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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays

Characterizing and controlling the uniformity of nanoparticles is crucial for their application in science and technology because crystalline defects in the nanoparticles strongly affect their unique properties. Recently, ultra-short and ultra-bright X-ray pulses provided by X-ray free-electron lasers (XFELs) opened up the possibility of structure determination of nanometre-scale matter with Å spatial resolution. However, it is often difficult to reconstruct the 3D structural information from single-shot X-ray diffraction patterns owing to the random orientation of the particles. This report proposes an analysis approach for characterizing defects in nanoparticles using wide-angle X-ray scattering (WAXS) data from free-flying single nanoparticles. The analysis method is based on the concept of correlated X-ray scattering, in which correlations of scattered X-ray are used to recover detailed structural information. WAXS experiments of xenon nanoparticles, or clusters, were conducted at an XFEL facility in Japan by using the SPring-8 Ångstrom compact free-electron laser (SACLA). Bragg spots in the recorded single-shot X-ray diffraction patterns showed clear angular correlations, which offered significant structural information on the nanoparticles. The experimental angular correlations were reproduced by numerical simulation in which kinematical theory of diffraction was combined with geometric calculations. We also explain the diffuse scattering intensity as being due to the stacking faults in the xenon clusters.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2023

Characterizing Density and Spatial Distribution of Trap States in Ta 3 N 5 Thin Films for Rational Defect Passivation

Tantalum nitride (Ta 3 N 5 ) has gained significant attention as a potential photoanode material, yet it has been challenged by material quality issues. Defect-induced trap states are detrimental to the performance of any semiconductor material. Beyond influencing the performance of Ta 3 N 5 films, defects can also accelerate the degradation in water during desired electrochemical applications. Defect passivation has provided an enormous boost to the development of many semiconductor materials but is currently in its infancy for Ta 3 N 5 . This is in part due to a lack of experimental understanding regarding the spatial and energetic distribution of trap states throughout Ta 3 N 5 thin films. Here, we employ drive-level capacitance profiling (DLCP) to experimentally resolve the spatial and energetic distribution of trap states throughout Ta 3 N 5 thin films. The density of deeper energetic traps is found to reach ∼2.5 to 6 × 10 22 cm –3 at the interfaces of neat Ta 3 N 5 thin films, over an order of magnitude greater than the bulk. In addition to the spatial profile of deep trap states, we report neat Ta 3 N 5 thin films to be highly n-type in nature, owning a free carrier density of ∼9.74 × 10 17 cm –3 . This information, coupled with the present understanding of native oxide layers on Ta 3 N 5 , has facilitated the rational design of a targeted passivation strategy that simultaneously provides a means for catalyst immobilization. Loading catalyst via silatrane moieties suppresses the density of defects at the surface of Ta 3 N 5 thin films by two orders of magnitude, while also reducing the free carrier density of films by over one order of magnitude, effectively dedoping the films to ∼2.40 × 10 16 cm –3 . The surface passivation of Ta 3 N 5 films translates to suppressed defect-induced trapping and recombination of photoexcited carriers, as determined through absorption, photoluminescence, and transient photovoltage. Here, this illustrates how developing a deeper understanding of the distribution and influence of defects in Ta 3 N 5 thin films has the potential to guide future works and ultimately accelerate the integration and development of high-performance Ta 3 N 5 thin film devices.

defect passivation↗
DOE OSTI2024

Identification and Suppression of Point Defects in Bromide Perovskite Single Crystals Enabling Gamma‐Ray Spectroscopy

Abstract Methylammonium lead tribromide (MAPbBr 3 ) stands out as the most easily grown wide‐band‐gap metal halide perovskite. It is a promising semiconductor for room‐temperature gamma‐ray ( γ ‐ray) spectroscopic detectors, but no operational devices are realized. This can be largely attributed to a lack of understanding of point defects and their influence on detector performance. Here, through a combination of crystal growth design and defect characterization, including positron annihilation and impedance spectroscopy, the presence of specific point defects are identified and correlated to detector performance. Methylammonium (MA) vacancies, MA interstitials, and Pb vacancies are identified as the dominant charge‐trapping defects in MAPbBr 3 crystals, while Br vacancies caused doping. The addition of excess MABr reduces the MA and Br defects and so enables the detection of energy‐resolved γ ‐ray spectra using a MAPbBr 3 single‐crystal device. Interestingly, the addition of formamidinium (FA) cations, which converted to methylformamidinium (MFA) cations by reaction with MA + during crystal growth further reduced MA defects. This enabled an energy resolution of 3.9% for the 662 keV 137 Cs line using a low bias of 100 V. The work provides direction toward enabling further improvements in wide‐bandgap perovskite‐based device performance by reducing detrimental defects.

