrometry (N-RBS), and X-ray absorption spectroscopy (XAS), which facilitated a detailed analysis that determined the phase, composition, and crystallinity of the films. Structural control was achieved via temperature-dependent oxygen in-diffusion, nitrogen out-diffusion, and the nucleation growth process related to adatom mobility. The XPS analysis indicates that the TiNO films consist of heterogeneous mixtures of TiN, TiNO, and TiO2 phases with temperature-dependent relative abundances. The correlation between the structure and electrochemical behavior of the thin films was examined. The TiNO films with relatively higher N/O ratio, meaning less oxidized, were more electrochemically active than the films with lower N/O ratio, i.e., more oxidized films. Films with higher oxidation levels demonstrated enhanced crystallinity and greater stability under electrochemical polarization. These findings demonstrate the importance of substrate temperature control in tailoring the properties of TiNO film, which is a fundamental part of designing and optimizing an efficient electrode material.

Cherono, Sheilah↗
DOE OSTI2025

Tensile Performance Sensitivity to Variations of Standard 17-4 PH Heat Treatments on LPBF-Produced Material

Standard heat treatments for metals of a particular composition are typically designed with the assumption of a conventional starting microstructure, such as that produced by casting or wrought processing. When applied to metals fabricated by Laser Powder Bed Fusion (LPBF) metal additive manufacturing (AM), these heat treatments can produce inconsistent performance due to the unique as-built microstructures. This study investigates how modifications to standard heat treatments for 17-4 PH steel influence the microstructure and mechanical properties of LPBF-fabricated material. Specimens were produced and subjected to varying solutionizing and homogenizing treatments followed by standard aging treatments. Microstructures were characterized using optical microscopy, Electron Backscatter Diffraction (EBSD), and X-ray diffraction (XRD), and mechanical properties were evaluated through uniaxial tensile testing. Based on these results, recommendations are provided for achieving improved wrought-like performance in LPBF 17-4 PH steel.

17-4 PH↗
DOE OSTI2021

Retaining Geochemical Signatures during Aragonite-Calcite Transformation at Hydrothermal Conditions

Transformation of aragonite, a mineral phase metastable at Earth’s surface, to calcite widely occurs in both sedimentary and metamorphic systems with the presence of an aqueous phase. The transformation process can affect geochemical signatures of aragonite (a protolith). This study focused on quantification of the retention of Mg/Ca and Sr/Ca ratios, and δ18O during the transformation process as well as evaluation of the transformation rate. To investigate the effect of transformation from aragonite to calcite on elemental and stable isotope ratios, we conducted a series of experiments in NaCl solutions at temperatures between 120 and 184 °C. Two additional experiments at 250 °C were conducted to estimate the transformation rate of aragonite to calcite. Protolith materials consist of (1) synthetic (Mg; Sr-bearing or non-Mg; Sr bearing) needle-shaped microcrystals of aragonite (<5 µm in size) and (2) larger chips (>100 µm in size) of natural aragonite. X-ray diffraction (XRD) showed that microcrystals successfully transformed to calcite within 30 h and scanning electron microscopy (SEM) yielded a change in the crystal size to >10 µm in rhombohedral shape. Electron backscatter diffraction (EBSD) of the larger aragonite chips showed that transformation to randomly oriented calcite occurred at the rims and along the cracks while the core retained an aragonite crystal structure. Isotope-ratio mass spectrometry (IRMS) analyses showed that calcite δ18O was controlled by temperature and δ18O of the solution. The obtained calibration curve of isotope fractionation factor versus temperature is consistent with other studies. Inductively coupled plasma optical emission spectroscopy (ICP-OES) analyses showed that calcite partially or completely retained Mg/Ca and Sr/Ca ratios through the transformation.

58 GEOSCIENCES↗
DOE OSTI2024

Characterization of Incremental Markings in the Sagittal Otolith of the Pacific Sardine ( Sardinops sagax ) Using Different Imaging Modalities

Teleost fish possess calcium carbonate otoliths located in separate chambers (utriculus, sacculus, and lagena) of their membranous labyrinth. This study analyzed the surface topography of the sagittal otolith of the Pacific sardine (Sardinops sagax) and the daily and annual increments in these otoliths. The otolith surface, characterized by laser scanning confocal microscopy for the first time, consisted of a system of prominent ridges and valleys (grooves), but it is unclear whether these structures are functional or represent time-resolving markings reflecting growth periodicity. Within the first-year volume, daily increments, each consisting of an incremental (more mineralized) and a discontinuous (less mineralized) zone, were resolved by optical microscopy and backscattered electron (BSE) imaging in the scanning electron microscope (SEM). Daily growth increments could, however, not be resolved in volumes formed after the first year, presumably because otolith growth markedly slows down and spacing of incremental markings narrows in older fish. Throughout otolith growth, the crystalline network continues across the discontinuous zones. Fluorochrome labeling provides additional information on growth after the first year. Compared with optical and BSE imaging, synchrotron microComputed Tomography of intact otoliths (with 0.69 µm volume elements) was less able to resolve daily increments; X-ray phase contrast reconstructions provided more detail than reconstructions with absorption contrast. Future research directions are proposed.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

