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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
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Materials Characterization, Prediction, and Control Project: Characterization of 316L Stainless Steel after Solid Phase Processing using Ultrasonic NDE Method

The Pacific Northwest National Laboratory undertook the Materials Characterization, Prediction, and Control Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). A motivation of the Materials Characterization, Prediction, and Control Project was to demonstrate ultrasonic testing as a nondestructive evaluation method to complement traditional destructive methods for characterizing material microstructure with emphasis on grain size determination using a method that may have future applications for real-time inline process monitoring. The objective of the work described in this report is to establish the process and an analysis method for measuring grain sizes of polycrystalline metals with ultrafine grains using ultrasonic shear wave backscattering, building on prior studies on coarser-grained material. The work involves five tasks: Measured ultrasonic backscattering experimentally for a series of 316L stainless steel specimens with various grain sizes made by friction stir processing. Calculated ultrasonic backscattering coefficients from experimental data based on a physical measurement model. Measured ground truth grain sizes of the specimens from electron backscatter diffraction grain boundary images using a generalization of the ASTM E112 (ASTM 2021) intercept method. Built a curve of ultrasonic backscattering coefficients versus the ground truth intercept-based grain sizes to determine the correlation between mean grain sizes and ultrasonic measurements. Demonstrated the ability of using the correlation curve to deduce grain sizes with measured ultrasonic backscattering coefficients for a few 316L stainless steel specimens whose grain sizes were unknown beforehand but were targeted to be an extrapolation to larger grain sizes than used to formulate the correlation curves. Experimental procedures and computational algorithms are developed and validated for these tasks. This work establishes an ultrasonic technique for characterizing material microstructure with ultrafine grains that are often resulted by solid-phase processing. The technique is nondestructive, and it has the potential to be used for real time inline process monitoring. This work successfully demonstrates the viability of an ultrasonic nondestructive evaluation method for microstructural characterization of material having ultrafine grain structure (as small as 1?mm) and produced by an advanced manufacturing method. This includes a demonstration of the method to extrapolate to other conditions. While not demonstrated here, the method is expected to be viable for in-line, or near-inline, process monitoring in advanced manufacturing applications with suitable consideration for access of instrumentation to the material being manufactured.

316 L Stainless Steel↗
DOE OSTI2022

Transmission electron microscopy characterization of the fuel-cladding chemical interactions in HT9 cladded U-10Zr fuel

Fuel cladding chemical interaction (FCCI) is a key phenomenon needs to be better understood to establish the design basis for U-10Zr metallic fuel performance. Characterizing the microstructure and chemical composition of FCCI at micron and sub-micron scale is critically important toward a more mechanistic understanding of FCCI phenomenon and its potential effects on cladding integrity and metallic fuel performance. This paper, by using transmission electron microscopy, investigated the FCCI region in HT9 cladded U-10Zr fuel irradiated to 5.7% FIMA burnup at a peak inner cladding temperature of 615 °C in Fast Flux Test Facility (FFTF). Four distinct layers are identified in the FCCI region. The migration of Fe into the fuel side leads to the formation of several U-Zr-Fe ternary phases, including ?-Fe0.5Zr0.32U0.18, e-Fe0.3Zr0.4U0.3, and ?-Fe0.06Zr0.23U0.71, mingled with UFe2, U6Fe, and U phase at various Fe penetration depth up to ~ 150 µm. On the cladding side, grain coarsening and significant lanthanides infiltration along grain boundaries are observed. Laves phase, (Fe,Cr)2(Mo,W), which typically does not exist in fresh HT9, is identified in a wide radial range in the cladding. The typical HT9 martensitic lath structure and pre-existing M23C6 precipitates disappear, partially or completely, depending on the radial distance from the fuel-cladding interface. Those microstructural and compositional changes could cause mechanical degradation in the HT9 cladding. The present characterization results will improve the understanding of FCCI phenomenon and facilitate the development of microstructure-informed FCCI modeling for metallic fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Application of X-ray computed tomography for the characterization of graphite morphology in compact-graphite iron

