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At least 415 records · Page 23

NSUF Rad-AFM: Nanoscale Material Property Measurements of Radioactive Materials

Many advances in our understanding of radiation induced damage mechanisms are due to imaging techniques including transmission electron microscopy and scanning electron microscopy. However, the effect of these radiation induced defects characterized on the atomic to micrometer scale are often interpreted by changes in bulk material properties measured in the hundreds of microns to cm scale. In order to bridge this gap, additional tools need to be developed for use with radioactive materials. To this end a new Asylum Infinity multimodal atomic force microscope (AFM) has been added to the library of Nuclear Science User Facility (NSUF) instruments for use on radioactive materials. This instrument is housed in the Radiochemical Processing Laboratory (RPL) which is a Department of Energy Hazard Category II Non-Reactor Nuclear Facility operated by Battelle at Pacific Northwest National Laboratory. This allows for the handling, sample preparation, and characterization of highly radioactive materials providing a unique capability to understand fundamental properties of nuclear materials and the effects of radiation induced damage.

Riechers, Shawn L.↗

Accelerating Discovery of Atomistic Defects via Machine Learning

The quantification of defects such as vacancies in crystalline structures is a cornerstone of materials science research. Traditional efforts often rely on manual detection, a process that is time-intensive, prone to human error, and challenging to scale. Here we leverage machine learning (ML) methods to identify and quantify vacancies within a crystalline lattice, aiming to expedite detection while improving accuracy. Additionally, we explore the transferability of these ML techniques, identifying characteristics of atomistic imaging data that complicate this task. We show how the integration of ML can drive innovation, providing a powerful tool that will play an increasingly crucial role in the future of materials science.

2D materials↗

Radiation effects in soils from five lunar missions.

Optical and high-voltage electron microscopy were used to study radiation-produced defects. There is no systematic decrease in solar flare track distributions in lunar fines even to a depth of 2.5 m. The soil gradually accumulates in thickness; stirring by impacts is usually on a small scale. The accumulation rate at Luna 16 site is far lower than at the Apollo sites; the mean track density in micron-size grains there exceeds one trillion per sq cm; more than 90% of those grains are metamict; the Luna 16 site is at high longitude where electrostatic charging and transport of soil by geomagnetic tail electrons are minimal. A large fraction of soil grains on sloping ground have been isotropically irradiated, suggesting a tumbling downhill motion.-

Phakey, P. P.↗

Effects of Ambient High Temperature Exposure on Alumina-Titania High Emittance Surfaces for Solar Dynamic Systems

Solar dynamic (SD) space power systems require durable, high emittance surfaces on a number of critical components, such as heat receiver interior surfaces and parasitic load radiator (PLR) elements. To enhance surface characteristics, an alumina-titania coating has been applied to 500 heat receiver thermal energy containment canisters and the PLR of NASA Lewis Research Center's (LeRC) 2 kW SD ground test demonstrator (GTD). The alumina-titania coating was chosen because it had been found to maintain its high emittance under vacuum (less than or equal to 10(exp -6) torr) at high temperatures (1457 F (827 C)) for an extended period (approximately 2,700 hours). However, preflight verification of SD systems components, such as the PLR require operation at ambient pressure and high temperatures. Therefore, the purpose of this research was to evaluate the durability of the alumina-titania coating at high temperature in air. Fifteen of sixteen alumina-titania coated Incoloy samples were exposed to high temperatures (600 F (316 C) to l500 F (816 C)) for various durations (2 to 32 hours). Samples, were characterized prior to and after heat treatment for reflectance, solar absorptance, room temperature emittance and emittance at 1,200 F (649 C). Samples were also examined to detect physical defects and to determine surface chemistry using optical microscopy, scanning electron microscopy operated with an energy dispersive spectroscopy (EDS) system, and x ray photoelectron spectroscopy (XPS). Visual examination of the heat-treated samples showed a whitening of samples exposed to temperatures of 1,000 F (538 C) and above. Correspondingly, the optical properties of these samples had degraded. A sample exposed to 1,500 F (816 C) for 24 hours had whitened and the thermal emittance at 1,200 F (649 C) had decreased from the non-heat treated value of 0.94 to 0.62. The coating on this sample had become embrittled with spalling off the substrate noticeable at several locations. Based on this research it is recommended that preflight testing of SD components with alumina-titania coatings be restricted to temperatures no greater than 600 F (316 C) in air to avoid optical degradation. Moreover, components with the alumina-titania coating are likely to experience optical property degradation with direct atomic oxygen exposure in space.