Ni, Zhenyi↗
DOE OSTI2020

Characterizing Dislocation Defects in Dark Field X-ray Microscopy Images of Bulk Aluminum

Material defects play a large role in material response under shock loading, yet the process of how these defects initiate, propagate, and annihilate is not well understood. Using a newly developed diagnostic, dark field X-ray microscopy (DFXM), we can now visualize the behavior of dislocation defects in materials at the mesoscale under varying conditions. Using data from the European Synchrotron Radiation Facility, we apply a variety of image processing techniques to capture relevant features to locate and characterize size and orientation of dislocation defects in bulk aluminum DFXM images. Beyond simple visualization, this analysis drives statistical characterization of the defects and their dynamic response to further improve the relevant physics models.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2023

Two disulfide-reducing pathways are required for the maturation of plastid c -type cytochromes in Chlamydomonas reinhardtii

Abstract In plastids, conversion of light energy into ATP relies on cytochrome f, a key electron carrier with a heme covalently attached to a CXXCH motif. Covalent heme attachment requires reduction of the disulfide-bonded CXXCH by CCS5 and CCS4. CCS5 receives electrons from the oxidoreductase CCDA, while CCS4 is a protein of unknown function. In Chlamydomonas reinhardtii, loss of CCS4 or CCS5 yields a partial cytochrome f assembly defect. Here, we report that the ccs4ccs5 double mutant displays a synthetic photosynthetic defect characterized by a complete loss of holocytochrome f assembly. This defect is chemically corrected by reducing agents, confirming the placement of CCS4 and CCS5 in a reducing pathway. CCS4-like proteins occur in the green lineage, and we show that HCF153, a distant ortholog from Arabidopsis thaliana, can substitute for Chlamydomonas CCS4. Dominant suppressor mutations mapping to the CCS4 gene were identified in photosynthetic revertants of the ccs4ccs5 mutants. The suppressor mutations yield changes in the stroma-facing domain of CCS4 that restore holocytochrome f assembly above the residual levels detected in ccs5. Because the CCDA protein accumulation is decreased specifically in the ccs4 mutant, we hypothesize the suppressor mutations enhance the supply of reducing power through CCDA in the absence of CCS5. We discuss the operation of a CCS5-dependent and a CCS5-independent pathway controlling the redox status of the heme-binding cysteines of apocytochrome f.

Genetics & Heredity↗
DOE OSTI2025

Comprehensive defect evaluation of advanced nuclear fuels using high-resolution acoustic signals and optimized sensor separation

Graphite pebble composite structures based on TRistructural-ISOtropic (TRISO) particles are being developed as core nuclear fuels in advanced power reactors, promising safe operation at increased temperatures. Ensuring the structural integrity of these nuclear fuels requires comprehensive and accurate non-destructive evaluation (NDE) techniques to characterize defects and damage in the pebbles. However, traditional acoustic evaluation methods face limitations in defect characterization due to the highly attenuative, and geometrically and compositionally complex nature of these structures. This study proposes an improved acoustic NDE technique for accurate detection and classification of anticipated relevant defects and damage in graphite pebbles using high-resolution acoustic signals and optimized transmit-receive sensor networks. The proposed approach utilizes a triangular three-sensor network as the base unit, comprising three transmit-receive sensors. The sensor separation distance, as well as acoustic excitation center frequency, pulse-width, and bandwidth are optimized to enhance spatial resolution and improve signal-to-noise ratio, enabling effective characterization of the smallest size and widest range of defects in pebbles. Furthermore, the use of the triangular sensor configuration instead of a more conventional transmit-receive sensor pair expands the inspection region from a one-dimensional linear path to a two-dimensional area, increasing spatial coverage. To mitigate challenges associated with processing of complex acoustic signals arising from high-frequency, high-bandwidth excitation in these structures, a machine-learning-based signal processing algorithm is integrated with the sensor network. In the machine-learning-based algorithm, multi-domain features are extracted from the acoustic signals to capture intricate signal characteristics, significantly improving defect identification and classification compared to traditional approaches. The proposed acoustic NDE technique offers considerable promise for practical and reliable defect/damage diagnostics of advanced nuclear pebble fuels.

