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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 73 records · Page 4

A data analysis method to rapidly characterize gallium concentration in plutonium matrices using LIBS

The processing of actinide samples is a complex and costly endeavor that requires compositional analysis at various stages. Laser-induced breakdown spectroscopy (LIBS) has been used to analyze actinide-containing samples in many nuclear applications including waste management, fuel processing and forensics. The LIBS spectrum obtained from actinide materials are generally extremely complex, exhibiting many thousands of strong emission lines. This makes it difficult to identify other elements within the sample of interest, given the rich and dominant actinide spectrum. Here, in this article, we describe a recent effort to identify and quantify impurities and alloying constituents in plutonium matrices using a hand-held LIBS instrument that is used to rapidly and efficiently measure an emission spectrum from a material sample. We tabulate the emission line positions and intensities of plutonium. We report the development of machine-learning software that can identify gallium and quantify its concentration in plutonium matrices. This work has the potential to provide a rapid and nearly non-destructive technique that allows more confidence in characterizing the composition of materials that are present within complex actinide associated targets. We describe how our LIBS measurements and data analysis methods have successfully quantified the gallium concentration in a variety of samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In Situ Infrared Ellipsometry for Protein Adsorption Studies on Ultrathin Smart Polymer Brushes in Aqueous Environment

The protein-adsorbing and -repelling properties of various smart nanometer-thin polymer brushes with high potential for biosensing and biomedical applications are studied by in-situ infrared-spectroscopic ellipsometry (IRSE). IRSE as a highly sensitive non-destructive technique allows us to investigate protein adsorption on polymer brushes in aqueous environment in dependence of external stimuli like temperature and pH. These stimuli are, for instance, relevant in switchable mixed brushes containing poly(N-isopropyl acrylamide) and poly(acrylic acid), respectively. We use such brushes as model surfaces for controlling protein adsorption of human serum albumin and human fibrinogen. IRSE can distinguish between polymer-specific vibrational bands, which yield insights into the hydration state of the brushes, and changes in the protein-specific amide bands, which are related to changes of the protein secondary structure.

36 MATERIALS SCIENCE↗

Learning heterogeneous reaction kinetics from X-ray videos pixel by pixel

Reaction rates at spatially heterogeneous, unstable interfaces are notoriously difficult to quantify, yet are essential in engineering many chemical systems, such as batteries and electrocatalysts. Experimental characterizations of such materials by operando microscopy produce rich image datasets, but data-driven methods to learn physics from these images are still lacking because of the complex coupling of reaction kinetics, surface chemistry and phase separation. Here we show that heterogeneous reaction kinetics can be learned from in situ scanning transmission X-ray microscopy (STXM) images of carbon-coated lithium iron phosphate (LFP) nanoparticles. Combining a large dataset of STXM images with a thermodynamically consistent electrochemical phase-field model, partial differential equation (PDE)-constrained optimization and uncertainty quantification, we extract the free-energy landscape and reaction kinetics and verify their consistency with theoretical models. We also simultaneously learn the spatial heterogeneity of the reaction rate, which closely matches the carbon-coating thickness profiles obtained through Auger electron microscopy (AEM). Across 180,000 image pixels, the mean discrepancy with the learned model is remarkably small (<7%) and comparable with experimental noise. Our results open the possibility of learning nonequilibrium material properties beyond the reach of traditional experimental methods and offer a new non-destructive technique for characterizing and optimizing heterogeneous reactive surfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Energy-resolved fast-neutron radiography using an event-mode neutron imaging detector

