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At least 451 records · Page 25
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Sulfur speciation in dacitic melts using X-ray absorption near-edge structure spectroscopy of the S K -edge (S-XANES): Consideration of radiation-induced changes and the implications for sulfur in natural arc systems

Abstract The synchrotron technique of micro X-ray absorption near-edge structure spectroscopy at the sulfur K-edge (S-XANES) provides a unique opportunity to measure the proportion of different oxidation states of sulfur (S) in silicate glasses. Although applied extensively in the analysis of basaltic silicate glasses, few S-XANES studies have investigated variations in S oxidation states with fO2 in felsic silicate glasses. In addition, no study has systematically compared the S-XANES results obtained from the same samples at different photon flux densities to quantify the relationship between exposure time and changes in S speciation in silicate glass, as has been done for Fe and V. This study evaluates observed differences in S speciation measured in experimentally produced H2O-saturated dacitic glasses over a range of reducing to oxidizing conditions (from log fO2 = ΔFMQ-0.7 to ΔFMQ+3.3; FMQ is the fayalite-magnetite-quartz mineral redox buffer) and equilibrated at 1000 °C and 300 MPa. S-XANES spectra were collected at three different photon flux densities using three microspectroscopy beamlines. As is observed in S-XANES analyses of basaltic silicate glasses, beam-induced changes to the S6+/ΣS are observed as a function of photon flux density and beam exposure time. Our results demonstrate that silicate glasses of dacitic composition undergo beam-induced photo-reduction in samples equilibrated at ΔFMQ > +1.75 and photo-oxidation if equilibrated at ΔFMQ < +1. The time required to observe beam-induced changes in the spectra varies as a function of flux density, and our study establishes an upper photon density limit at ~1.0 × 1012 photons/µm2. The S6+/ΣS calculated from spectra collected below this absorbed photon limit at intermediate flux densities (~1–4 × 109 photons/s per µm2) are affected by beam damage, as no conditions were found to be completely free of beam-induced changes. However, the S6+/ΣS ratios calculated below the limit at intermediate flux densities are consistent with thermodynamic constraints, demonstrating that S6+/ΣS ratios calculated from S-XANES spectra can be considered reliable for estimating the oxygen fugacity. Our results carry important implications for the S budget of felsic magmas and dissolution mechanisms in evolved melts. While our results from all three flux densities show the presence of S4+ dissolved in relatively oxidized (ΔFMQ > +1.75) dacitic glass, even in the spectra exposed to the lowest photon densities, we are unable to rule out the possibility that the S4+ signal is the result of instantaneous X-ray irradiation induced beam damage using S-XANES alone. When our spectra are compared to S-XANES spectra from basaltic silicate glasses, important differences exist in the solubility of S2– and S6+ between dacitic silicate melts, pointing to differences in solubility mechanisms as melt composition changes. This study highlights the need for further investigation into beam damage systematics, presence of S4+, and the solubility mechanisms of different oxidation states of S as silicate melt composition changes.

Geochemistry & Geophysics↗
DOE OSTI2024

Damage evolution and ductile fracture of commercially-pure titanium sheets subjected to simple tension and cyclic bending under tension

This paper describes a study into the evolution of damage in commercial-purity titanium (CP–Ti) sheets subjected to cyclic bending under tension (CBT) and uniaxial tension (simple tension, ST). Sections were taken from sheets that were strained to various levels under both methods and were imaged using X-ray computed tomography (XCT) to reveal insights into the size, density, and distribution of microvoids in the sheets. Digital image correlation (DIC) was also used to observe the surface strain of CBT and ST sheets during testing. These results showed that elongation to failure (ETF) for CBT deformation is about 2.5× higher than for ST, local longitudinal strains in the bulk of the CBT sample are around 1.3× higher than the peak strain in the ST necked region, and 1.7× higher in the localized region of CBT failure. It was found that the volume-density of voids in both sheets followed a similar exponential increase with strain, reaching nearly 45× higher in the CBT than the ST sheets before the onset of failure, mainly due to the higher strain levels achieved. A higher volume density of voids developed in the center of sheets at high levels of strain, for both processes, with the density in the sheet center becoming approximately double that found near the edges. Scanning electron microscopy (SEM) was used to examine the fracture surface of CBT and ST sheets after failure. The observations are presented and discussed highlighting the CBT process as effective to delay ductile fracture of the CP-Ti sheets.

