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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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In situ characterization of post-synthetic metalation in porous salt thin films
Controlled growth of porous, optically transparent thin films reveals structure- and thickness-dependent effects and enablesin situstudy of post-synthetic metalation kinetics.
High-resolution in-situ characterization of laser powder bed fusion via transmission X-ray microscopy at X-ray free electron lasers
In this work, we describe the instrumentation used to perform the first operando transmission X-ray microscopy (TXM) and simultaneous X-ray diffraction of laser melting simulating laser powder bed fusion on the XCS instrument at the Linac Coherent Light Source (LCLS) X-ray free-electron laser (XFEL). Our TXM with 40× magnification in the X-ray regime at 11 keV gave spatial resolutions down to 940 nm per line pair, with effective pixel sizes down to 206 nm, image integration times of <100 fs, and frame rates tunable between 2.1 and 119 ns for two probe frames (0.48 GHz to 8.4 MHz). Images were recorded on Zyla and Icarus (UXI) detectors to trade off between spatial resolution and time dynamics. A 1 kW CW IR laser was coupled into the interaction point to conduct pump–probe studies of laser melting and solidification dynamics. Our temporal and spatial resolution with attenuation-based contrast exceeds that currently possible with synchrotron-based high-speed radiography. This system was sensitive to feature velocities of 10–12000 m s −1 but we did not observe any motion in this range in the laser melting of Al6061 alloy. Shockwaves were not observed and hot cracking proceeded at velocities below the detection limits. Pore accumulation was observed between successive shots, indicating that bubble escape mechanisms were not active. With proper experimental design, the spatial resolution, contrast and field of view could be further improved or modified. The increased brightness and narrower bandwidth of the XFEL allowed for this imaging technique and it lays the groundwork for a wide range of operando techniques to study additive manufacturing.
In situ characterization of residual stress evolution during heat treatment of SiC/SiC ceramic matrix composites using high-energy X-ray diffraction
Volumetric strains were measured in silicon carbide/silicon carbide melt-infiltrated ceramic matrix composites (CMCs) at ambient and high temperatures using high-energy synchrotron X-ray diffraction (XRD). Both silicon and silicon carbide constituents were interrogated utilizing a broad spectrum of diffracting planes that would be largely inaccessible to common laboratory XRD equipment. Residual room-temperature principal strains in the melt-infiltrated silicon phase were found to be approximately 1100 mu epsilon in compression, corresponding to stresses of approximately 300 MPa using simplifying constitutive assumptions. Residual room-temperature principal strains in silicon carbide particles found throughout the matrix were approximately 500 mu epsilon in tension, corresponding to approximately 300 MPa. Residual strains were found to decrease considerably as temperatures increased from ambient temperature to 1250 degrees C. Additionally, residual strains returned to approximately preheat treatment values after cool-down to ambient temperature. Strain measurements in the silicon phase were found to be significantly affected by dissolved boron dopant levels causing contraction of the silicon lattice. This contraction must be accounted for in high-temperature experiments for accurate calculation of stresses in the silicon phase.
In situ characterization of laser-generated melt pools using synchronized ultrasound and high-speed X-ray imaging
Metal additive manufacturing is a fabrication method that forms a part by fusing layers of powder to one another. An energy source, such as a laser, is commonly used to heat the metal powder sufficiently to cause a molten pool to form, which is known as the melt pool. The melt pool can exist in the conduction or the keyhole mode where the material begins to rapidly evaporate. The interaction between the laser and the material is physically complex and difficult to predict or measure. Here, high-speed X-ray imaging was combined with immersion ultrasound to obtain synchronized measurements of stationary laser-generated melt pools. Furthermore, two-dimensional and three-dimensional finite-element simulations were conducted to help explain the ultrasonic response in the experiments. In particular, the time-of-flight and amplitude in pulse-echo configuration were observed to have a linear relationship to the depth of the melt pool. These results are promising for the use of ultrasound to characterize the melt pool behavior and for finite-element simulations to aid in interpretation.