A Facile Aqueous Solution Route for the Growth of Chalcogenide Perovskite BaZrS 3 Films

The prototypical chalcogenide perovskite, BaZrS 3 (BZS), with its direct bandgap of 1.7–1.8 eV, high chemical stability, and strong light–matter interactions, has garnered significant interest over the past few years. So far, attempts to grow BaZrS 3 films have been limited mainly to physical vapor deposition techniques. Here, we report the fabrication of BZS thin films via a facile aqueous solution route of polymer-assisted deposition (PAD), where the polymer-chelated cation precursor films were sulfurized in a mixed CS 2 and Ar atmosphere. The formation of a single-phase polycrystalline BZS thin film at a processing temperature of 900 °C was confirmed by X-ray diffraction and Raman spectroscopy. The stoichiometry of the films was verified by Rutherford Backscattering spectrometry and energy-dispersive X-ray spectroscopy. The BZS films showed a photoluminescence peak at around 1.8 eV and exhibited a photogenerated current under light illumination at a wavelength of 530 nm. Temperature-dependent resistivity analysis revealed that the conduction of BaZrS 3 films under the dark condition could be described by the Efros–Shklovskii variable range hopping model in the temperature range of 60–300 K, with an activation energy of about 44 meV.

36 MATERIALS SCIENCE↗
DOE OSTI2022

A Laser Frequency Transverse Modulation Might Compensate for the Spectral Broadening Due to Large Electron Energy Spread in Thomson Sources

Compact laser plasma accelerators generate high-energy electron beams with increasing quality. When used in inverse Compton backscattering, however, the relatively large electron energy spread jeopardizes potential applications requiring small bandwidths. We present here a novel interaction scheme that allows us to compensate for the negative effects of the electron energy spread on the spectrum, by introducing a transverse spatial frequency modulation in the laser pulse. Such a laser chirp, together with a properly dispersed electron beam, can substantially reduce the broadening of the Compton bandwidth due to the electron energy spread. We show theoretical analysis and numerical simulations for hard X-ray Thomson sources based on laser plasma accelerators.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2022

Polar Aerosol Vertical Structures and Characteristics Observed with a High Spectral Resolution Lidar at the ARM NSA Observatory

Aerosol vertical distributions impact both the direct and indirect radiative effects of aerosols. High Spectra Resolution Lidar (HSRL) separates between atmospheric molecular signals and aerosol particle signals and therefore can provide reliable measurements of aerosol properties. Six years of HSRL measurements between 2014 and 2019 from the Department of Energy (DOE) Atmospheric Radiation Measurement (ARM) North Slope of Alaska (NSA) atmospheric observatory at Utqiaqvik are used to statistically analyze Arctic aerosol vertical distributions. The annual cycle of aerosol vertical distributions in terms of aerosol particulate backscatter coefficient ($β_p$), lidar scattering ratio (SR), and aerosol particulate depolarization ratio ($δ_p$) profiles at the wavelength of 532 nm shows that Arctic Haze events are prevalent in later winter and spring at the NSA site. Mineral dust is frequently presented in strong aerosol layers in the spring, fall, and winter seasons. Over the summer season, the NSA site has large aerosol loadings that are dominated by small spherical aerosol particles.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Realistic Noise Generation to Enhance Realism of Virtual Lidar Scans

Many real-world phenomena corrupt light detection and ranging (lidar) measurements, such as laser energy attenuation, variations in aerosol concentration and composition with height, and hard target returns. Accurate studies of lidar scans using virtual lidar methods should include some realistic model of these corrupting effects to generate more realistic simulations of lidar scans. We present a simple model that characterizes noise caused by energy attenuation and aerosol stratification. The model requires limited inputs and is developed for a Halo Photonics Streamline XR lidar but is readily generalizable for other lidar systems. A critical component of this model is a model of the standard deviation of measured wind speed as a function of the backscattered signal’s signal-to-noise ratio. We derive a general model for this behavior that can be adapted to different scan settings.