42 ENGINEERING↗
DOE OSTI2024

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Multiscale characterization and representation of variability in ceramic matrix composites

Low density, high strength, and high creep and oxidation resistance properties of ceramic matrix composites (CMCs) make them an ideal choice for use in extreme environments in space and military applications. This paper presents a detailed characterization study of structural and manufacturing flaws in Carbon fiber Silicon-Carbide-Nitride matrix (C/SiNC) CMCs at different length-scales. Energy-dispersive spectroscopy (EDS) is used for the chemical characterization of the material’s elemental constituents. High-resolution multiscale graphs obtained from scanning electron microscope (SEM) and confocal laser scanning microscope (LSM) are used to characterize the distribution and morphology of defects at different length scales. This is followed by the classification and quantification of the common manufacturing defects. An image processing algorithm based on the image segmentation process is developed to quantify the variability of various scale-dependent architectural parameters. Finally, a three-dimensional stochastic representative volume element (SRVE) generation algorithm is developed to provide precise representations of material textures at multiple length scales. The developed algorithm accurately accounts for material features and flaws based on a range of multiscale structural and defects characterization results.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evaluation of Flaw Detection with SLDV Methods Before/After Mechanical Patch

This report provides a summary of the testing and the experiments to evaluate the utility of laser ultrasonic testing (UT) in detecting and characterizing defects on the surface of steel plates before and after the application of an engineered composite patch for crack repair. Included are the detection and characterization of defects from a section of welded plate material taken from the Sandia National Laboratories’ full-size mockup of a spent nuclear fuel (SNF) dry storage canister which had been pre-flawed and exposed to deliquescent sea salt conditions for 2 years. The information includes a review of previously reported metallurgical characterization, and new work on detailed surface characterization of the corrosion attack using laser UT.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Strain-Driven Evolution of Structural and Carrier Recombination Dynamics in Germanium

Strain engineering in group-IV semiconductors, in particular germanium (Ge), offers a promising route for advancing next-generation optoelectronic device performance. High minority carrier lifetime serves as a direct indicator of superior material quality and device efficiency. Several factors govern the minority carrier lifetime in both strained Ge and strained GeSn, such as strain level, epilayer thickness, defects, surface roughness, and Sn alloying. In this study, the impact of biaxial strain on effective minority carrier lifetimes of tensile-strained Ge (0% ..epsilon..-Ge/Al?As, 0.78% ..epsilon..-Ge/In0.115?Ga0.885?As, and 0.93% ..epsilon..-Ge/In0.16?Ga0.84?As) and compressively strained GeSn (-0.53% c-Ge0.97?Sn0.03/Al?As) epilayers, grown by molecular beam epitaxy, was experimentally investigated via the microwave-reflection photoconductive decay (..mu..-PCD) technique as a simultaneous function of thickness and strain. The structural and strain-relaxation properties were analyzed by high-resolution x-ray diffraction and Raman spectroscopy, while surface morphology analysis using atomic force microscopy provided insights into the surface roughness of strained Ge-based epilayers. Defect characterization by cross-section transmission electron microscopy revealed superior crystalline quality of ..epsilon..-Ge in one epilayer, while twin boundary formation was observed in the other. We investigated the carrier recombination dynamics in epitaxially strained Ge by extracting the bulk recombination lifetime and surface recombination velocity using the thickness-dependent minority carrier lifetime. High effective minority carrier lifetimes of approximately 60-340 ns were achieved at high strain levels with minimal dependence on the thickness of the strained Ge-based epilayers by means of the ..mu..-PCD technique. Minority carrier lifetimes in Ge-based epilayers exhibit a quadratic dependence on the biaxial strain, ranging from -0.88% (compressive) to +1.6% (tensile). The analysis of the carrier recombination dynamics in strained Ge-based heterostructures offers a pathway to designing group-IV based optoelectronic devices.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Detecting keyhole porosity and monitoring process signatures in additive manufacturing: an in situ pyrometry and ex situ X-ray radiography correlation

Creation of pores and defects during laser powder bed fusion (LPBF) can lead to poor mechanical properties and thus must be minimized. Post-build inspection is required to ensure the printed parts contain acceptably low defect concentrations. These inspections are time consuming and costly, especially for large or complex parts. As a potential solution, in situ process monitoring can be used to detect the creation of defects, characterize local material behavior and predict expected component properties. However, the precise relationship between pore creation and in situ process monitoring still needs to be understood. In this work, high-speed infrared diode-based pyrometry and high-speed optical imaging signals were used to monitor LPBF printing of 446 stainless steel 316 L single tracks with varying laser power and velocity. Results indicate an increase in pyrometer signal and melt pool dimensions with increasing laser power and decreasing velocity in agreement with previous work. In addition, careful analysis of pyrometer signal reveals a distinct signature of the conduction-to-keyhole mode transition which was confirmed by metallography. Critically, pore defect initiation as characterized by ex situ X-ray radiography was correlated with in situ thermal monitoring signals to derive the probability of defect creation. Our results show that, in principle, a probabilistic prediction of pore formation can be achieved based on in situ high-speed pyrometry monitoring of the LPBF melt pool.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Ultrahigh‐Flux X‐ray Detection by a Solution‐Grown Perovskite CsPbBr 3 Single‐Crystal Semiconductor Detector

