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At least 325 records · Page 18

Characterization and repair of core gap manufacturing defects for wind turbine blades

Various wind turbine blade components, such as shear webs and skins, commonly use fiber-reinforced composite sandwich structures with a core material like balsa or foam. During manufacturing, core gap defects may result from the misalignment of adjacent foam or balsa core sheets in the blade mold. It is important to understand the influence that core gaps have on the structural integrity of wind turbine blades and how to mitigate their influence. This research characterized the effects of core gap defects at the manufacturing and mechanical levels for both epoxy and next-generation thermoplastic composites. Common repair methods were assessed and compared. Multiple defect sizes were compared using temperature data gathered with thermocouples embedded during manufacturing to core gap defect characteristics obtained using image-mapping techniques, optical microscopy, and mechanical characterization by long beam flexure. Results showed that peak exothermic temperatures during curing were closely related to core gap size. The long beam flexure tests determined that transverse core gaps under pure bending loads can have a substantial effect on the ultimate facesheet strength of both epoxy and thermoplastic composite sandwich structures (up to 25% strength reduction), although the size of the defect itself had less of an influence on the magnitude of the strength reduction. The supporting image-mapping techniques indicated that the distortion of the composite facesheets by the core gaps contributed to the premature failures. The repair methods used in this study did very little to improve the ultimate strength of the sandwich panels that previously had core gap defects. The repair of the thermoplastic panel resulted in a further loss in ultimate facesheet strength. This research demonstrated that there is a vital need for the development of a compatible thermoplastic polymer repair resin system and appropriate resin specific repair procedures for the next generation of recyclable thermoplastic wind blades.

17 WIND ENERGY↗

The influence of iron incorporation on the microstructure and crystal chemistry of UO 2 fuel

The incorporation of dopants into UO 2 is of interest for both doped advanced fuel and nuclear forensics research. Suitable forensics dopants, or taggants, for nuclear fuels are ones that do not adversely affect the performance of the parent material while still being traceable during key stages of the fuel’s life cycle. In this paper, we present our efforts to understand the effects of doping UO 2 with Fe 2 O 3 under multiple parameters, such as Fe concentration (0–3000 wppm), sintering temperature (1673 K, 1773 K, and 1973 K), sintering time (2–12 h), and atmosphere (reducing and inert). Here, we investigated densification behavior, microstructure evolution, and lattice defects based on the geometric densities, scanning electron microscopy (SEM), X-ray diffractograms, and Raman spectra. The effect of Fe on the microstructure and crystal chemistry of UO 2 is very complex, especially at the intermediate temperature (1773 K), where we found that densification kinetics are enhanced and that lattice contraction occurs for doping concentrations greater than 1000 wppm Fe.

Crystallography↗

Light-Driven Iodine Loss and Photoluminescence Homogenization in Mixed-Halide Perovskite Semiconductors

Carrier-induced instabilities in lead halide perovskites are often investigated as either transient phenomena, e.g., photoinduced halide segregation or permanent performance changes, e.g., photodegradation, while the mechanistic links between them remain unclear. Here, we aim to connect these observations by studying a model mixed-halide system, MAPb(Br x I 1–x ) 3 . By combining grazing-incidence X-ray diffraction, photothermal deflection spectroscopy, and photoluminescence measurements with hyperspectral microscopy, we investigate the role of mobile halide defects and local chemistry on reversible and long-term instabilities in these materials. Our results show that mixed-halide perovskites are uniquely susceptible to photoinduced changes with illumination driving initial iodide redistribution (i.e., halide segregation), eventual selective iodine expulsion, and subsequent changes in photoinduced halide segregation behavior. By quantifying structural and compositional changes, we estimate an approximately 3–5% iodine loss in our mixed-halide samples after only 24 h of illumination. Further, using microscale measurements, we identify pre-existing iodide-rich domains as key contributors to both the observed transient photostability and permanent iodine loss in MAPbBrI 2 , and see evidence that extended light soaking results in iodide redistribution that improves optoelectronic homogeneity. Overall, our results emphasize the importance of carrier-induced halide oxidation in creating a dynamic defect landscape in mixed-halide perovskites and provide a framework for interpreting apparent light-driven changes in optoelectronic behavior through the lens of permanent compositional changes.

electrical conductivity↗

Surface Nanostructure Control and Thermodynamic Stability Analysis of Femtosecond Laser-Ablated CuCoMn 1.75 NiFe 0.25 Nanoparticles