Elucidating the formation mechanisms of zeolites using data-driven modelling and in-situ characterization
Zeolites are the main solid catalysts used by the chemical industry. The use of zeolites in separations and as shape selective catalysts requires control of the width and connectivity of their pores. 235 distinct zeolite frameworks have been synthesized to date, of over 2 million that have been proposed. Recent work indicates that the limitation is in large part kinetic: new synthetic pathways are required to access new zeolites. Organic cations are used to direct the synthesis towards specific zeolites. However, the molecular mechanisms by which cations direct the nucleation towards specific zeolites is not known. Elucidating these mechanisms is key to realize new zeolites for catalysis and separations, and is the focus of this project. This project developed and implemented a synergistic, data-driven computational and experimental approach to resolve the molecular pathways of nucleation, growth, and polymorph selection of zeolites and the role of organic cations in directing their formation. The project developed computationally efficient and accurate models for the study of the nucleation and growth of pure silica zeolites in molecular simulations, using machine learning with data from experiments. Simulations with these models were integrated with scanning tunneling electron microscopy, computer vision, and deep learning to unveil the molecular pathways of formation of a zeolite. Of particular interest in this project was to elucidate the role of amorphous precursors in the nucleation of the zeolite. Previous experiments indicate that zeolites are born within non-crystalline aggregates in which the silicates and organic cations have local and medium range order similar to that of the zeolite. The organic cations that direct the formation of zeolites and those that direct the formation of ordered mesoporous silicas are similar. We hypothesized that the frustrated attraction that for large organic cations leads to the formation of stable mesophases that direct the synthesis of mesoporous silicas, could promote the formation of metastable mesophases that can assist in the nucleation and polymorph selection of zeolites. The simulations resolved how structure directing agents build crystalline order and showed that mesoscopic pre-ordering occurs is not required to facilitate the nucleation of zeolites, because the synthesis occurs at high driving forces, where the barriers for nucleation are negligible. This project unveiled that polymorph selection in zeolite synthesis occurs after nucleation, opening a distinct area of control through the kinetics of growth and not through nucleation barriers.
In situ Characterization of Soot Aggregates Produced by Burning Contaminated Liquid Fuels with Nuclear Waste Surrogate
The motivation of this work was to complement other studies intended to enhance and update DOE-HDBK-3010-94 for hazard scenarios like nuclear waste fires. In this work, a uniquely designed combustion chamber was successfully integrated with a light scattering technique to characterize soot aggregates. The chamber design allowed for soot investigation within the flame as well as after soot left the incandescent flame region.
Study on Pipeline Polyethylenes in Hydrogen Gas Environments Using In-Situ and Ex-Situ Characterization Methods
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In-Situ Characterization of Direct Ink Write Feedstock Using Ultrasound
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Increasing imaging resolution through scattering media via in-situ characterization of the point-spread function
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Editorial: Advanced in situ characterization of biological interfaces and materials
Rapid changes are occurring on this dynamic planet–in 2020 anthropogenic mass was reported to not only match but exceed the mass of natural origins (Elhacham et al., 2020). These indications do not bold well for humanity in the coming generations, as we face 2 degree overall temperature increases over the next 5 years, CO 2 is spewing into the atmosphere at the Gigatonne (Gt) rate per year without any signs of mitigation in the foreseeable future, ocean water levels are rising to incredible levels, drinking water availability is disappearing, humanity is heavily reliant on the “drill-and-fill” culture, and two wars are currently being fought in Gaza and Ukraine (Carr et al., 2024). And even with these pressures, humanity continues to eke out impressive scientific and technological achievements in the recent past including mRNA vaccines to counter a global pandemic (Hogan and Pardi, 2022) and the development of CRISPR-Cas9 drugs (Parums, 2024). All these developments are only possible from the incremental methodological improvements taking place presently.
In-situ Characterization of Nanomaterials in Extreme Environments with the I3TEM.
Abstract not provided.
In-situ Characterization of Metal/Oxide Catalysts for CO2 Conversion: From Fundamental Aspects to Real Catalysts Design
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Final Report--Optical Photothermal Infrared (OPTIR) microscope for in-situ characterization of cellular metabolism and chemical processes
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In-situ characterization of a background calibration line for east coast aerial measuring
Report outlines the methodology used to establish a background calibration line for AMS-East operations at Joint Base Andrews. The results provide a general isotopic characterization of the soil within the calibration line at Joint Base Andrews, and the expected terrestrial exposure rate which can be used to aerial measuring.
Robust Split Laser Spectroscopic Sensor for In-situ Characterization of Rare Earth Elements and Critical Minerals in Mining Deposits
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Strong metal–support bonding enhanced thermal stability in Au–Al 2 O 3 core–shell nanowires characterized by in situ transmission electron microscopy
In this study, the thermal stability of Au–Al 2 O 3 core–shell and Au nanowires was investigated by in situ scanning transmission electron microscopy and other techniques. Here, the nanowires were synthesized by the helium droplets method and deposited on various substrates. The in situ characterization of Au–Al 2 O 3 thermal stability demonstrated a substantially enhanced stability as compared to that of pure Au nanowires, which can be a transformative approach to design more durable Au-based nanocatalysts. Our study also revealed the existence of strong metal–support bonding in the Au/Al 2 O 3 system.