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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

Analysis of neptunium oxides produced through modified direct denitration

Production of neptunium-237 ( 237 Np) target materials for plutonium-238 ( 238 Pu) radioisotope thermoelectric generators (RTGs) for deep space exploration requires advanced chemistry and engineering development. Currently, the domestic Pu-238 Supply Program at Oak Ridge National Laboratory produces neptunium dioxide (NpO 2 ) for target material using a modified direct denitration (MDD) flowsheet. Although the chemistry, reaction mechanisms, and product characteristics of MDD are well understood for uranium, corresponding studies of the neptunium system are still needed to continue optimization of target material properties, production equipment design, and production flowsheets. Here, the objective of this work is to characterize crystalline phases, morphology, surface texture, and particle size of NpO 2 produced via MDD reactions. Solid-phase characterization techniques, including powder X-ray diffraction (pXRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), were employed to achieve this objective. Subsequent data processing using the Morphological Analysis for Material Attribution (MAMA) software was performed to analyze particle morphology and size. Broadly, the powders were found to contain a mixture of NpO 2 and Np 2 O 5 after denitration with a variety of morphologies. After high-firing, the product was found to be NpO 2 with a typical polycrystalline oxide morphology and a grain size ranging from 0.72 to 0.94 µm. These analyses provide knowledge on the reaction pathway for a non-traditional NpO 2 synthesis method and offer additional unique insight into production-scale environments for transuranic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

In Situ High Energy X-ray Diffraction Characterization of Phase Transformations and Mechanical Behaviors in Rapidly Solidified Titanium and Stainless Steel Alloys [Thesis]

Advanced manufacturing techniques like additive manufacturing (AM) have poised themselves to revolutionize metal manufacturing. A wide range of AM techniques are capable of manufacturing metal components with unique, complex geometries and hastening the scientific-engineering-development cycle. Metal AM relies on a layer-by-layer rapid manufacturing process to build components from the substrate up. Rapid solidification is a large departure from traditional metal manufacturing due to its complex physics. Characterization of rapid solidification is difficult, stemming from the small volumes used in AM and the fast dynamics of the process. High energy X-ray diffraction (HEXRD) is a solution to the characterization problems of rapidly solidified alloys and AM. HEXRD can probe small volumes at fast rates and provides a wide range of thermomechanical and kinetic information. This thesis presents the application of HEXRD to rapidly solidified titanium and stainless steel alloys through a series of case studies. In the first two studies, HEXRD is applied to rapidly solidified titanium and stainless steel welds. The materials are characterized for their temperature history, phase changes, kinetics, and microstructural evolution. In the next case study, HEXRD is applied to characterize phase changes in elastocaloric NiTi shape memory alloys (SMAs) under thermomechanical load. HEXRD, in conjunction with other tools, is used to explain the superior performance of the additively manufactured SMAs. In the final two case studies, HEXRD is used to measure the mechanical response of AM parts with complex geometries; namely, the octet truss lattice. Diffraction reveals a wide range of materials information about the AM microstructure including unexpected phases, texture, and mechanical response to loading. The mechanical results from HEXRD and then compared with theoretical predictions about the performance of octet truss lattices. Summarily, HEXRD is a diverse tool that is poised to address the complex characterization problems of many aspects of the additive manufacturing process.

36 MATERIALS SCIENCE↗

Wideband Single Crystal Transducer for Bone Characterization

Phase II objectives: Optimize the Phase I transducer for sensitivity; Test different transmit signals for optimum performance; Demonstrate compatibility with electronics; Confirm additional transducer capabilities over conventional systems by calibrating with other methods.

Sahul, Raffi↗

Ultrasonic Phased-Array Characterization for NDE Applications

Southwest Research Institute (SwRI) recently fabricated and delivered the 100-channel Ultrasonic Phased-Array Testbed System (UPATS) for NASA's Langley Research Center. NASA prepared the specifications and provided the funding to develop UPATS in order to provide a tool for the improvement of ultrasonic nondestructive evaluation (NDE) and characterization of materials. UPATS incorporates state-of-the-art phased-array concepts such as beam steering, focusing, apodization, and phase-sensitive detection which make it possible to develop more sophisticated testing methodologies. It also can be used to investigate fundamental ultrasonic propagation and detection phenomena such as refraction, diffraction, scattering, and beam broadening.