Abstract Solution‐processed perovskites are promising for hard X‐ray and gamma‐ray detection, but there are limited reports on their performance under extremely intense X‐rays. Here, a solution‐grown all‐inorganic perovskite CsPbBr 3 single‐crystal semiconductor detector capable of operating at ultrahigh X‐ray flux of 10 10 photons s −1 mm −2 is reported. High‐quality solution‐grown CsPbBr 3 single crystals are fabricated into detectors with a Schottky diode structure of eutectic gallium indium/CsPbBr 3 /Au. A high reverse‐bias voltage of 1000 V (435 V mm − 1 ) can be applied with a small and stable dark current of ≈60–70 nA (≈9–10 nA mm − 2 ), which enables a high sensitivity larger than 10 000 µC Gy air −1 cm − 2 and a simultaneous low detection limit of 22 nGy air s − 1 . The CsPbBr 3 semiconductor detector shows an excellent photocurrent linearity and reproducibility under 58.61 keV synchrotron X‐rays with flux from 10 6 to 10 10 photons s − 1 mm − 2 . Defect characterization by thermally stimulated current spectroscopy shows a similar low defect density of a synchrotron X‐ray and a lab X‐ray irradiated device. Solid‐state nuclear magnetic resonance spectroscopy suggests that the excellent performance of the solution‐grown CsPbBr 3 single crystal may be associated with its good short‐range order, comparable to the spectrometer‐grade melt‐grown CsPbBr 3 .

Pan, Lei↗
DOE OSTI2022

A combined theoretical-experimental investigation of thermal transport in low-dose irradiated thorium dioxide

During reactor operation, nuclear fuels are subject to extreme temperature and irradiation conditions which can significantly degrade the fuel's thermal transport properties. The reduction in thermal conductivity of the fuel as a result of irradiation-induced lattice defects is arguably the most important fuel performance metric in regard to reactor efficiency and safety. Because thorium dioxide (ThO2) is suitable as a model system for more complex materials such as UO2 and its mixed oxides, we present a theoretical investigation of thermal conductivity reduction seen in defect-bearing thorium dioxide and compare directly to experimental measurements. Phonon-mediated thermal transport of the fuel is modeled by a solution to the Boltzmann transport equation (BTE) for phonons. A cluster dynamics (CD) model for lattice defect evolution during irradiation predicts defect densities which are used as input to the BTE for modeling phonon-defect scatterings. Phonon scatterings by lattice defects include those from point defects and vacancy clusters and interstitial clusters of various sizes. The CD model is benchmarked against structural defect characterization of irradiated thorium dioxide using electron microscopy. Thermal conductivity predicted by the BTE model is compared to measured values for irradiated thorium dioxide specimens below room temperature to isolate effects of phonon-defect scattering from intrinsic 3-phonon processes, which dominate at higher temperatures. The computed conductivity values are in partial agreement at temperatures close to room temperature while slight deviations are observed at the lowest measured temperatures, suggesting that implemented phonon-defect scattering cross-section expressions may not be adequate for low temperatures. The presented work provides a necessary investigation of the influence of irradiation induced defects on fuel performance and represents a first step toward a full characterization of phonon mediated thermal transport in irradiated materials with complex defect microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructurally informed synchrotron x-ray analysis revealing helium defect transitions in ultrafine grained tungsten

The formation of insoluble gaseous defects in materials due to nuclear transmutation or ion implantation involves the diffusion of impurity atoms to form atomic defect clusters that coalesce into bubbles or cavities and ultimately degrade the material properties. Transmission electron microscopy (TEM) is limited in its ability to resolve sub-nanometer gas clusters whereas X-ray diffraction (XRD) provides information pertaining to local atomic changes. Here, in this study, helium (He) implanted ultrafine grained tungsten is explored through a multimodal defect characterization campaign combining TEM-informed Small Angle X-ray Scattering (SAXS) analysis, XRD lattice parameter measurements, and nanoscale He cluster quantification from a region of reciprocal space accessible via Wide Angle X-ray Scattering (WAXS). Moderate elevated temperature implantations are shown to produce high concentrations of sub-nanoscale He clusters and small, homogeneously distributed cavities, which collectively are linked to lattice expansion and further substantiated through complementary atomistic simulations. Increased implantation temperatures encourage the diffusion of these defects to the grain boundaries (GBs), leading to lattice relaxation and the growth of large GB cavities manifesting as bimodal size distributions in the SAXS analysis. Overall, our results demonstrate the utility of multimodal synchrotron X-ray analysis in bridging the gap between microscale He cavity quantification and atomic-scale defect analysis.

36 MATERIALS SCIENCE↗