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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 19 records

Identifying Spectral Descriptors for Protonation in BaZr 0.8 Y 0.2 O 3-x with Electron Energy Loss Spectroscopy

Hydrogen economy is of paramount importance in the global transition to a sustainable, clean energy source that contributes to decarbonization efforts. In particular, the proton conducting proton ceramic fuel cells (PCFCs) play a crucial role in promoting hydrogen energy technology [1-5]. In a PCFC, the electrolyte is typically a solid oxide material that enables proton transport and can operate at temperatures lower than those of traditional oxygen ion conducting fuel cells [6]. The reduced operating temperature of PCFCs contributes to their durability, scalability, and efficiency [7,8]. BaZr 0.8 Y 0.2 O 3-x (BZY) is a promising proton conducting solid oxide electrolyte [9,10]. The emphasis on proton conductivity entails the importance of understanding proton content in the system. However, previous studies have largely relied on bulk techniques such as electrochemical impedance spectroscopy [7,11], Karl-Fischer titration [12,13], and thermogravimetric analysis [14] to obtain proton concentration. This is due to the small atomic size and light mass of hydrogen species making direct detection challenging. Bulk methods may be useful in estimating the proton content; however, it overlooks possible proton concentration gradient or segregation that may occur across or within a nanoparticle, especially when proton incorporation occurs nonuniformly through steam exposure on powder samples. In this paper, BZY is protonated at an estimated 0.15 mol of protons via steam exposure. Electron energy loss spectroscopy (EELS) with nanoscale spatial resolution is explored to identify proxy signals for proton detection using a JEOL ARM300 microscope operated at 300 kV with a Gatan GIF Continuum detector.

08 HYDROGEN↗

Atomic-Scale Behavior of Radiation-Resistant ZnO under High-Energy Electron Bombardment

Understanding the atomic structure and defect characteristics of ZnO thin films is crucial for optimizing their electronic properties and performance in advanced applications. Here, we investigate the atomic structure and defect characteristics of atomic layer deposition (ALD)-grown ZnO thin films by using aberration-corrected scanning transmission electron microscopy (STEM). Atomic-resolution imaging identifies prevalent stacking faults, dipole disorder, and various grain boundary types, which are believed to influence the electronic properties of ZnO. Additionally, real-time electron beam exposure experiments demonstrate structural transformations, including crystal growth and surface rearrangements. These findings provide insights into the growth mechanisms of ALD ZnO under high-energy electron irradiation conditions, an important finding for the use of polycrystalline ZnO wide bandgap semiconductors in space-like conditions. In conclusion, our results underscore the capability of STEM in directly visualizing and quantifying atomic-scale defects and beam-induced transformations in radiation-resistant ZnO.

Defects↗

Beam-water Interaction System for PFAS Treatment

Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants that resist conventional water treatment due to the strength of their carbon fluorine bonds. Electron-beam irradiation has shown potential for PFAS degradation; however, its effectiveness is limited by shallow energy penetration, restricting treatment to the upper region of the water surface. This project addresses this limitation through the design of a compact mixing chamber and recirculation system to enhance surface renewal and improve treatment efficiency. The system, constrained to approximately 10 cm 20 cm 20 cm, was developed using computer-aided design, computational fluid dynamics (CFD), and MATLAB-based hydraulic analysis to evaluate flow behavior, head loss, and pump compatibility. A perforated-baffle geometry and controlled flow range of 1 3 GPM were implemented to promote uniform mixing while maintaining a stable free surface for electron-beam exposure. Modeling results indicate improved flow distribution and reduced dead zones, supporting more consistent interaction between contaminated water and the beam. The final design enhances hydrodynamic performance within system constraints, contributing to scalable electron-beam water treatment technologies for improved PFAS degradation.

Ramos, Gerardo [Northern Illinois U.]↗

Effects of electron beam irradiation on CrMnV and CrMnTiV high entropy alloys: Nano-mechanical, structural, and thermodynamic perspectives