17 WIND ENERGY↗
DOE OSTI2020

High Speed, Localized Multi-Point Strain Measurements on a Containment Vessel at 1.7 MHz Using Swept-Wavelength Laser-Interrogated Fiber Bragg Gratings

Dynamic elastic strain in ~1.8 and 1.0 m diameter containment vessels containing a high explosive detonation was measured using an array of fiber Bragg gratings. The all-optical method, called real-time localized strain measurement, recorded the strain for 10 ms after detonation with additional measurements being sequentially made at a rate of 1.7 MHz. A swept wavelength laser source provided the repetition rate necessary for such high-speed measurements while also providing enough signal strength and bandwidth to simultaneously measure 8 or more unique points on the vessel’s surface. The data presented here arethen compared with additional diagnostics consisting of a fast spectral interferometer and an optical backscatter reflectometer to show a comparison between the local and global changes in the vessel strain, both dynamically and statically to further characterize the performance of the localized strain measurement. The results are also compared with electrical resistive strain gauges and finite element analysis simulations.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

An Impedance-Loaded Surface Acoustic Wave Corrosion Sensor for Infrastructure Monitoring

Passive surface acoustic wave (SAW) devices are attractive candidates for continuous wireless monitoring of corrosion in large infrastructures. However, acoustic loss in the aqueous medium and limited read range usually create challenges in their widespread use for monitoring large systems such as oil and gas (O&G) pipelines, aircraft, and processing plants. This paper presents the investigation of impedance-loaded reflective delay line (IL-RDL) SAW devices for monitoring metal corrosion under O&G pipeline-relevant conditions. Specifically, we studied the effect of change in resistivity of a reflector on the backscattered signal of an RDL and investigated an optimal range through simulation. This was followed by the experimental demonstrations of real-time monitoring of Fe film corrosion in pressurized (550 psi) humid CO 2 conditions. Additionally, remote monitoring of Fe film corrosion in an acidic solution inside a 70 m carbon steel pipe was demonstrated using guided waves. This paper also suggests potential ways to improve the sensing response of IL-RDLs.

47 OTHER INSTRUMENTATION↗
DOE OSTI2026

Laboratory Tests of Laser Control of Electron Beams for Future Colliders

Laser-driven Compton backscattering (CBS) has been proposed as method for controlling the intensity of colliding bunches in the FCC-ee so as to avoid the flip-flop instability caused by intensity asymmetry in colliding bunches. Laser-based collimation has also been proposed as an indestructible collimator for high-intensity electron beams. We have initiated a laboratory-based test program of these concepts with the E344 experiment at FACET-II. In this paper, we describe simulations of laser-beam interactions at FACET-II and the relevant scaling for FCC-ee. We also describe the experimental setup and diagnostics that will be used to make the measurements at FACET-II.

Accelerator Physics (physics.acc-ph)↗
DOE OSTI2024

Focused Ion Beam Tomography of Alloy 617 Corroded in Molten Chloride Salt

Materials qualification of reactor structural materials is a critical step in rapid implementation of advanced nuclear reactor technologies, particularly to assess the corrosion performance in these designs. Accelerated qualification of reactor structural materials requires incorporating powerful computational toolsets, such as phase field modelling in the Multiphysics Object-Oriented Simulation Environment (MOOSE) framework, to predict the evolution of structural materials due to corrosion. Accordingly, computational toolsets will require experimental data generated at appropriate length scales to validate accuracy. Focused ion beam (FIB) provides a high degree of control over manipulation of materials for analytical purposes, including capturing data on the evolution in the microstructure and elemental composition of materials at the mesoscale, an appropriate length scale for phase field modelling of intergranular diffusion phenomena using the MOOSE framework. For instance, the FEI Helios G4 UX dual beam plasma FIB microscope at the Irradiated Materials Characterization Laboratory (IMCL) is capable of backscatter diffraction (EBSD) and energy-dispersive x-ray spectroscopy (EDS) documenting the evolution in the microstructure and elemental composition, respectively. The Helios can perform EDS and EBSD three-dimensionally (3D) using tomography, which is then combined using different software packages to visualize 3D volumes correlating elemental composition to microstructural data. The purpose of this investigation was to develop a streamlined characterization and data processing workflow for 3D tomography studies on the FEI Helios G4 plasma FIB. The investigation is segmented into three parts: 1) Optimizing the data collection workflow, 2) identifying appropriate data processing and visualization software (i.e. DREAM.3D, MIPAR, and VGStudioMax), and 3) establishing an infrastructure for public release. The optimization of the data collection workflow is in collaboration with members of the U220 department to setup formal training on the tomography operation of the G4, through ThermoFisher Scientific, and exploring DREAM.3D, MIPAR, and VGStudioMax data processing/visualization software packages. VGStudioMax currently demonstrates the most promise for future use. Optimization of the data collection and processing workflow is still ongoing. A collaboration with INL High Performance Computing (HPC) established an open-source license for expediting the public release of FIB tomography datasets through HPC. FIB tomography data generated by the G4 will provide comprehensive data for validating 3D phase field mesoscale modelling tools within the MOOSE framework for accelerated qualification of reactor structural materials.