Surface nanostructure control is the key to functionalizing nanomaterials. This paper presents a characterization with thermodynamic stability analysis of CuCoMn 1.75 NiFe 0.25 high-entropy alloy (HEA) nanoparticles synthesized by femtosecond laser ablation in ethanol and liquid nitrogen (LN2). Using multimodal electron microscopy and spectroscopy, we examine phase, particle size, defect structure, chemical distribution, and surface composition and relate them to HEA stability. Elemental distributions are uniform in both media, but LN2 produces smaller particles with a narrower size distribution and mainly single- or few-domain interiors, whereas ethanol yields larger particles built from 2–4 nm crystallites with domain aggregation. Edge defects appear in both but energy-dispersive X-ray spectroscopy (EDS) is broadly uniform with local fluctuations in ethanol. X-ray photoelectron spectroscopy (XPS), supported by an attenuation model, indicates an ∼1 nm oxide overlayer that suppresses Mn 2p intensity; correcting for it returns Mn toward the bulk value. UV–NIR and photoluminescent spectra independently support a thin oxide shell. Composition-based thermodynamic descriptors place LN2 closer to bulk mixing parameters, while ethanol raises ΔH_mix and lowers Ω. Cooling simulations are consistent (LN2 ∼ 0.1 μs quench, ethanol ∼1 μs). In conclusion, these results connect solvent-controlled kinetics and thermodynamics to crystalline state and surface chemistry, informing surface control of HEA nanoparticles.

Femtosecond Laser Ablation↗

Spontaneous Formation of 1D Pattern in Monolayer VSe 2 with Dispersive Adsorption of Pt Atoms for HER Catalysis

Creation of functional patterns in two-dimensional (2D) materials provides opportunities to extend their potential for applications. Transition-metal dichalcogenides (TMDCs) are suitable 2D materials for pattern generation because of properties including alterable polymorphic phases, easy chalcogen-vacancy formation, metal-atom insertion, and alloying. Such patterning can be used for selective functionalization. Here we report the spontaneous formation of long-range, well-ordered 1D patterns in monolayer vanadium diselenide (VSe 2 ) by a single annealing stage during growth. Atomic-resolution images in real space combined with density-functional-theory (DFT) calculations reveal the 1D features of patterned VSe 2 . Further experimental characterization of the intermediate states in the growth process confirm the spontaneous formation of the 1D pattern by annealing-induced Se-deficient linear defects. The 1D pattern can be reversibly transformed to homogenous VSe 2 monolayer by reintroducing Se atoms. Moreover, additional experiments demonstrate that a dispersive deposition of Pt atoms along the 1D structures of patterned VSe 2 is achieved, while DFT calculations find that their catalytic activity for hydrogen evolution reaction (HER) is as good as that of Pt surfaces. Further, the formation of long-range, well-ordered 1D patterns not only demonstrates an effective way of dimension modulation in 2D materials but also enriches the potential of intrinsically patterned 2D materials for promising catalytic activities.

Chemical structure↗

Atomistic Probing of Defect-Engineered 2H-MoTe 2 Monolayers

Point defects dictate various physical, chemical, and optoelectronic properties of two-dimensional (2D) materials, and therefore, a rudimentary understanding of the formation and spatial distribution of point defects is a key to advancement in 2D material-based nanotechnology. In this work, we performed the demonstration to directly probe the point defects in 2H-MoTe 2 monolayers that are tactically exposed to (i) 200 °C-vacuum-annealing and (ii) 532 nm-laser-illumination; and accordingly, we utilize a deep learning algorithm to classify and quantify the generated point defects. We discovered that tellurium-related defects are mainly generated in both 2H-MoTe 2 samples; but interestingly, 200 °C-vacuum-annealing and 532 nm-laser-illumination modulate a strong n-type and strong p-type 2H-MoTe 2 , respectively. While 200 °C-vacuum-annealing generates tellurium vacancies or tellurium adatoms, 532 nm-laser-illumination prompts oxygen atoms to be adsorbed/chemisorbed at tellurium vacancies, giving rise to the p-type characteristic. This work significantly advances the current understanding of point defect engineering in 2H-MoTe 2 monolayers and other 2D materials, which is critical for developing nanoscale devices with desired functionality.