Beam exit windows are crucial components of any particle accelerator as they provide an interface between the beamline vacuum and target material at atmospheric media. For high beam power machines, special materials and designs are required to withstand high radiation and mechanical loads, while minimizing energy loss during transition and maximizing window lifetime. This research investigates the impact of electron beam exposure to bulk CrMnV and CrMnTiV high entropy alloys (HEAs) with the primary goal of identifying suitable candidate materials for the design of robust and durable exit window settings. The selection criteria include intrinsic characteristics, power dissipation, and mechanical responses. According to the thermodynamic calculations, both equiatomic CrMnV and the addition of 7% of Ti with equiatomic CrMnV yield solid-solutions phases. The structural and mechanical properties of CrMnV and CrMnTiV samples were tested using field emission scanning electron microscopy, atomic force microscopy, scanning electron microcopy with energy dispersive x-ray spectroscopy, x-ray diffraction, and nanoindentation before and after exposure to a dose of ~66 kGy from a 10 MeV e-beam accelerator. Despite exhibiting beam transmission characteristics comparable to Cr and V, the indentation hardness of HEAs exceeded that of the Cr and V samples by five to six times. The examination of the CrMnTiV irradiated samples revealed organized deformation patterns depicting new features, which we suspect twinning and twin boundaries due to the addition of Ti to CrMnV. Ti, a hexagonal-close-packed crystal structure, is commonly known for deformation twinning behavior.

36 MATERIALS SCIENCE↗

Characterization of γ′/γ″ compact and sandwich type precipitates during long-term high-temperature exposure in Ni-based superalloys

Here, the formation of γ′/γ″ co-precipitates is investigated in Ni-based superalloys with a varying Ti/Al ratio and Ta content and their stability is studied using long-term high-temperature exposure. Transmission electron microscopy and atom probe tomography analyses demonstrate that both higher Ti/Al ratios and increased Ta promote γ″ phase formation, leading to sandwich and compact structures. The compact co-precipitation significantly reduces γ′ precipitate coarsening during 10,000 h exposure at 700°C by restricting elemental diffusion, particularly of aluminum, from the γ matrix to the γ′ phase. For the alloy without a compact structure, and only γʹ precipitates, at the beginning of the exposure, the coarsening rate over 10,000 h was 3.5 times faster than for the alloy with compact γʹ/γʺ precipitates. Evidence of destabilization of the compact morphology was found to occur between 5,000 and 10,000 h exposure and originated from the extensive formation and growth of δ platelets that extended throughout the grains. Thus, the outer layer of the compact, which consists of γʺ, was subjected to the γ″ to δ phase transformation.

gamma double prime↗

Study of electron-induced chemical transformations in polymers

In extreme ultraviolet (EUV) photoresist exposure, the primary and secondary electrons drive chemistry rather than the EUV photons themselves. These electrons have a wide range of energies below approximately 80 eV, which are capable of complex network of reactions during exposure. To better understand the ability of electrons of different energies within the EUV primary and secondary electron range, we want to characterize and compare the chemistry induced in pure polymer films by direct exposure to electrons. Thin films of poly(tert-butyl methacrylate), poly(methyl methacrylate), and poly(4-hydroxystyrene) were exposed to a 20 to 80 eV electron beam. Outgassing during exposure was characterized in-situ using a quadrupole residual gas analyzer. The thickness changes were measured using ellipsometry and chemical bond structure data were collected using Fourier-transform infrared spectroscopy (FTIR) after exposure to compare different exposure conditions. Poly(4-hydroxystyrene) demonstrated stability during electron exposures. Exposures of the other two materials led to outgassing of protecting groups, the intensity of which decayed in time. Outgassing, FTIR, and thickness loss data exhibited approximately linear relationships to each other.

Mueller, Maximillian↗

Decoupling Li out-diffusion and surface diffusion in the lithiation-assisted epitaxial growth of lithium tungstate

Lithiation-assisted epitaxy offers a flexible and robust approach for synthesizing high-quality Li-containing materials and interfaces with precise control. Here, in this study, we use lithium tungstate (Li x WO 3+x/2 , where x = 0 to 2) as a model system to investigate the intertwined effects of Li out-diffusion-induced compositional changes and surface-diffusion-induced morphological changes. By systematically varying synthesis and processing conditions, we uncover their impact on lithium tungstate film formation. Comprehensive characterizations, including X-ray diffraction, atomic force microscopy, X-ray photoemission spectroscopy and time-of-flight secondary ion mass spectrometry, reveal that low-temperature growth (< 300 °C) followed by high-temperature annealing yields continuous lithium tungstate films with significantly reduced surface roughness. In contrast, high-temperature deposition (≥ 300 °C) accelerates surface diffusion and Li out-diffusion, leading to island formation. Furthermore, in situ scanning transmission electron microscopy demonstrates the beam sensitivity of Li 2 WO 4 and reveals a phase transition from Li 2 WO 4 to LiWO 3.5 under prolonged electron beam exposure. These findings deepen our understanding of how to control composition and morphology of Li-containing films, providing valuable insights for the design and integration of energy materials.