Commercially pure titanium↗
DOE OSTI2021

Evolution of Permeability in Sandstone During Confined Brazilian Testing

Permeability measurements were made on sandstone during confined Brazilian strength tests. The test involves 50 mm diameter disk-shaped, jacketed samples that are subjected to confining stresses while they are diametrically loaded. Specially designed end caps allow for concurrent gas flow measurements. The test configuration allows for the samples to be subjected to a range of stresses, with the confining stress as the intermediate principal stress. Furthermore, the majority of the tests measured permeability during loading to failure in the confined extension region. The permeability of the sandstone sample increases significantly well before the peak load is reached due to newly formed microcracks that continue to coalesce and dilate with further loading. Permeability increases are inversely proportional to the intermediate principal stress as increased confining pressures suppress growth, coalescence, and dilation of microcracks. Additional testing includes unloading and reloading cycles prior to failure. With each unloading–reloading cycle, permeability at comparable stresses is increased compared to the previous cycle, consistent with increasing damage in the form of an expanding microcrack network.

58 GEOSCIENCES↗
DOE OSTI2021

Defect Characterization Using Positron Annihilation Spectroscopy on Laser-Ablated Surfaces

In recent years, short, pulsed laser ablation has been gaining popularity for machining small-scale test geometries from bulk samples and for efficient serial sectioning. These laser-based techniques are being added to the toolbox in material science, which makes it necessary to understand the changes in the material that occur from the laser–material interaction. Positron annihilation spectroscopy is a unique, nondestructive technique to investigate small defects in materials difficult to investigate by other tools. In this work, Doppler broadening and positron lifetime annihilation spectroscopy are utilized to help quantify the damage in materials treated with short, pulsed lasers. Using a femtosecond laser on single crystal silicon, this manuscript shows that clusters of vacancy-like defects and small voids increase systematically with laser power. Lastly, the damage induced by the laser can also reach to micrometer depths.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Multiple-platform and multiple-Doppler radar observations of a supercell thunderstorm in South America during RELAMPAGO

On 10 November 2018, during the RELAMPAGO field campaign in Argentina, South America, a thunderstorm with supercell characteristics was observed by an array of mobile observing instruments, including three Doppler on Wheels (DOW) radars. This is believed to be the first such storm ever sampled by multiple Doppler radars in South America, and one of perhaps two such sets of observations in the Southern Hemisphere. The observational strategies employed within the Córdoba Province on 10 November are described, as also is the evolution of the initial deep convective clouds through their organization into a supercell. In contrast to the archetypal supercell, the updraft rotation in this storm was rather short lived (~20 min), as also was the occurrence of damaging hail, causing us to question whether this indeed was indeed a supercell. However, additional data collected within the Córdoba Province provide us with evidence of other storms with this behavior, which appears to be attributable in part to effects of the local terrain. Thus, the structure and evolution of this storm documented during RELAMPAGO may be typical in this region.

Trapp, Robert↗
DOE OSTI2022

The effect of helium on cavity swelling in dual-ion irradiated Fe and Fe-10Cr ferritic alloys

We report Ferritic-martensitic (FM) steels for in-vessel components in proposed fusion reactors are expected to suffer from high levels of displacement damage and helium (He) generation by neutron transmutation. However, a thorough understanding of the He synergistic effects on the cavity swelling in FM steels is still not well established. To gain fundamental insights into the He effect on cavity swelling, high purity Fe and Fe-10 wt.% Cr ferritic model alloys were irradiated with 8 MeV Ni ions and co-implanted He ions at 400 to 550 °C up to 30 displacements per atom (dpa) with He implantation rates of 0.1, 10 and 50 appm He/dpa. The current study focuses on the 50 appm He/dpa, 500 °C behavior vs. 0.1 and 10 appm He/dpa. Irradiation-induced defects, including cavities, dislocation loops, and dislocation networks were characterized using transmission electron microscopy (TEM). In the grain interior, a bimodal cavity size distribution was observed in the 10 and 50 appm He/dpa samples, but not for 0.1 appm He/dpa. Cavity swelling was maximized at intermediate He implantation rates of ~10 appm He/dpa for both ion-irradiated Fe and Fe-10Cr alloys. The cavity swelling behavior as a function of He implantation rate appears to be controlled by the He/dpa-dependent variation of cavity sink strengths. Treating small bubbles as biased sinks for interstitial absorption can significantly increase the ratio of biased to unbiased sink strengths (Q) and results in maximized cavity swelling for a Q ratio close to one.