Energy-resolved fast-neutron radiography is a powerful non-destructive technique that can be used to remotely measure the quantity and distribution of elements and isotopes in a sample. This is done by comparing the energy-dependent neutron transmission of a sample with the known cross-sections of individual isotopes. The reconstruction of the composition is possible due to the unique features (e.g. resonances) in the cross-sections of individual isotopes. At short-pulsed (≲ 1 ns) neutron sources, such information is accessible via time-of-flight neutron imaging in principle, but requires a detector with nanosecond temporal resolution. Conventional neutron detectors can meet this requirement only by heavily compromising spatial resolution or efficiency. Here, we present a unique approach on fast neutron resonance radiography using a scintillator-based event-mode imaging detector at a short-pulsed neutron source, including first results on spatially mapped resonance profiles using MeV neutrons. The event mode approach applied in the presented detector allows recording of individual neutron interactions with nanosecond precision in time and sub-mm resolution in space. As a result, the entire available neutron energy spectrum can be measured for each pulse. At the same time, the use of a thick scintillator screen and lenses to focus the produced light results in a highly flexible field of view and a high interaction probability in the sensitive volume of the detector.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Powder diffraction

Powder diffraction is a non-destructive technique, which is experimentally simple in principle. Because the physics behind diffraction is well understood, an exceptionally large amount of information can be obtained from a single measurement. The positions and relative intensities of the peaks yield a fingerprint that can be used for qualitative phase analysis. Quantitative phase analysis can be obtained by detailed analysis of the intensities. Unit cells can be derived from the peak positions. Crystal structures can be solved using powder diffraction data and refined by the Rietveld method. The peak profiles contain information about crystallite size, strain and nanostructure. Non-idealities in the intensities give information on texture. Abandoning the crystallographic model provides information about local structure, by pair distribution function analysis. For powder diffraction, everything is a sample; the technique is commonly applied to characterize minerals, ceramics, metals and alloys, catalysts, polymers, pharmaceuticals, organic compounds, environmental and forensic samples, among others. The major features of contemporary laboratory powder diffractometers are described. Methods for obtaining suitable powder specimens are summarized. Major applications of qualitative and quantitative phase analysis, structure solution, size/strain/nanostructure analysis using peak profiles, texture analysis and pair distribution function analysis are introduced.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Process monitoring of additive manufacturing by using optical tomography

Parts fabricated by means of additive manufacturing are usually of complex shape and owing to the fabrication procedure by using selective laser melting (SLM), potential defects and inaccuracies are often very small in lateral size. Therefore, an adequate quality inspection of such parts is rather challenging, while non-destructive-techniques (NDT) are difficult to realize, but considerable efforts are necessary in order to ensure the quality of SLM-parts especially used for aerospace components. Thus, MTU Aero Engines is currently focusing on the development of an Online Process Control system which monitors and documents the complete welding process during the SLM fabrication procedure. A high-resolution camera system is used to obtain images, from which tomographic data for a 3dim analysis of SLM-parts are processed. From the analysis, structural irregularities and structural disorder resulting from any possible erroneous melting process become visible and may be allocated anywhere within the 3dim structure. Results of our optical tomography (OT) method as obtained on real defects are presented.

42 ENGINEERING↗

Simultaneous parameter optimization of x-ray and neutron reflectivity data using genetic algorithms

X-ray and neutron reflectivity are two non destructive techniques which provide a wealth of information on thickness, structure and interracial properties in nanometer length scale. Combination of X-ray and neutron reflectivity is well suited for obtaining physical parameters of nanostructured thin films and superlattices. Neutrons provide a different contrast between the elements than X-rays and are also sensitive to the magnetization depth profile in thin films and superlattices. The real space information is extracted by fitting a model for the structure of the thin film sample in reflectometry experiments. We have applied a Genetic Algorithms technique to extract depth dependent structure and magnetic in thin film and multilayer systems by simultaneously fitting X-ray and neutron reflectivity data.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

In situ measurement of phase transformations and residual stress evolution during welding using spatially distributed fiber-optic strain sensors