Hanley, John J.↗

Transmission electron microscopy study of a high burnup U-10Zr metallic fuel

To support the development of U-10 wt.% Zr (U-10Zr) metallic fuel for Gen IV sodium-cooled fast reactors, we analysed a solid, Na-bonded, U-10Zr (by weight percent) fuel cross section that was irradiated to a burnup of ~ 12.4 % at.% at the Fast Flux Test Facility (FFTF). Advanced characterization techniques, including site specific sample preparation by focused ion beam (FIB) and phase/chemical determination by transmission electron microscopy (TEM), were used to reveal the constituent redistribution of Zr, characterize the fuel phases and the secondary phases (such as solid fission products) present at the end of life. It is shown that the fuel pin cross section is divided into three major concentric zones: a Zr-rich central region, a Zr-lean intermediate region, and a Zr intermediate peripherical region. The phase characterization revealed that the irradiation environment enhanced the development and stabilization of phases not predicted by the standard equilibrium U-Zr phase diagrams. Comparing the current results with the ones from previous studies, it is reaffirmed that the irradiation temperature and the time spent in the reactor, rather than the fuel burnup, are the two factors that most influence the formation of redistribution zones and their extension along the fuel cross section. Various solid fission products precipitated inside the fission gas pores, such as lanthanides, ZrRu, BaTe, CsI, and Ba and Sr oxides. Here, this study provides unprecedented nanoscale understandings in the U-10Zr fuel system that may benefit fuel performance modelling and advanced fuel development.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Preliminary Characterization Results from the DebriSat Project

The DebriSat project is a continuing effort sponsored by NASA and DoD to update existing break-up models using data obtained from two separate hypervelocity impact tests used to simulate on-orbit collisions. To protect the fragments resulting from the impact tests, "soft-catch" arenas made of polyurethane foam panels were utilized. After each impact test, the test chamber was cleaned and debris resulting from the catastrophic demise of the test article were collected and shipped to the University of Florida for post-impact processing. The post-impact processing activities include collecting, characterizing, and cataloging of the fragments. Since the impact tests, a team of students has been working to characterize the fragments in terms of their mass, size, shape, color and material content. The focus of the 20 months since the impact tests has been on the collection of 2 millimeters- and larger fragments resulting from impact test on the 56 kilogram-representative LEO (Low Earth Orbit) satellite referred to as DebriSat. To date we have recovered in excess of 115,000 fragments, 30,000 more than the prediction of 85,000 fragments from the existing model. We continue to collect fragments but have transitioned to the characterization phase of the post-impact activities. Since the start of the characterization phase, the focus has been to utilize automation to (i) expedite fragment characterization process and (ii) minimize human-in-the- loop. We have developed and implemented such automated processes; e.g., we have automated the data entry process to reduce operator errors during transcription of the measurement data. However, at all steps of the process, there is human oversight to ensure the integrity of the data. Additionally, we have developed and implemented repeatability and reproducibility tests to ensure that the instrumentation used in the characterization process is accurate and properly calibrated. In this paper, the implemented processes are described and preliminary results presented. Additionally, lessons learned from the implemented automations and their impacts on the integrity of the results are discussed.

Rivero, M.↗

Thermal property characterization of phase change materials in building applications: A systematic review of fundamentals, recent progress, and future directions