36 MATERIALS SCIENCE↗
DOE OSTI2025

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↗
DOE OSTI2024

Elastic thermobarometry on metapelites across the crustal section of the Famatinian Arc, Argentina

We applied elastic thermobarometry on garnet-bearing migmatites along two transects through the crustal section at Sierra Valle Fértil-La Huerta, Argentina. We performed quartz-in-garnet barometry and zircon-in-garnet thermometry on metapelites from different paleo-depths across the crustal section. Our work recovers entrapment pressures ranging from 240 to 1330 MPa and entrapment temperatures between 691 and 1574 °C. The entrapment conditions are broadly consistent with anticipated pressures and temperatures along the crustal section derived previously using conventional, thermodynamic thermobarometers. The quartz-in-garnet barometer reproduces those conventionally established entrapment conditions when samples only experienced conditions within the alpha-quartz stability field. Raman-derived pressures for samples that experienced beta-quartz reference conditions are commonly much higher than those established by conventional barometry. Samples that preserve compressive (positive) residual pressures best reproduce reference entrapment pressures. Entrapment temperatures show high variability and overestimation of temperature conditions compared to conventional results. These results indicate elastic thermobarometry over- or under-estimates crystallization conditions in rocks crystallized at high temperatures, as is common in the Famatinian Arc deep-crust. We suggest that modeling quartz behavior across the alpha–beta transition may present challenges, as does shape maturation, viscous deformation, and radiation damage in zircon.

58 GEOSCIENCES↗
DOE OSTI2026

Toward an AI-Powered Software Pipeline for Real-Time Tracking and Analysis of Wildfire and Smoke

Real-time tracking of wildfires and smoke is crucial for effective response, minimizing damage, protecting lives, and efficiently managing resources during fire emergencies. We develop a web-based AI-powered pipeline that detects wildfires in aerial video and estimates deployment-relevant behavior metrics, including cumulative burned area, burned-area growth rate, fire spread direction, and smoke dispersion. The system combines a YOLO-based detector with YCbCr-based fire segmentation, HSV-based smoke segmentation, Farneback optical flow, and centroid-based spatiotemporal tracking. Using ground sampling distance (GSD), pixel-level fire masks are converted to physical burned-area measurements by correlating fire pixel counts with camera altitude and tilt angle. We benchmark YOLO variants and non-YOLO baselines (GoogLeNet, CNN, DBN, Autoencoder, U-Net, and AlexNet) on the IEEE FLAME dataset and a newly created aerial frame dataset, Wildfire-DB. Cross-dataset evaluation uses a strict threshold-transfer protocol: decision thresholds are selected on FLAME validation and transferred unchanged to Wildfire-DB to quantify generalization under domain shift. YOLOv6 achieves the strongest cross-dataset frame-level fire detection on Wildfire-DB (ROC-AUC 0.8200, PR-AUC 0.8044, and transferred-threshold F1 0.7596). For tracking-oriented deployment requiring oriented localization, YOLO11-OBB provides the most reliable cross-dataset behavior among OBB-capable models while remaining computationally feasible. To analyze the feasibility of UAV deployment, we further measure inference efficiency using synchronized GPU and CPU power logs on a fixed workload of 1569 frames. YOLO-family models process the video in 5.73–12.47 seconds with net energy of 1247.28–1775.39 J, substantially lower latency and energy than heavier classification and reconstruction baselines. Overall, model optimality depends on operational objectives: YOLOv6 is best for cross-dataset detection robustness, whereas YOL...