Highlights: • X-ray Tomography is a powerful technique for graphite morphology characterization. • 3D characterization reveals true nodularity and spatial connectivity of graphite. • Tri-modal distribution of SG suggests a multi-stage graphite nucleation process. - Abstract: In the present study, high-energy X-ray tomography technique was used to characterize the graphite morphology of compact graphite iron. The size, shape, spatial connectivity and structure of different graphite morphologies were examined in 3D using computer-aided image analysis. In addition, nodularity analysis was performed in 3D and the results are compared to the traditional 2D technique. It is found that the variation of nodularity within 2 × 2 × 1.2 mm{sup 3} of the sample can be as high as 20 (%) from 2D analysis and the averaged nodularity (2D) is higher than that from 3D analysis. The size distribution of spheroidal graphite shows a tri-modal distribution, which suggests a multi-step nucleation process during solidification.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of natural organic matter in low-carbon sediments: Extraction and analytical approaches

Sediment-associated natural organic matter (NOM) is a complex assemblage of organic molecules with a wide range of sizes, functional groups, and structures, which is intricately associated with mineral particles. Organic carbon (OC) concentrations in subsurface sediments are typically 10 to 200 times lower than in surface soils, posing a distinct challenge for characterization. A range of chemical extractions were evaluated for extraction of NOM, and a NOM extraction scheme was developed using a combination of sequential extraction with water (MQ) and sodium pyrophosphate at pH 10 (PP), and purification by dialysis and solid phase extraction in order to isolate different fractions of sediment-associated NOM. Analysis of these different NOM fractions was then carried out by Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible (UV-Vis) spectroscopy, and electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS). The OC extraction efficiency of the tested extractions followed the order PP>NaOH>HCl=hydroxylamine hydrochloride>dithionite. Greater concentrations of OC in PP vs NaOH extracts suggest that metal complexation and/or ligand exchange plays an important role in OC stabilization. Characterization of different pools of extraction NOM by FITR shows that the water soluble fraction has a higher fraction of aliphatic and carboxylic groups, while the PP fractions have higher C=C groups. This trend from aliphatic to more aromatic is also supported by the UV-Vis and ESI-FTICR-MS data.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2024

Addressing Critical Problems in Materials Science Through Multiscale and Multimode Characterization (Project 1); Characterization and Optimization of Novel Triple-Conducting Oxide Materials for Energy Applications (Project 2) (CRADA Final Report)

PROJECT 1: Address critical problems in materials science and simultaneously advance the state-of-the-art in multiscale and multimode characterization using the combined advanced analytical capabilities and expertise of Colorado School of Mines (CSM) and the National Renewable Energy Laboratory (NREL). The primary effort of the Phase I of this CRADA is to establish the International Center for Multiscale Characterization using shared resources at both NREL and CSM. Phase II will focus on capability development and marketing, choosing candidate materials science issues in the areas of structure imaging, chemical composition mapping, and correlating properties and performance of materials for impact in energy-related, environmental and critical materials areas. The CRADA will be modified to include specific topics of concern in materials science to industry member partners. Advanced analytical capabilities and expertise at CSM and NREL will be used to advance materials understanding and performance through characterization of multiscale phenomena including structural imaging, chemical composition mapping, and other techniques correlating properties and performance of materials. PROJECT 2: As part of the International Center for Materials Characterization, work under Modification #1 will be led by Colorado School of Mines (CSM), working in collaboration with NREL staff to mentor and advise CSM postdoctoral researchers on set up of diffusion annealing experiments. The purpose of the modification is to provide for NREL staff to mentor and advise CSM postdoctoral researchers on set up of diffusion annealing experiments, including mentoring and advising the CSM-NREL team on proper Secondary Ion Mass Spectrometry (SIMS) data analysis as needed. SIMS measurements of 10-20 samples will be performed at NREL during the project duration.