2H-MoTe 2↗

In-situ visualization of solute-driven phase coexistence within individual nanorods

Nanorods are promising components of energy and information storage devices that rely on solute-driven phase transformations, due to their large surface-to-volume ratio and ability to accommodate strain. Here we investigate the hydrogen-induced phase transition in individual penta-twinned palladium nanorods of varying aspect ratios with ~3 nm spatial resolution to understand the correlation between nanorod structure and thermodynamics. We find that the hydrogenated phase preferentially nucleates at the rod tips, progressing along the length of the nanorods with increasing hydrogen pressure. While nucleation pressure is nearly constant for all lengths, the number of phase boundaries is length-dependent, with stable phase coexistence always occurring for rods longer than 55 nm. Moreover, such coexistence occurs within individual crystallites of the nanorods and is accompanied by defect formation, as supported by in situ electron microscopy and elastic energy calculations. In conclusion, these results highlight the effect of particle shape and dimension on thermodynamics, informing nanorod design for improved device cyclability.

25 ENERGY STORAGE↗

Effect of manganese substitution of ferrite nanoparticles on particle grain structure

To investigate the influence of manganese substitution on the saturation magnetization of manganese ferrite nanoparticles, samples with various compositions (Mn x Fe 3–x O 4 , x = 0, 0.25, 0.5, 0.75, and 1) were synthesized and characterized. The saturation magnetization of such materials was both calculated using density functional theory and measured via vibrating sample magnetometry. A discrepancy was found; the computational data demonstrated a positive correlation between manganese content and saturation magnetization, while the experimental data exhibited an inverse correlation. X-ray diffraction (XRD) and magnetometry results indicated that the crystallite diameter and the magnetic diameter decrease when adding more manganese, which could explain the loss of magnetization of the particles. For 20 nm nanoparticles, with increasing manganese substitution level, the crystallite size decreases from 10.9 nm to 6.3 nm and the magnetic diameter decreases from 15.1 nm to 3.5 nm. Further high resolution transmission electron microscopy (HRTEM) analysis confirmed the manganese substitution induced defects in the crystal lattice, which encourages us to find ways of eliminating crystalline defects to make more reliable ferrite nanoparticles.

36 MATERIALS SCIENCE↗

Defect accommodation in off-stoichiometric (SrTiO 3 ) n SrO Ruddlesden–Popper superlattices studied with positron annihilation spectroscopy

he low dielectric loss underlying the record performance of strained (SrTiO 3 ) n SrO Ruddlesden–Popper films as tunable microwave dielectrics was postulated to arise from (SrO) 2 faults accommodating local non-stoichiometric defects. Here, we explore the effect of non-stoichiometry on (SrTiO 3 ) n SrO using positron annihilation lifetime spectroscopy on a composition series of 300 nm thick n = 6 (Sr 1+δ TiO 3 ) n SrO thin films. These films show titanium-site vacancies across the stoichiometry series, with evidence that TiO x vacancy complexes dominate. Little change in defect populations is observed across the series, indicating the ability of Ruddlesden–Popper phases to accommodate ± 5% off-stoichiometry. This ability for defect accommodation is corroborated by scanning transmission electron microscopy with electron energy loss spectroscopy.

Physics↗

A practical guide for crystal growth of van der Waals layered materials

This Tutorial provides an overview of the techniques that are most commonly utilized to grow bulk van der Waals crystals. The materials discussed were selected to highlight various challenges that are often encountered during crystal growth. Additionally, in relatively equal parts, the text covers melt-based techniques, vapor transport growths, and the characterization of crystal quality with an emphasis on structural and chemical homogeneities. Furthermore, pertinent details are given regarding the growth and characterization of many specific compounds, with examples mostly drawn from our own research, and an effort is made to highlight cases where the growths offer a particular lesson or the conditions have a significant impact on the crystal’s physical properties. A primary goal is to motivate more researchers to grow crystals by providing general descriptions and considerations for different growth techniques and equipment while sharing some of our own lessons learned and best practices for the growth and characterization of layered van der Waals crystals. The Tutorial is not written solely for aspiring crystal growers, however, because any researcher who collaborates with a crystal grower can benefit from having a greater understanding and appreciation of the processes of crystal growth and materials development.