Color segmentation↗
DOE OSTI2020

Success Using A Granular-Activated Carbon Filtration Swab to Rehabilitate Westbay{sup R} Multi-level Groundwater Monitoring Wells at the INL - 20544

In November 2015, tetrachloroethylene (PCE) was discovered in groundwater samples collected from a Westbay{sup R} multi-level groundwater monitoring well at the Idaho National Laboratory (INL).a Subsequent investigation determined that PCE was not present in the groundwater. The detected PCE was instead due to inadvertent contamination of the internal tubing fluid in the Westbay well-monitoring system, which is isolated from the surrounding groundwater. Further investigation showed that three of the 11 Westbay wells at the INL contained PCE-contaminated tubing fluid at concentrations above the U.S. Environmental Protection Agency's maximum contaminant level for drinking water (5 μg/L). Loose sediment at the bottom of some Westbay wells was also found to contain PCE; the three wells were then identified for rehabilitation as part of the INL well maintenance program. The unique construction of the Westbay wells - i.e., the small diameter (5.72 cm [2.25 in.]) and the depths of the tubing fluid ranging from 144.8 to 419 m (475 to 1,376 ft) below ground surface - posed unique challenges to the rehabilitation. Because the tubing fluid provides structural integrity, the fluid cannot be removed and then replaced without damaging the integrity of the Westbay well. Additionally, the small diameter of the systems and the associated depths limit the availability of equipment that can be used for the rehabilitation. After an evaluation of potential methods, it was determined that the use of an in-well, custom-fabricated, granular-activated-carbon filtration swab deployed via a wire line would provide the safest and most cost-effective method for rehabilitation. Westbay well rehabilitation started at well MIDDLE-2051 in late June 2018 and paused in December 2018 for the season. The PCE concentration in the tubing fluid at MIDDLE-2051 was initially reduced to a maximum concentration of 3.81 μg/L from a maximum of 642 μg/L, while the concentration of PCE in the sediment had been reduced from 5,360 to 2,270 μg/kg. Sampling was performed at MIDDLE-2051 again in August 2019, and the tubing fluid increased to a maximum concentration of 45.4 μg/L, while the concentration in the sediment decreased further to 1,890 μg/kg due to desorption of PCE from the sediment to the tubing fluid. Rehabilitation resumed at well MIDDLE-2050A in late August 2019, and the PCE concentration in the tubing fluid had been reduced to a maximum concentration of 19.0 μg/L. Although the method has been shown to be time-consuming, it has proven to be effective and safe for personnel performing the work and to the integrity of the well. Future sample data results at all wells will help determine an estimated completion of the rehabilitation. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Radiolysis and Radiation-Driven Dynamics of Boehmite Dissolution Observed by In Situ Liquid-Phase TEM

We report over the last several decades, there have been several studies examining the radiation stability of boehmite and other aluminum oxyhydroxides, yet less is known about the impact of radiation on boehmite dissolution. Here, we investigate radiation effects on the dissolution behavior of boehmite by employing liquid-phase transmission electron microscopy (LPTEM) and varying the electron flux on the samples consisting of either single nanoplatelets or aggregated stacks. We show that boehmite nanoplatelets projected along the [010] direction exhibit uniform dissolution with a strong dependence on the electron dose rate. For nanoplatelets that have undergone oriented aggregation, we show that the dissolution occurs preferentially at the particles at the ends of the stacks that are more accessible to bulk solution than at the others inside the aggregate. In addition, at higher dose rates, electrostatic repulsion and knock-on damage from the electron beam causes delamination of the stacks and dissolution at the interfaces between particles in the aggregate, indicating that there is a threshold dose rate for electron-beam enhancement of dissolution of boehmite aggregates.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Contrasting Chemical Kinetic Parameters for Near In‐Service‐Temperature Aging and High‐Temperature Thermal Decomposition of Triaminotrinitrobenzene Formulations