Copeland-Johnson, Trishelle↗
DOE OSTI2022

Evaluation of Applied Stress on Atmospheric Corrosion and Pitting Characteristics in 304L Stainless Steel

For this study, the effects of applied stress, ranging from tensile to compressive, on the atmospheric pitting corrosion behavior of 304L stainless steel (SS304L) were analyzed through accelerated atmospheric laboratory exposures and microelectrochemical cell analysis. After exposing the lateral surface of a SS304L four-point bend specimen to artificial seawater at 50°C and 35% relative humidity for 50 d, pitting characteristics were determined using optical profilometry and scanning electron microscopy. The SS304L microstructure was analyzed using electron backscatter diffraction. Additionally, localized electrochemical measurements were performed on a similar, unexposed, SS304L four-point bend bar to determine the effects of applied stress on corrosion susceptibility. Under the applied loads and the environment tested, the observed pitting characteristics showed no correlation with the applied stress (from 250 MPa to -250 MPa). Pitting depth, surface area, roundness, and distribution were found to be independent of location on the sample or applied stress. The lack of correlation between pitting statistics and applied stress was more likely due to the aggressive exposure environment, with a sea salt loading of 4 g/m 2 chloride. The pitting characteristics observed were instead governed by the available cathode current and salt distribution, which are a function of sea salt loading, as well as pre-existing underlying microstructure. In microelectrochemical cell experiments performed in Cl - environments comparable to the atmospheric exposure and in environments containing orders of magnitude lower Cl - concentrations, effects of the applied stress on corrosion susceptibility were only apparent in open-circuit potential in low Cl - concentration solutions. Cl - concentration governed the current density and transpassive dissolution potential.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Processes contributing to cloud dissipation and formation events on the North Slope of Alaska

Abstract. Clear-sky periods across the high latitudes have profound impacts on the surface energy budget and lower atmospheric stratification; however an understanding of the atmospheric processes leading to low-level cloud dissipation and formation events is limited. A method to identify clear periods at Utqiaġvik (formerly Barrow), Alaska, during a 5-year period (2014–2018) is developed. A suite of remote sensing and in situ measurements from the high-latitude observatory are analyzed; we focus on comparing and contrasting atmospheric properties during low-level (below 2 km) cloud dissipation and formation events to understand the processes controlling clear-sky periods. Vertical profiles of lidar backscatter suggest that aerosol presence across the lower atmosphere is relatively invariant during the periods bookending clear conditions, which suggests that a sparsity of aerosol is not frequently a cause for cloud dissipation on the North Slope of Alaska. Further, meteorological analysis indicates two active processes ongoing that appear to support the formation of low clouds after a clear-sky period: namely, horizontal advection, which was dominant in winter and early spring, and quiescent air mass modification, which was dominant in the summer. During summer, the dominant mode of cloud formation is a low cloud or fog layer developing near the surface. This low cloud formation is driven largely by air mass modification under relatively quiescent synoptic conditions. Near-surface aerosol particles concentrations changed by a factor of 2 around summer formation events. Thermodynamic adjustment and increased aerosol presence under quiescent atmospheric conditions are hypothesized as important mechanisms for fog formation.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Wind-driven emissions of coarse-mode particles in an urban environment

Abstract. Quantifying surface–atmosphere exchange rates of particles is important for understanding the role of suspended particulate matter in radiative transfer, clouds, precipitation, and climate change. Emissions of coarse-mode particles with a diameter greater than 0.5 µm provide giant cloud condensation nuclei and ice nuclei. These emissions are critical for understanding the evolution of cloud microphysical properties yet remain poorly understood. Here we introduce a new method that uses lidar retrievals of the elastic backscatter and Doppler velocity to obtain surface number emissions of particles with a diameter greater than 0.53 µm. The technique is applied to study particle number fluxes over a 2-month period from 1 June to 10 August 2022 during the TRACER campaign at an urban site near Houston, TX, USA. We found that all the observed fluxes were positive (upwards), indicating particle emission from the surface. The fluxes followed a diurnal pattern and peaked near noon local time. Flux intensity varied through the 2 months with multi-day periods of strong fluxes and multi-day periods of weak fluxes. Emission particle number fluxes peaked near ∼ 100 cm−2 s−1. The daily averaged emission fluxes correlated with friction velocity and were anticorrelated with surface relative humidity. The emission flux can be parameterized as F= 3000 u*4, where u* is the friction velocity in m s−1 and the emission flux F is in cm−2 s−1. The u* dependence is consistent with emission from wind-driven erosion. Estimated values for the mass flux are in the lower range of literature values from non-urban sites. These results demonstrate that urban environments may play an important role in supplying coarse-mode particles to the boundary layer. We anticipate that quantification of these emissions will help constrain aerosol–cloud interaction models that use prognostic aerosol schemes.

54 ENVIRONMENTAL SCIENCES↗