Phase change materials (PCMs) can reduce building peak loads and enable demand-responsive thermal energy storage (TES), but their deployment depends on reliable measurement and interpretation of thermal properties across laboratory, intermediate, and application scales. Here, this review systematically examines characterization methods, testing protocols, and recent advances for neat PCMs and PCM composites, emphasizing thermal conductivity, enthalpy-related properties (phase change temperature, latent heat, specific heat), and cycling stability. For thermal conductivity, we compare steady-state and transient techniques and note limitations when phase transition and contact resistance affect measurements. For enthalpy–temperature characterization, we discuss differential scanning calorimetry together with intermediate- and bulk-scale methods, including T-history, heat flow meter testing, and three-layer calorimetry (3LC), to generate application-relevant enthalpy–temperature profiles. Cycling stability is organized into four experimental families: thermoelectric–air, fully thermoelectric, water-bath, and in situ chamber approaches, with attention to separating reversible supercooling from true degradation such as phase segregation. We highlight emerging noncontact diagnostics, including infrared thermography and embedded sensing, for spatially resolved validation and multiscale interpretation. Finally, we review the growing use of AI and machine learning for property prediction, inverse characterization from experimental signals, and real-time state estimation in building-integrated TES. Key needs include harmonized protocols, interlaboratory benchmarking, uncertainty reporting, and metadata-rich datasets to accelerate reproducible PCM qualification for grid-flexible buildings.

AI↗

Spitzer Mission Operation System Planning for IRAC Warm-Instrument Characterization

This paper will describe how the Spitzer Mission Operations System planned and executed the characterization phase between Spitzer's cryogenic mission and its warm mission. To the largest extend possible, the execution of this phase was done with existing processing and procedures. The modifications that were made were in response to the differences of the characterization phase compared to normal phases before and after. The primary two categories of difference are: unknown date of execution due to uncertainty of knowledge of the date of helium depletion, and the short cycle time for data analysis and re-planning during execution. In addition, all of the planning and design had to be done in parallel with normal operations, and we had to transition smoothly back to normal operations following the transition. This paper will also describe the re-planning we had to do following an anomaly discovered in the first days after helium depletion.

IWIC↗

In situ characterization of phase transformations in petroleum pitch by high temperature X-ray diffraction

The phase transformation from isotropic to mesophase of a petroleum-derived pitch was monitored by in situ X-ray diffraction at 410 °C. The kinetics of the transformation were characterized by monitoring the growth of a broad peak at 2θ~24° and could be described by Avrami’s equation. The volatilization of low molecular weight components originally present in the pitch, or produced during the condensation reaction, was assessed by thermal gravimetry analysis, following the same thermal history. Ex situ characterizations of the pitch precursor before and after thermal treatment provided insight into the evolution of the molecular structure associated with mesophase generation (optical polarized microscopy, molecular weight distribution by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, X-ray photoelectron spectroscopy, Auger spectroscopy, and thermal stability). Here, this investigation demonstrates the value of using complementary in situ and ex situ experimental techniques to characterize complex mechanisms during the processing of organic materials.

02 PETROLEUM↗

An Investigation of Oxides of Tantalum Produced by Pulsed Laser Ablation and Continuous Wave Laser Heating

Recent progress has seen multiple Ta 2 O 5 polymorphs generated by different synthesis techniques. However, discrepancies arise when these polymorphs are produced in widely varying thermodynamic conditions and characterized using different techniques. This work aimed to characterize and compare Ta 2 O 5 particles formed at high and low temperatures using nanosecond pulsed laser ablation (PLA) and continuous wave (CW) laser heating of a local area of tantalum in either air or an 18 O 2 atmosphere. Scanning electron microscopy (SEM) and Raman spectroscopy of the micrometer-sized particles generated by PLA were consistent with either a localized amorphous Ta 2 O 5 phase or a similar, but not identical, crystalline β-Ta 2 O 5 phase. The Raman spectrum of the material formed at the point of CW laser impingement was in good agreement with the previously established ceramic “H-Ta 2 O 5 ” phase. TEM and electron diffraction analysis of these particles indicated the phase structure matched an oxygen-vacated superstructure of monoclinic H-Ta 2 O 5 . Further from the point of laser impingement, CW heating produced particles with a Raman spectrum that matched β-Ta 2 O 5 . We confirmed that the high-temperature ceramic phase characterized in previous work by Raman spectroscopy was the same monoclinic phase characterized in different work by TEM and could be produced by direct laser heating of metal in air.