Triaminotrinitrobenzene-based high explosives such as LX-17 offer high energy density and exceptional safety, yet their long-term aging behavior at low temperatures remains poorly understood. In this study, several legacy and new production lots of LX-17 were subjected to accelerated aging experiments below 100°C, during which the formation rate of the initial degradation product, monofurazan (F1), was monitored. Kinetic analysis was performed using a sample-age-aware computational approach, yielding activation energy estimates of 82–91 kJ mol −1 for the low-temperature initiation step—markedly lower than the ∼200 kJ mol −1 associated with high-temperature thermal decomposition. Extrapolation from established cookoff models supports the conclusion that the dominant degradation mechanism at low temperatures differs from that at high temperatures. In conclusion, our results provide a unified kinetic framework that bridges the gap between in-service conditions and high-temperature damage.

Chemistry - Chemical explosives↗
DOE OSTI2020

Differences in the response of two light guide technologies and two readout technologies after an exchange of liquid argon in the dewar

In this investigation the response to the scintillation light generated by through-going cosmic muons in liquid argon (LAr) was measured by two light guide technologies and two readout technologies after five weeks of running in the TallBo dewar at Fermilab. The response was remeasured after the dewar was drained of LAr, refilled, and then run again for an additional four weeks. After the dewar was refilled, there was clear evidence that the scintillation signal had dropped significantly. The two light guide technologies were developed at Indiana University and MIT/Fermilab. The two readout technologies were boards that passively or actively ganged 12 Hamamatsu MPPCs. Two possible explanations were identified for the degraded signal: the response of the two light guide technologies degraded due to damage caused by thermal cycling, and/or unknown differences in the trace residual Xe contamination in the fills of LAr led to the observed drop in scintillation light. Neither absorption nor quenching by N 2 , O 2 , and H 2 O contamination can account for the degradation. Neither the individual Hamamatsu MPPCs nor the passive/active ganging boards appear to have been affected by the thermal cycling. The path length distributions of the cosmics traversing the dewar appear quite similar in both event samples.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Use of Transmission Electron Microscopy for Analysis of Aerosol Particles and Strategies for Imaging Fragile Particles

For over 25 years, transmission electron microscopy (TEM) has provided a method for the study of aerosol particles with sizes from below the optical diffraction limit to several microns, resolving the particles as well as smaller features. The wide use of this technique to study aerosol particles has contributed important insights about environmental aerosol particle samples and model atmospheric systems. TEM produces an image that is a 2D projection of aerosol particles that have been impacted onto grids and, through associated techniques and spectroscopies, can contribute additional information such as the determination of elemental composition, crystal structure, and 3D particle structures. Soot, mineral dust, and organic/inorganic particles have all been analyzed using TEM and spectroscopic techniques. TEM, however, has limitations that are important to understand when interpreting data including the ability of the electron beam to damage and thereby change the structure and shape of particles, especially in the case of particles composed of organic compounds and salts. In this paper, we concentrate on the breadth of studies that have used TEM as the primary analysis technique. Another focus is on common issues with TEM and cryogenic-TEM. Insights for new users on best practices for fragile particles, that is, particles that are easily susceptible to damage from the electron beam, with this technique are discussed. Tips for readers on interpreting and evaluating the quality and accuracy of TEM data in the literature are also provided and explained.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Electron-beam-driven chemical processes during liquid phase transmission electron microscopy

Liquid phase (or liquid cell) transmission electron microscopy (LP-TEM) has been established as a powerful tool for observing dynamic processes in liquids at nanometer to atomic length scales. However, the simple act of observation using electrons irreversibly alters the nature of the sample. A clear understanding of electron beam-driven processes during LP-TEM is required to interpret in situ observations and utilize the electron beam as a stimulus to drive nanoscale dynamic processes. In this review, we discuss recent advances toward understanding, quantifying, mitigating, and harnessing electron beam-driven chemical processes occurring during LP-TEM. We will highlight progress in several research areas, including modeling electron beam-induced radiolysis near interfaces, electron beam-induced nanocrystal formation, and radiation damage of soft materials and biomolecules.