Shi, Jueli [Pacific Northwest National Laboratory ↗

Dynamic STEM-EELS for single-atom and defect measurement during electron beam transformations

This study introduces the integration of dynamic computer vision–enabled imaging with electron energy loss spectroscopy (EELS) in scanning transmission electron microscopy (STEM). This approach involves real-time discovery and analysis of atomic structures as they form, allowing us to observe the evolution of material properties at the atomic level, capturing transient states traditional techniques often miss. Rapid object detection and action system enhances the efficiency and accuracy of STEM-EELS by autonomously identifying and targeting only areas of interest. This machine learning (ML)–based approach differs from classical ML in that it must be executed on the fly, not using static data. We apply this technology to V-doped MoS 2 , uncovering insights into defect formation and evolution under electron beam exposure. This approach opens uncharted avenues for exploring and characterizing materials in dynamic states, offering a pathway to increase our understanding of dynamic phenomena in materials under thermal, chemical, and beam stimuli.

47 OTHER INSTRUMENTATION↗

Microscopic Measurement: Need for Nuclear Material Sample Specimen Characterization Capability

The Surveillance, Fabrication, and Off-Site Operations team at Lawrence Livermore National Laboratory is beginning an update to the nuclear material machining lab in Superblock. Plutonium and other nuclear materials tend to accelerate the aging process for equipment and machines that would otherwise be maintainable for long lives. They have their lifespans shortened from deteriorated seals, embrittled polymer components, accelerated corrosion, and damage to electronics from exposure to radioactive materials. The cost of installation of equipment into a glove box (GB) tends to outstrip the cost of the equipment itself. Due to the magnification of cost, the historical approach to equipment installs has been to purchase and install the highest-quality and most robust equipment available to maximize time between failures and updates. To make room for the installation of a new lathe, the inspection GB is being moved to a different location within the machining lab. As part of the overall effort, the equipment within the inspection GB is being revisited. Current measurement capabilities are antiquated and starting to become problematic due to age. Advances in metrology are sought for more comprehensive characterization of scientific samples. This document aims to identify several options for the replacement of current measurement equipment and identify a system for purchase and eventual installation. The intention is not to select the cheapest system, but rather to identify a system that best meets the needs of both the operators and principal investigators (PI). Following the convention of the SYSM-5620 Design Thinking and System Engineering, it was determined that a laser confocal measurement system from Keyence is the most suitable option for our programmatic need. Form factor, capability, and maintainability were considered. Along with stakeholder input, to ensure the best decision for the Nuclear Material Technology Program.

36 MATERIALS SCIENCE↗

Search for New Physics via Low-Energy Electron Recoils with a 4.2 Tonne-Year Exposure from the LZ Experiment

We report results from searches for new physics models through electron recoils using data collected by the LUX-ZEPLIN experiment during its first two science runs, with a total exposure of 4.2 tonne−years. The observed data are consistent with a background-only hypothesis. Constraints are derived for electromagnetic interactions of solar neutrinos, solar axionlike particles (ALPs), mirror dark matter, and the absorption of bosonic dark matter candidates. The inverse Primakoff process for 57 Fe deexcitation solar ALPs is considered for the first time. These results represent the most stringent constraints to date on keV-scale Primakoff and 57 Fe solar ALPs, bosonic dark matter, mirror dark matter, and neutrino millicharge, while remaining competitive for the other signal models investigated.

Axion-like particles↗

Thermally induced PtOx interfacial layer enhances stability of Pt/β-Ga2O3 vertical Schottky diodes

This study investigates the long-term stability of Pt/β-Ga2O3 field-plated Schottky barrier diodes at high temperatures, with extended thermal cycling and soaking stress. The device characteristics reveal a strong dependence on operating temperature, leading to an ON/OFF current ratio of ∼10× at ±3 V and 600 °C. Extensive thermal cycling (25 cycles over 100 h) between room temperature and 350 °C shows that leakage currents stabilize after the initial ten cycles. This stabilization is likely due to the formation of a thin PtOx layer at the Pt/β-Ga2O3 interface, as confirmed by high-resolution scanning transmission electron microscopy. Further exposure to a constant 350 °C environment for 10 h reveals a slight increase in the leakage current from 10−7 to 10−6 A at −5 V and degradation of the forward current, due to potential thermodynamic instability of the Ohmic contacts. This study provides insights into the changes in the Pt/β-Ga2O3 diode performance with thermal stress, offering a basis for predicting the device’s operational reliability at high temperatures for sensing and power applications.