deGroh, Kim K.↗

Near-Infrared Photon-Counting Camera for High-Sensitivity Observations

The dark current of a transferred-electron photocathode with an InGaAs absorber, responsive over the 0.9-to-1.7- micron range, must be reduced to an ultralow level suitable for low signal spectral astrophysical measurements by lowering the temperature of the sensor incorporating the cathode. However, photocathode quantum efficiency (QE) is known to reduce to zero at such low temperatures. Moreover, it has not been demonstrated that the target dark current can be reached at any temperature using existing photocathodes. Changes in the transferred-electron photocathode epistructure (with an In- GaAs absorber lattice-matched to InP and exhibiting responsivity over the 0.9- to-1.7- m range) and fabrication processes were developed and implemented that resulted in a demonstrated >13x reduction in dark current at -40 C while retaining >95% of the approximately equal to 25% saturated room-temperature QE. Further testing at lower temperature is needed to confirm a >25 C predicted reduction in cooling required to achieve an ultralow dark-current target suitable for faint spectral astronomical observations that are not otherwise possible. This reduction in dark current makes it possible to increase the integration time of the imaging sensor, thus enabling a much higher near-infrared (NIR) sensitivity than is possible with current technology. As a result, extremely faint phenomena and NIR signals emitted from distant celestial objects can be now observed and imaged (such as the dynamics of redshifting galaxies, and spectral measurements on extra-solar planets in search of water and bio-markers) that were not previously possible. In addition, the enhanced NIR sensitivity also directly benefits other NIR imaging applications, including drug and bomb detection, stand-off detection of improvised explosive devices (IED's), Raman spectroscopy and microscopy for life/physical science applications, and semiconductor product defect detection.

Jurkovic, Michael↗

Role of mechanical stress localizations on the radiation hardness of AlGaN/GaN high electron mobility transistors

Multi-material, multi-layered systems such as AlGaN/GaN high electron mobility transistors (HEMTs) contain residual mechanical stresses that arise from sharp contrasts in device geometry and materials parameters. These stresses, which can be either tensile or compressive, are difficult to detect and eliminate because of their highly localized nature. We propose that their high-stored internal energy makes potential sites for defect nucleation sites under radiation, particularly if their locations coincide with the electrically sensitive regions of a transistor. In this study, we validate this hypothesis with molecular dynamic simulation and experiments exposing both pristine and annealed HEMTS to 2.8 MeV Au +3 irradiation. Our unique annealing process uses mechanical momentum of electrons, also known as the electron wind force (EWF) to mitigate the residual stress at room temperature. High-resolution transmission electron microscopy and cathodoluminescence spectra reveal the reduction of point defects and dislocations near the two-dimensional electron gas region of EWF-treated devices compared to pristine devices. The EWF-treated HEMTs showed relatively higher resilience with approximately 10% less degradation of drain saturation current and ON-resistance and 5% less degradation of peak transconductance. Both mobility and carrier concentration of the EWF-treated devices were less impacted compared to the pristine devices. Our results suggest that the lower density of nanoscale stress localization contributed to the improved radiation tolerance of the EWF-treated devices. Intriguingly, the EWF is found to modulate the defect distribution by moving the defects to electrically less sensitive regions in the form of dislocation networks, which act as sinks for the radiation induced defects and this assisted faster dynamic annealing.

AlGaN/GaN HEMTs↗

Kinetics of amorphous defect phases measured through ultrafast nanocalorimetry

Recognition of the role of extended defects on local phase transitions has led to the conceptualization of the defect phase, localized thermodynamically stable interfacial states that have since been applied in a myriad of material systems to realize significant enhancements in material properties. Here, we explore the kinetics of grain boundary confined amorphous defect phases, utilizing the high temperature and scanning rates afforded by ultrafast differential scanning calorimetry to apply targeted annealing/quenching treatments at high rates capable of capturing the kinetic behavior. Four Al-based nanocrystalline alloys, including two binary systems, Al–Ni and Al–Y, and two ternary systems, Al–Mg–Y and Al–Ni–Y, are selected to probe the materials design space (enthalpy of mixing, enthalpy of segregation, chemical complexity) for amorphous defect phase formation and stability, with correlative transmission electron microscopy applied to link phase evolution and grain stability to nanocalorimetry signatures. A series of targeted isothermal annealing heat treatments is utilized to construct a Time–Temperature-Transformation curve for the Al–Ni system, from which a critical cooling rate of 2400 °C/s was determined for the grain boundary confined disordered-to-ordered transition. Finally, a thermal profile consisting of 1000 repeated annealing sequences was created to quantify the recovery of the amorphous defect phase following sequential annealing treatments, with results indicating remarkable microstructural stability after annealing at temperatures above 90% of the melting temperature. This work contributes to a deeper understanding of grain boundary localized thermodynamics and kinetics, with potential implications for the design and optimization of advanced materials with enhanced stability and performance.