36 MATERIALS SCIENCE↗

Direct Cation Exchange in Monolayer MoS 2 via Recombination-Enhanced Migration

In addition to their unique optical and electronic properties, two-dimensional materials provide opportunities to directly observe atomic-scale defect dynamics. Here we use scanning transmission electron microscopy to observe substitutional Re impurities in monolayer MoS 2 undergo direct exchanges with neighboring Mo atoms in the lattice. Density-functional-theory calculations find that the energy barrier for direct exchange, a process that has only been studied as a diffusion mechanism in bulk materials, is too large for either thermal activation or energy directly transferred from the electron beam. The presence of multiple sulfur vacancies next to the exchanged Re-Mo pair, as observed by electron microscopy, does not lower the energy barrier sufficiently to account for the observed atomic exchange. Instead, the calculations find that a Re dopant and surrounding sulfur vacancies introduce an ever-changing set of deep levels in the energy gap. We propose that these levels mediate an “explosive” recombination-enhanced migration via multiple electron-hole recombination events. As a proof of concept, we also show that Re-Mo direct exchange can be triggered via controlled creation of sulfur vacancies. The present experimental and theoretical findings lay a fundamental framework towards manipulating single substitutional dopants in two-dimensional materials.

36 MATERIALS SCIENCE↗

Tailoring Thermal and Mechanical Performance Through Multimaterial Laser Powder Directed Energy Deposition of Copper and 17-4PH Stainless Steel

This study investigates the additive manufacturing (AM) processing, microstructural evolution, and resulting mechanical and thermal properties of multimaterial components combining 17-4PH stainless steel and pure copper (Cu) fabricated via laser powder directed energy deposition (LP-DED). Conventional tooling steels exhibit limited thermal conductivity, significantly constraining production throughput in high-volume processes. Incorporating Cu, with its superior thermal conductivity, could significantly enhance tool performance, though Cu and steel present metallurgical incompatibilities when processed via AM. A systematic investigation was conducted across compositions ranging from 0 to 100 wt% Cu, revealing critical thresholds influencing solidification behavior, defect formation, microstructure, hardness, and thermal transport. Optical microscopy, electron backscatter diffraction (EBSD), hardness testing, and thermal conductivity measurements provided comprehensive process–structure–property correlations. Severe hot cracking occurred at low-Cu contents (6–25 wt%), aligning generally well with crack susceptibility modeling, with an unexpected discrepancy at 25 wt%. Porosity remained low (≥99% dense) throughout the compositional spectrum. EBSD analysis revealed a transformation from columnar martensitic structures at low-Cu contents to equiaxed FCC Cu-dominated structures at higher Cu concentrations, highlighting the complex microstructural transitions driven by Cu-induced changes in solidification and phase stability. Hardness decreased from 330 HV (pure 17-4PH) to 62 HV (pure Cu), consistent with microstructural changes. Concurrently, thermal conductivity improved substantially from 13.5 W/m K to 367.9 W/m K, emphasizing Cu’s dominant role in thermal transport. The findings highlight the feasibility of leveraging compositional gradients between 17-4PH and Cu to achieve tailored tooling with optimized thermal and mechanical performance.

17-4PH↗

Heterovalent semiconductor structures and devices grown by molecular beam epitaxy

Heterovalent structures consisting of group II-VI/group III-V compound semiconductors offer attractive properties, such as a very broad range of bandgaps, large conduction band offsets, high electron and hole mobilities, and quantum-material properties such as electric-field-induced topological insulator states. These properties and characteristics are highly desirable for many electronic and optoelectronic devices as well as potential condensed-matter quantum-physics applications. Here, we provide an overview of our recent studies of the MBE growth and characterization of zincblende II-VI/III-V heterostructures as well as several novel device applications based on different sets of these materials. By combining materials with small lattice mismatch, such as ZnTe/GaSb (Δa/a~0.13%), CdTe/InSb (Δa/a~0.05%), and ZnSe/GaAs (Δa/a~0.26%), epitaxial films of excellent crystallinity were grown once the growth conditions had been optimized. Cross-sectional observations using conventional and atomic-resolution electron microscopy revealed coherent interfaces and close to defect-free heterostructures. Measurements across CdTe/InSb interfaces indicated a limited amount (~1.5 nm) of chemical intermixing. Results for ZnTe/GaSb distributed Bragg reflectors, CdTe/Mg x Cd 1-x Te double heterostructures, and CdTe/InSb two-color photodetectors are briefly presented, and the growth of a rock salt/zincblende PbTe/CdTe/InSb heterostructure is also described.

Materials Science↗

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↗