Welding of high-strength steels can result in large tensile strains as the base metal and filler material cool from their molten state. To combat these large tensile strains, low-transformation-temperature (LTT) metal fillers have been proposed. These fillers undergo a martensitic phase transformation at a lower temperature which can ultimately reduce the tensile strain or can even introduce compressive strain adjacent to the weld metal. However, the process for optimizing the composition of the LTT material, as well as various weld parameters for each unique weld geometry, can be quite expensive, especially if the acceptance criterion requires using neutrons, x-ray beams, or destructive techniques to characterize residual stresses. This work describes a simple, low-cost method for quantifying residual stresses and phase transformations in situ during welding. Spatially distributed fiber-optic sensors were bonded to a cast iron plate, along with tack-welded thermocouples, to measure temperature and strain during multiple passes with LTT filler metals. Results show that the fiber-optic sensors can successfully resolve compressive strain adjacent to the weld region caused by the martensitic phase transformations in the LTT filler material.

47 OTHER INSTRUMENTATION↗

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10 −4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

3DXRD↗

A Metallurgical Inspection Method to Assess the Damage in Performance-Limiting Nb 3 Sn Accelerator Magnet Coils

The design and production of Nb 3 Sn-based dipole and quadrupole magnets is critical for the realization of the High-Luminosity Large Hadron Collider (HL-LHC) at the European Organization for Nuclear Research (CERN). Nb 3 Sn superconducting coils are aimed at enhancing the bending and focusing strengths of accelerator magnets for HL-LHC and beyond. Due to the brittle nature of Nb 3 Sn, the coil fabrication steps are very challenging and require very careful QA/QC. Flaws in the Nb 3 Sn filaments may lead to quenches, and eventually, performance limitation below nominal during magnet testing. A novel inspection method, including advanced non-destructive and destructive techniques, was developed to explore the root-causes of quenches occurring in performance-limiting coils. The most relevant results obtained for MQXF coils through this innovative inspection method are presented. This approach allows for precise assessment of the physical events associated to the quenches experienced b y magnet coils, mainly occurring under the form of damaged strands with transversely broken sub-elements. Coil-slice preparation, micro-optical observations of transverse and longitudinal cross-sections, and a deep etching technique of copper will be illustrated in the present work, with a focus on the results achieved for a CERN coil from a non-conforming quadrupole magnet prototype, and two coils fabricated in the US, in the framework of the Accelerator Upgrade Project (AUP) collaboration, from two different non-conforming quadrupole magnets, respectively. The results obtained through the proposed inspection method will be illustrated.

43 PARTICLE ACCELERATORS↗

Evaluating the Potential for Remote In-Process Monitoring of Tool Wear in Friction Stir Welding of Stainless Steel

A wear characterization study was performed to determine the useful lifetime of Polycrystalline Cubic Boron Nitride tooling for the friction stir welding (FSW) of stainless steel samples in support of a nuclear repair welding research and development program. In-situ and ex-situ laser profilometry were utilized as primary methods of monitoring tool geometry degradation, and volumetric defects were detected through both non-destructive and destructive techniques, as repeated welds of a standard sample configuration were produced. The spectral content of weld forces were examined to search for indications of evolving material flow conditions, caused by significant tool wear, that would result in the formation of defects, and an artificial neural network was trained and evaluated as a means of automatically detecting these conditions. Here, the resulting performance constituted a successful demonstration of in-process monitoring of tool wear and weld quality in FSW of a high melting temperature, high hardness material.

36 MATERIALS SCIENCE↗

Infrared thermography NDT for in-situ defect detection in sandwich composite panel manufacturing

Composite manufacturing presents numerous challenges, as defects can arise from various sources throughout the process. In sandwich composite structures, the integration of a foam core introduces additional complexity and increases the likelihood of defect formation like delamination. To mitigate these issues and reduce the risk of future structural failures, in-situ monitoring during manufacturing is essential. This study investigates infrared (IR) thermography as a non-destructive technique for detecting manufacturing defects in foam-core sandwich composite panels under thermally excited conditions representative of in-situ processing. A stationary FLIR A8590 IR camera (640 × 512 pixels, 30Hz, 17mm lens, 9 ft stand-off distance) was used to monitor prefabricated panels subjected to controlled external heating simulating compression molding and resin cure exotherm. Interlaminar delamination defects with characteristic sizes ranging from 0.25 × 0.25in² to 5 × 5in² produced measurable surface temperature depressions of approximately 4–10°C during transient cooling, exceeding the effective noise floor of the camera by more than two standard deviations. Thicker laminates exhibited prolonged defect detectability windows due to increased thermal diffusion time. In contrast, embedded Teflon inclusions generated weak thermal contrasts of ≤ 3°C, approaching the measurement noise floor, due to limited thermal property contrast with the surrounding glass fiber composite. These results establish quantitative detectability limits for stationary thermographic inspection of sandwich composite panels under manufacturing-representative thermal cycles.