Amorphous defect phases↗

Structure and strain relaxation effects of defects in In{sub x}Ga{sub 1–x}N epilayers

The formation of trench defects is observed in 160 nm-thick In{sub x}Ga{sub 1–x}N epilayers with x≤0.20, grown on GaN on (0001) sapphire substrates using metalorganic vapour phase epitaxy. The trench defect density increases with increasing indium content, and high resolution transmission electron microscopy shows an identical structure to those observed previously in InGaN quantum wells, comprising meandering stacking mismatch boundaries connected to an I₁-type basal plane stacking fault. These defects do not appear to relieve in-plane compressive strain. Other horizontal sub-interface defects are also observed within the GaN pseudosubstrate layer of these samples and are found to be pre-existing threading dislocations which form half-loops by bending into the basal plane, and not basal plane stacking faults, as previously reported by other groups. The origins of these defects are discussed and are likely to originate from a combination of the small in-plane misorientation of the sapphire substrate and the thermal mismatch strain between the GaN and InGaN layers grown at different temperatures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Light Microscopy Module Biophysics - 4 (LMM-B4)

Compare incorporation of protein aggregates into growing protein crystals on ISS (International Space Station) and on Earth. Measure growth rates in 1g (1 gravity) versus microgravity (micro-g) for different size aggregates of proteins. Compare the defect density and crystal quality via fluorescent-based atomic force microscopy and X-ray diffraction quality of crystals grown at different rates in a 1g environment.

Penn, Benjamin G.↗

In Situ Visualization of the Pinning Effect of Planar Defects on Li Ion Insertion

Longevity of Li ion batteries strongly depends on the interaction of transporting Li ions in electrode crystals with defects. However, detailed interactions between the Li ion flux and structural defects in the host crystal remain obscure due to the transient nature of such interactions. Here, by in situ transmission electron microscopy and density function theory calculations, we reveal how the diffusion pathways and transport kinetics of a Li ion can be affected by planar defects in a tungsten trioxide lattice. We uncover that changes in charge distribution and lattice spacing along the planar defects disrupt the continuity of ion conduction channels and dramatically increase the energy barrier of Li diffusion, thus, arresting Li ions at the defect sites and twisting the lithiation front. In conclusion, the atomic-scale understanding holds critical implications for rational interface design in solid-state batteries and solid oxide fuel cells.

25 ENERGY STORAGE↗

Non-invasive airway health measurement using synchrotron x-ray microscopy of high refractive index glass microbeads

Cystic fibrosis (CF) is caused by a gene defect that compromises the ability of the mucociliary transit (MCT) system to clear the airways of debris and pathogens. To directly characterise airway health and the effects of treatments we have developed a synchrotron X-ray microscopy method that non-invasively measures the local rate and patterns of MCT behaviour. Although the nasal airways of CF mice exhibit the CF pathophysiology, there is evidence that nasal MCT is not altered in CF mice1. The aim of this experiment was to determine if our non-invasive local airway health assessment method could identify differences in nasal MCT rate between normal and CF mice, information that is potentially lost in bulk MCT measurements. Experiments were performed on the BL20XU beamline at the SPring-8 Synchrotron in Japan. Mice were anaesthetized, a small quantity of micron-sized marker particles were delivered to the nose, and images of the nasal airways were acquired for 15 minutes. The nasal airways were treated with hypertonic saline or mannitol to increase surface hydration and MCT. Custom software was used to locate and track particles and calculate individual and bulk MCT rates. No statistically significant differences in MCT rate were found between normal and CF mouse nasal airways or between treatments. However, we hope that the improved sensitivity provided by this technique will accelerate the ability to identify useful CF lung disease-modifying interventions in small animal models, and enhance the development and efficacy of proposed new therapies.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Large-Area Material and Junction Damage in c–Si Solar Cells by Potential-Induced Degradation

This paper reports a new potential-induced degradation (PID) mechanism for crystalline silicon (c-Si), where Na diffuses everywhere and causes large-area material and junction degradation with point defects. Multiple characterization techniques are combined - Kelvin probe force microscopy, electron-beam induced current, dark lock-in thermography, transmission electron microscopy, time-of-flight secondary-ion mass spectrometry, and microwave photoconductance decay - as well as density functional theory (DFT) calculations. These characterization techniques and theoretical calculations are complementary in various aspects of a material's chemical, structural, electrical, and optoelectrical nature, as well as in atomic, nanometer, micrometer, millimeter, and cell and module scales. All results point consistently to a new discovery: substantial large-area deterioration of materials and junctions play a major role in c-Si PID (in addition to the previously reported local shunting defect caused by Na diffusion to planar defects). Furthermore, this new finding reveals a key PID component and leads to a new strategy for tailoring c-Si photovoltaics to ultimately resolve the PID issue.