08 HYDROGEN↗

In Situ Analysis of Electron-Induced Chemical Transformations in Vapor-Phase-Synthesized Al-Based Inorganic–Organic Hybrid Thin Films for EUV Resist Platform

The rapid advancement and stringent requirements of extreme ultraviolet (EUV) lithography technology necessitate the development of advanced photoresist systems for next-generation microelectronics. Recent studies have demonstrated that inorganic-based hybrid photoresists offer notable improvements in EUV sensitivity, etch resistance, and greater insusceptibility to pattern collapse compared to their purely organic counterparts. However, variations in the synthesis/coating approaches and chemistry of inorganic–organic photoresists can result in distinct exposure mechanisms. In this work, an Al-based hybrid thin film resist system synthesized via molecular (atomic) layer deposition (MLD or MALD) is explored, focusing on its electron-beam and EUV patterning mechanisms. The Al-based hybrid thin films are deposited using trimethylaluminum (TMA) and the organic precursor hydroquinone, exhibiting a saturated growth rate within the temperature range of 150–200°C. In diluted tetramethylammonium hydroxide (TMAH)-based developer solutions, the electron-irradiated Al-based hybrid thin film system behaves as a negative tone resist, achieving a sensitivity of 10.4 mC/cm 2 at 0.1 kV electron beam lithography (EBL). Chemical changes induced by electron exposure are also analyzed in this study using X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and a unique infrared spectroscopy setup, revealing the potential cross-linking pathways. To further correlate the electron-induced chemical transformations with those mediated by EUV irradiations, a combination of X-ray photoemission electron microscopy/low-energy electron microscopy (XPEEM/LEEM) system is also employed. In conclusion, this study provides critical insights into the mechanisms underlying solubility switching and contributes to the design of advanced resist materials for EUV lithography.

36 MATERIALS SCIENCE↗

Two-neutrino double electron capture of 124 Xe in the first LUX-ZEPLIN exposure

The broad physics reach of the LUX-ZEPLIN (LZ) experiment covers rare phenomena beyond the direct detection of dark matter. We report precise measurements of the extremely rare decay of 124Xe through the process of two-neutrino double electron capture, utilizing a 1.39 kg × yr isotopic exposure from the first LZ science run. A half-life of $T$$^{2v2EC}_{1/2}$ = (1.09 ± 0.14 stat ± 0.05 sys ) x 10 22 yr is observed with a statistical significance of 8.3σ, in agreement with literature. First empirical measurements of the KK capture fraction relative to other K-shell modes were conducted, and demonstrate consistency with respect to recent signal models at the 1.4σ level.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Redistribution of Ru in Fe 2 O 3 –Ru Nanocatalysts through an Oxidative Pretreatment Improves Reverse Water–Gas Shift Activity

We have synthesized Fe–Ru nanoparticles via a solvothermal method to create catalysts for the reverse water–gas shift reaction and demonstrated the impact of reductive and oxidative pretreatments on both catalytic performance and structure. Catalytic testing showed improved activity after exposure to O 2 at 600 °C. In contrast, the activity became lower if then exposed to H 2 at 600 °C. Environmental scanning transmission electron microscopy and scanning electron microscopy showed that exposure to O 2 at 600 °C changes the morphology and completely oxidizes Fe into Fe 2 O 3 . Exposure to H 2 at elevated temperature caused Ru coalescence at the surface of the nanoparticle, forming clusters which decreased the optimization of Ru. Reoxidation of the particles exposed to H 2 , however, caused a redistribution of Ru that appears beneficial in maximizing Ru exposure and synergy with Fe oxide, with no major changes in the morphology and oxide structure. Furthermore, our diagnostics demonstrate the complex and reversible rearrangements possible in these multicomponent particles and the benefits of oxidative pretreatment to enhance or regenerate Fe–Ru catalysts in other important catalytic reactions such as Fischer–Tropsch synthesis.