Barakat, Abdallah [ORNL] (ORCID:0000000296141398)↗

Boson Peak Related to Ga Nanoclusters in AlGaN Layers Grown by Plasma-Assisted Molecular Beam Epitaxy at Ga-Rich Conditions

We report the results of systematic Raman spectroscopy studies of Al{sub x}Ga{sub 1 –x}N (x ~ 0.75) layers grown using plasma-assisted molecular beam epitaxy at various stoichiometric conditions and growth fluxes. The high-intensity asymmetric low-frequency peak obeying Bose statistics is discovered in Raman spectra of the layers grown by temperature-modulated epitaxy at strongly Ga-enriched conditions. Theoretical model is developed to explain the origin and the high intensity of the observed low-frequency peak, which is attributed to the presence of excessive metallic gallium in AlGaN layers and can be explained by vibrations of gallium clusters with a diameter of ~1 nm. The nature of the low-frequency peak is similar to that of the boson peak in glasses, which occupies the same frequency range in Raman spectra. We demonstrate the capabilities of Raman spectroscopy as an express and non-destructive technique for optimization of growth conditions of AlGaN layers to achieve simultaneously the atomically-smooth droplet-free surface morphology and the high structural quality.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Shallow-etched thin-film lithium niobate waveguides for highly-efficient second-harmonic generation

High-fidelity periodic poling over long lengths is required for robust, quasi-phase-matched second-harmonic generation using the fundamental, quasi-TE polarized waveguide modes in a thin-film lithium niobate (TFLN) waveguide. Here, a shallow-etched ridge waveguide is fabricated in x-cut magnesium oxide doped TFLN and is poled accurately over 5 mm. The high fidelity of the poling is demonstrated over long lengths using a non-destructive technique of confocal scanning second-harmonic microscopy. We report a second-harmonic conversion efficiency of up to 939 %.W −1 (length-normalized conversion efficiency 3757 %.W −1 .cm −2 ), measured at telecommunications wavelengths. The device demonstrates a narrow spectral linewidth (1 nm) and can be tuned precisely with a tuning characteristic of 0.1 nm/°C, over at least 40 °C without measurable loss of efficiency.

Zhao, Jie (ORCID:0000000306230125)↗

Overview and Current Status of Neutron Imaging at Oak Ridge National Laboratory

Neutron imaging is a non-destructive technique used to study the internal structure and composition of a wide range of materials. At Oak Ridge National Laboratory (ORNL), there are two neutron imaging beamlines that provide complementary capabilities that serve a diverse community, from materials science and engineering to biomedical and plant sciences. This report provides an overview of the current ORNL imaging capabilities that support materials research for a broad user community.