Woehl, Taylor J.↗
DOE OSTI2020

p-type conductivity and damage recovery in implanted GaN annealed by rapid gyrotron microwave annealing

We demonstrate p-type activation of GaN doped by Mg ion implantation, and in situ during metalorganic chemical vapor deposition through sequential short-duration gyrotron microwave heating cycles at temperatures of 1200–1350 °C. GaN is implanted with 1019 cm−3 Mg ions, capped with AlN, and annealed under 3 MPa N2 overpressure in 5 s heating cycles for less than 60 s total using a high-power gyrotron microwave heating source. Through I–V characterization, photoluminescence spectroscopy, and Raman spectroscopy, we study the evolution of electrical properties, optically active point defects, and material strain in response to implantation and annealing. For Mg-implanted samples, increasing annealing temperature is characterized by an increase in the PL substitutional Mg-related peak (UVL) relative to the shallow-donor vacancy-related peak (GL2). Through comparison of implanted and in situ doped samples, it is demonstrated that the origin of compensating VN lies primarily in implantation rather than degradation from the annealing process. Transmission line measurements and diode I–V measurements show a sheet resistance of 1083 kΩ/□ and a hole concentration of 1.23 × 1015 cm−3, respectively, in the Mg-implanted material annealed at 1350 °C. We conclude that temperature-cycled gyrotron annealing at 1350 °C decreases implant-induced compensating point defects and activates Mg to obtain selective p-type conduction.

Meyers, V. (ORCID:0000000176731553)↗
DOE OSTI2025

Microstructure, stored energy, and stability of H/He-filled nanocavities in low temperature irradiated Inconel 718

The microstructure, trapped transmutation gases, stored energy, and mechanical behavior of samples from an irradiated Inconel 718 proton beam window were characterized using transmission electron microcopy, thermal desorption spectrometry (TDS), differential scanning calorimetry (DSC), and tensile testing. In the as-irradiated condition the microstructure contained a high number density of 1–3 nm gas-filled nanocavities. Emissions of trapped gases, H and He, during TDS correlated with peaks of the energy release curves from DSC examinations, which suggest these gases were likely stored in highly stable defect traps. The stored energy from radiation damage saturated at doses of a few dpa and did not increase with increasing radiation dose, but the amount of stored H and He increased with increasing dose. Effects of post-irradiation annealing were studied as well. After exposure to 700 °C, the nanocavities grew only slightly to 2–4 nm in diameter, but after exposure to 900 °C, the cavities grew to 10–20 nm in diameter and electron energy-loss spectroscopy showed these cavities contained a core of He surrounded by a shell of H. Further, this study demonstrated that the irradiation defect structures containing H and He were remarkably stable during irradiation and after exposure up to 700 °C. The effect of the irradiation temperature, defect mobility, and interaction of H, He, and irradiation defects on mechanical behavior provides insight into the processes responsible for the unusual recovery in ductility with increasing radiation dose observed in Inconel 718 after high energy proton and spallation neutron irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Feature Engineering and Ensemble Methods for Imbalanced ICS Intrusion Detection: Pipeline Audit and Constrained Evaluation

Industries are becoming increasingly connected and are more vulnerable to cyberattacks due to the widened attack surface. Industrial Control Systems (ICS) are among the most critical sectors that malicious actors can target, as such attacks can cause significant operational disruption and physical damage. It is imperative to detect such attacks as early as possible. This paper evaluates constraint-conditioned optimistic performance estimates for traditional ML models in ICS intrusion detection (i.e., estimates obtained under contiguous, non-shuffled temporal evaluation without test-set alteration, but with pre-split feature engineering that may introduce temporal leakage, due to dataset constraints). Our findings are threefold. First, we quantify how iterative feature engineering affects tree-based ensemble performance and examine how pipeline decisions (split strategy, sampling scope, and cleaning policy) can inflate or reduce reported IDS results under constraint-bound evaluation. Second, we compare intrinsic class-imbalance handling across ensemble models. Third, under our current pipeline constraints (including pre-split feature engineering), CatBoost achieves the best performance on Water Storage Tank (accuracy: 0.9831, class-1 F1: 0.9682), while Light- GBM achieves the best performance on Gas Pipeline (accuracy: 0.9618, class-1 F1: 0.9086).

97 MATHEMATICS AND COMPUTING↗