14 SOLAR ENERGY↗

Investigation on Explosive Welding of Zr{sub 53}Cu{sub 35}Al{sub 12} Bulk Metallic Glass with Crystalline Copper

A Zr{sub 53}Cu{sub 35}Al{sub 12} bulk metallic glass (BMG) was welded to a crystalline Cu using explosive welding technique. The morphology and the composition of the composite were characterized using optical microscopy, scanning electron microscopy, energy-dispersive x-ray spectroscopy and transmission electron microscopy. The investigation indicated that the BMG and Cu were tightly joined together without visible defects, and a thin diffusion layer appeared at the interface. The captured jet at the end of the welding region mostly comes from the Cu side. Amorphous and partially crystallized structures have been observed within the diffusion layer, but the BMG in close proximity to the interface still retains its amorphous state. Nanoindentation tests reveal that the interface exhibits an increment in hardness compared with the matrix on both sides.

36 MATERIALS SCIENCE↗

An Electron Backscatter Diffraction (EBSD)-Based Automated Tool for Ceramic Capacitor Grain Size Analysis

Ceramic capacitors continue to be recurring problem parts for NASA, despite best efforts to screen out potential defects and failures through environmental and electrical testing and nondestructive inspection techniques such as acoustic microscopy. The physical properties of ceramic capacitors necessitates thin dielectric layers capable of withstanding significant electric fields. Any defects in those ceramic layers can result in reduced insulation resistance failure modes including short circuit failures, so the quality and consistency of the dielectric material is critical. The size of the individual ceramic grains in the dielectric material is a critical parameter. However, judging “grain size” is not so simple—in a single capacitor there can be wide variation in grain sizes observed. It is theorized that by studying the grain size distributions of “known good” and “known bad” lots of capacitors, some conclusions could be drawn that would allow us to better predict to the reliability of future lots based on grain size distributions. The initial goal of this effort was to find or develop an automated tool that could inspect a capacitor and return grain size distribution results.

Robert Hodson↗

Study of Bronze Statues “John the Baptist” and “Dancing Cupid” from the Collections of the Pushkin State Museum

Bronze statues “John the Baptist” and “Dancing Cupid” from the collections of the Pushkin State Museum of Fine Arts have been investigated at the National Research Centre “Kurchatov Institute.” These statues were previously damaged in fire. Before carrying out restoration, it was necessary to perform their complex study, including identification of statue materials; elemental and phase analysis of contaminations; estimation of the state of surfaces and internal parts; and detection of technological elements, as well as hidden defects, corroded parts, and cracks. To this end, scanning electron microscopy with X-ray microanalysis, synchrotron radiation diffraction, and neutron radiography and tomography have been used.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Revealing the Hidden Third Dimension of Point Defects in Two-Dimensional MXenes

Point defects govern many important functional properties of two-dimensional (2D) materials. However, resolving the three-dimensional (3D) arrangement of these defects in multi-layer 2D materials remains a fundamental challenge, hindering rational defect engineering. Here, we overcome this limitation using an artificial intelligence-guided electron microscopy workflow to map the 3D topology and clustering of atomic vacancies in Ti3C2TX MXene. Our approach reconstructs the 3D coordinates of vacancies across hundreds of thousands of lattice sites, generating robust statistical insight into their distribution that can be correlated with specific synthesis pathways. This large-scale data enables us to classify a hierarchy of defect structures-from isolated vacancies to nanopores-revealing their preferred formation and interaction mechanisms, as corroborated by molecular dynamics simulations. This work provides a generalizable framework for understanding and ultimately controlling point defects across large volumes, paving the way for the rational design of defect-engineered functional 2D materials.

2D materials↗

Substrate-Dependent Structure, Magnetic, and Ferroelectric Properties of Multiferroic Bi{sub 0.9}Ba{sub 0.1}FeO{sub 3} Thin Film

The structure characteristic of substrate is a key parameter to modify the structure of as-grown thin film and tune physical properties for oxide thin film materials. Three various substrates are selected to identify the change of structure as well as ferroelectric and magnetic properties of the fabricated Bi{sub 0.9}Ba{sub 0.1}FeO{sub 3} thin film. XRD and TEM combined with AFM were used to confirm the detailed structure and epitaxial growth of Bi{sub 0.9}Ba{sub 0.1}FeO{sub 3} thin film on different substrates. Correspondingly, the changes of the ferroelectric and magnetic properties were investigated. It is found that the lattice mismatch between substrate and thin film significantly promotes the structure distortion of Bi{sub 0.9}Ba{sub 0.1}FeO{sub 3} thin film inducing the change of ferroelectric and magnetic properties. Our results further reveal that the structure characteristic of substrate plays a major role in determining the structure of epitaxial thin film and the enhancement of physical properties, which sheds light to understanding the effect of lattice mismatch in many other functional oxide thin films as well.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