Torres, James [ORNL] (ORCID:0000000289407610)↗

Report on Concepts & Approaches for SSBD for eCHEM

The verification of special nuclear material (SNM) in spent fuel pyroprocessing is an important safeguards challenge. The detection of spontaneous fission (SF) neutrons from curium is an accepted, non-destructive technique that has been applied to verify special nuclear material (SNM) content in used fuel and other materials in the fuel cycle. The nuclear material accounting (NMA) technique at the Korea Atomic Energy Research Institute’s Reference Engineering-scale Pyroprocessing Facility (REPF) is based on the Cm balance technique. Several publications have demonstrated the safeguards benefit from using process monitoring (PM) on nuclear facilities as a complementary measure to NMA. More recently, this concept was expanded and preliminarily demonstrated for pyroprocessing. The concept of Signature Based Safeguards (SBS) is part of this expansion, and is built around the interpretation of input from various sensors in a declared facility coupled with complementary NMA methods to increase confidence and lower standard error inventory differences (SEID). The SBS methodology was conceptually developed and relies on near real time analysis of process monitoring data to detect material diversion complemented by robust containment and surveillance (C/S) measures. This work demonstrates one example of how the SBS framework can be used in the electrorefiner. In this SBS application, a combination of cyclic voltammetry (CV) and neutron counting is applied to track and monitor Pu mass balance. The main purpose of this experiment is to determine if meaningful information can be gained from CV measurements with regard to the Mg/Gd ratio. This data will be coupled with ICP-MS to verify Gd concentrations and analyzed for statistical significance. It is expected the CV data will register a significant change under the off-normal operating conditions. Knowing how to identify and interpret those changes may help inform how to target more traditional neutron counting methods, which could support a more efficient safeguards system. The experimental results will be compared with theoretical calculations and the ERAD simulations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Postirradiation Examination of the ATF-1 Experiments - 2018 Status

The Advanced Fuels Campaign in collaboration with industry are working to develop enhanced accident tolerant fuels for light water reactors. The initial irradiations of these concepts were performed in the Idaho National Laboratory Advanced Test Reactor using simple drop-in style irradiations. These irradiations are collectively referred to as ATF 1. The postirradiation examination of ATF 1 has begun and some concepts have now completed initial examination. This report describes the results of examinations on ATF 1 irradiations designed to test the feasibility of enhancing UO 2 thermal conductivity with additives, ATF 1 irradiations of uranium silicide, and the current status of ATF 1 irradiations that are in process at the hot cell. Enhanced thermal conductivity uranium dioxide composites containing silicon carbide (UO 2 SiC) and diamond (UO 2 diamond) have been irradiated to low burnup. The conditions of this irradiation test and subsequent postirradiation examinations are discussed. These irradiations evaluate fuel microstructure and potential fuel cladding interaction under representative light water reactor power conditions. Both non destructive and destructive techniques have been used to evaluate fuel integrity, fission gas release, fission product distribution, burnup, fuel swelling and cladding strain. Examination of the UO 2 SiC pellets revealed enhanced cracking when compared to a UO 2 rodlet also irradiated under similar conditions. Additionally, instability of the SiC whiskers in the uranium dioxide matrix was observed in the pellet central region, where the local temperatures exceeded 1300 °C. The microstructure of the diamond added UO 2 was severely disrupted during irradiation, resulting in local migration of cesium along the fuel stack and increased fission gas release when compared with the expected release from the Vitanza curve at corresponding values of burnup and irradiation temperature. The postirradiation examination results cast doubt on the suitability of these additives to improve UO 2 fuel performance in a way that would lead to enhanced accident tolerance. Additionally, postirradiation examination data of U 3 Si 2 fuels at low burnup (i.e., < 20 GWd/tHM) for application in advanced Light Water Reactor (LWR) is presented. The U 3 Si 2 pellets show limited cracking in comparison to the expected behavior of UO 2 at same power level. In addition, gamma scanning data did not reveal migration of fission products. Minor homogeneous hardening along the pellet radius due to accumulation of fission products and radiation damage was measured by microindentation. The fission gas release and swelling remains very low. Formation of fission gas bubbles resolvable with optical microscopy occurs from the pellets center outward to approximately 60% of the fuel pellet radius. The overall data suggest a good performance of this accident tolerant fuel candidate at low burnup. Finally, the current status of postirradiation examination on other ATF 1 irradiations will be discussed. These irradiations include UO 2 clad in an FeCrAl alloy, an alternative uranium silicide compound U 3 Si 5 also clad in a FeCrAl alloy, and an interaction test between UO 2 and different FeCrAl alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