Fe−Ru nanoparticles↗

Studying single-electron traps in newly fabricated Skipper-CCDs for the Oscura experiment using the pocket-pumping technique

Understanding and characterizing very low-energy (⁠ ∼eV) background sources is a must in rare-event searches. Oscura, an experiment aiming to probe electron recoils from sub-GeV dark matter using a 10 kg skipper-CCD detector, has recently fabricated its first two batches of sensors. In this work, we present the characterization of defects/contaminants identified in the buried-channel region of these newly fabricated skipper-CCDs. These defects/contaminants produce deferred charge from trap emission in the images next to particle tracks, which can be spatially resolved due to the sub-electron resolution achieved with these sensors. Using the trap-pumping technique, we measured the energy and cross section associated with these traps in three Oscura prototype sensors from different fabrication batches which underwent different gettering methods during fabrication. Results suggest that the type of defects/contaminants is more closely linked to the fabrication batch rather than to the gettering method used. The exposure-dependent single-electron rate (SER) of one of these sensors was measured ∼100 m underground, yielding (1.8±0.3)×10−3e−/pix/day at 131 K. The impact of the identified traps on the measured exposure-dependent SER is evaluated via a Monte Carlo simulation. Results suggest that the exposure-dependent SER of Oscura prototype sensors would be lower in lower background environments as expected.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Online Dynamic Cyber-Attack Diagnosis in Power Electronics Systems Based on Few-Shot Learning

With increasing exposure to software-based sensing and control, power electronics systems are facing higher risks of cyber-physical attacks. To ensure system stability and minimize potential economic losses, it is critical to monitor the operating states and detect those attacks at the early stage. However, anomaly detection and diagnosis of attacks are still challenging, especially when labeled anomaly data is difficult or even infeasible to obtain. To overcome this problem, we propose a Few-Shot Learning (FSL) based approach for cyber-attack diagnosis leveraging the waveform data. To the best of our knowledge, this work is the first attempt at leveraging FSL for cyber-attack diagnosis in power electronics systems. Extensive experimental results demonstrate that our proposed approach can achieve comparable diagnosis accuracy with the state-of-the-art data-driven methods using less than 0.04% of the training samples.

Li, Qi↗

Combining four-point bending and corrosion to map stress-dependent corrosion susceptibility of 316H stainless steel in FLiNaK

Understanding the effect of stress on the corrosion of steels in molten salts is important for material screening and safety assessment of molten salt reactors. We present a method that combines four-point bending with corrosion testing, enabling the mapping of corrosion susceptibility as a function of local stress from a single specimen. Guided by finite element analysis, a four-point bending setup was used to bend a 316H stainless-steel bar under controlled elastic stress during a 100-hour exposure in FLiNaK at 700 °C. Post-exposure characterization using scanning electron microscopy and energy-dispersive X-ray spectroscopy revealed a pronounced correlation between stress and corrosion. Regions under tensile stress exhibited significantly deeper attack depths and greater chromium depletion along grain boundaries, whereas compressive zones showed shallower corrosion cracks. The stress effect is attributed to stress concentration under tensile loading, which promotes chromium dissolution and crack propagation. This technique can be readily applied to other structural alloys, enabling quantitative measurement of corrosion susceptibility as a function of local stress.

316H↗

Mechanism of Vapor-Phase Infiltration of Organometallic Hf in Poly(Methyl Methacrylate) for Hybrid Resist Applications

Inorganic–organic hybrid thin films synthesized by vapor-phase infiltration (VPI) of metal oxides into organic photoresists, such as poly(methyl methacrylate) (PMMA), have recently demonstrated their utility in extreme ultraviolet lithography, critical for angstrom-era semiconductor device miniaturization. Hafnium oxide infiltration has been reported recently for this purpose, but its detailed VPI mechanism has remained largely unexplored. In this study, we investigated the VPI characteristics and mechanisms of tetrakis(dimethylamido)hafnium (TDMAHf)─the hafnium precursor predominantly used for VPI in the field─into PMMA and examined its impact on electron-beam lithography (EBL) exposure behavior. VPI was performed at temperatures ranging from 85 to 150 °C, with chemical interactions characterized using infrared reflection-absorption spectroscopy, and resist patterning performance was evaluated through EBL dose-sensitivity assessments. The results indicate that TDMAHf forms a reversible adduct with PMMA at temperatures up to 120 °C, whereas at 150 °C, covalent bond formation occurs, most likely via dealkylation that leads to acetate formation. EBL studies reveal that resist sensitivity is influenced by both infiltration temperature and developer selection, with aqueous isopropyl alcohol development demonstrating enhanced sensitivity compared to organic solvent-based development. The optimized infiltration protocol at 120 °C ensures a uniform inorganic distribution without compromising resist dissolution. These findings not only help refine hybrid resist patterning performance but also offer insights potentially applicable to the VPI of other homoleptic metal-amide organometallic VPI precursors that include TDMA ligands.

36 MATERIALS SCIENCE↗