36 MATERIALS SCIENCE↗

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi- component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma- sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia-yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging fiom 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗

Diffusion and phase change characterization by mass spectrometry

The high temperature diffusion of trace elements in metals and alloys was investigated. Measurements were made by high sensitivity mass spectrometry in which individual atoms were detected, and quantitative data was obtained for zircaloy-2, 304 stainless steel, and tantalum. Additionally, a mass spectrometer was also an analytical tool for determining an allotropic phase change for stainless steel at 955 C, and a phase transition region between 772 C and 1072 C existing for zircaloy-2. Diffusion rates were measured in thin (0.001" (0.0025 cm) and 0.0005" (0.0013 cm)) ribbons which were designed as high temperature thermal ion sources, with the alkali metals as naturally occurring impurities. In the temperature and pressure regime where diffusion measurements were made, the solute atoms evaporated from the ribbon filaments when the impurities diffused to the surface, with a fraction of these impurity atoms ionized according to the Langmuir-Saha relation. The techniques developed can be applied to many other alloys important to space vehicles and supersonic transports; and, with appropriate modifications, to the diffusion of impurities in composites.

Koslin, M. E.↗

Characterization of submicron matrix phyllosilicates from Murray and Nogoya carbonaceous chondrites

The combined techniques of high-resolution transmission electron microscopy and energy-dispersive X-ray analysis have been used to study dispersed, submicron phyllosilicates and the 'poorly characterized phase' of C2 matrix material. Morphologies and structure types observed are similar to terrestrial chrysotile. Distinctive morphologies and 7.3-A characteristic basal spacings combined with composition information rule out phyllosilicates other than serpentine group minerals as the predominant phyllosilicate material. The 'poorly characterized phase' is composed of chemically similar very fine-grained phyllosilicate and amorphous material. The observation of interstratified phyllosilicate material sheds additional doubt on compositional data which is not accompanied by structural data from the same particle.

Mckee, T. R.↗

Two-phase flow characterization for fluid components and variable gravity conditions

This paper describes a program initiated by the NASA Johnson Space Center to investigate vapor-liquid flow regimes and pressure drops in pipe components and variable gravity conditions. This program supports the Space Station Freedom External Active Thermal Control System design and future space missions, including the Space Exploration Initiative activities. The objectives for this program include studying two-phase flow behavior in fluid components (smooth pipes, bellows lines, quick-disconnect fittings), expanding the two-phase database for zero-g conditions, developing a database for low-g conditions (for example, Moon-g, Mars-g), and validating models for two-phase flow analyses. Zero-g and low-g data will be gathered using a Freon-12 flow loop during four test series on the KC-135 aircraft beginning in August 1991.

Dzenitis, John M.↗

Phased Array Characterization of Slat Noise Radiation from a High-Lift Common Research Model

A test campaign was conducted in the open-jet test section of the NASA Langley 14- by 22-Foot Subsonic Tunnel on a 10%-scale, semispan version of a High-Lift Common Research Model (CRM-HL) incorporating a leading-edge slat, trailing-edge flap and removable high-fidelity main landing gear. Far field acoustic measurements were obtained on baseline and acoustically treated model configurations using a traversing 97-microphone phased array that viewed the pressure side of the airframe. A modified version of the DAMAS deconvolution method incorporating corrections for shear layer acoustic wave decorrelation was employed to determine the locations and strengths of relevant noise sources along the span of the slat and in the vicinity of the flap edges and landing gear. The main goal of the test campaign was to use the array data to evaluate the effectiveness of various slat noise reduction concepts. It was found that slat-gap fillers produced significant broadband noise reduction for all Mach numbers and airfoil angles of attack that were investigated. Mach number scaling revealed an approximate velocity to the sixth power relationship for the slat noise at higher frequencies. Directivity measurements obtained from integration of DAMAS pressure-squared values over defined geometric zones around the model showed that baseline slat noise radiation approximated a dipole as a function of polar emission angle, becoming approximately omnidirectional with the introduction of the slat-gap filler. The test campaign clearly demonstrated the noise reduction benefits that can be obtained by applying appropriate treatments to leading edge slats on commercial transport-class aircraft.

William M Humphreys, Jr.↗