08 HYDROGEN↗
DOE OSTI2020

High-resolution Hindcasts for U.S. Wave Energy Resource Characterization

The marine and hydrokinetic (MHK) industry is at an early stage of development and has the potential to play a significant role in diversifying the U.S. energy portfolio and reducing the U.S. carbon footprint. Wave energy is the largest among all the U.S. MHK energy resources, which include wave energy, ocean current, tidal-instream, ocean thermal energy conversion, and river-instream. Wave resource characterization is an essential step for regional wave energy assessments, Wave Energy Converter (WEC) project development, site selection and WEC design. The present paper provides an overview of a joint modelling effort by the Pacific Northwest National Laboratory and Sandia National Laboratories on high-resolution wave hindcasts to support the U.S. Department of Energy’s Water Power Technologies Office’s program of wave resource characterization, assessment and classifications in all US coastal regions. Topics covered include the modelling approach, model input requirements, model validation strategies, high performance computing resource requirements, model outputs and data management strategies. Examples of model setup and validation for different regions are provided along with application to development of classification systems, and analysis of regional wave climates. Lessons learned and technical challenges of the long-term, high-resolution regional wave hindcast are discussed.

Yang, Zhaoqing↗
DOE OSTI2018

Mass spectrometry-based proteomics for system-level characterization of biological responses to engineered nanomaterials

The widespread applications of engineered nanomaterials or nanotechnology make the characterization of biological responses to nanomaterials as an important area of research. The applications of omics-based approaches such as mass spectrometry-based proteomics have revealed new insights into the cellular responses upon exposure to nanomaterials, including how nanomaterials interact and alter cellular pathways. For instance, a redox-dependent response is often associated with exposure of nanomaterials, which leads to the generation of reactive oxygen species. In this review, we discuss the general quantitative proteomics approaches, with an emphasis on redox proteomics and their applications for characterizing the biological responses to nanomaterials.

Zhang, Tong↗
DOE OSTI2018

280 GHz Focal Plane Unit Design and Characterization for the Spider-2 Suborbital Polarimeter

We describe the construction and characterization of the 280 GHz bolometric focal plane units (FPUs) to be deployed on the second flight of the balloon-borne Spider instrument. These FPUs are vital to Spider’s primary science goal of detecting or placing an upper limit on the amplitude of the primordial gravitational wave signature in the cosmic microwave background (CMB) by constraining the B-mode contamination in the CMB from Galactic dust emission. Each 280 GHz focal plane contains a $16 \times 16$ grid of corrugated silicon feedhorns coupled to an array of aluminum–manganese transition-edge sensor (TES) bolometers fabricated on 150 mm diameter substrates. In total, the three 280 GHz FPUs contain 1530 polarization-sensitive bolometers (765 spatial pixels) optimized for the low loading environment in flight and read out by time-division SQUID multiplexing. In this paper, we describe the mechanical, thermal, and magnetic shielding architecture of the focal planes and present cryogenic measurements which characterize yield and the uniformity of several bolometer parameters. The assembled FPUs have high yields, with one array as high as 95% including defects from wiring and readout. We demonstrate high uniformity in device parameters, finding the median saturation power for each TES array to be $\sim $ 3 pW at 300 mK with a less than 6% variation across each array at $1\sigma $ . These focal planes will be deployed alongside the 95 and 150 GHz telescopes in the Spider-2 instrument, slated to fly from McMurdo Station in Antarctica in December 2018.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2018

Fourier Transform-Ion Cyclotron Resonance Mass Spectrometry as a Platform for Characterizing Multimeric Membrane Protein Complexes

Membrane protein characterization is consistently hampered by challenges with expression, purification, and solubilization. Among several biophysical techniques employed for their characterization, native-mass spectrometry (MS) has emerged as a powerful tool for the analysis of membrane proteins and complexes. Here, two MS platforms, the FT-ICR and Q-ToF, have been explored to analyze the homotetrameric water channel protein, AquaporinZ (AqpZ), under non-denaturing conditions. This 97 kDa membrane protein complex can be readily liberated from the octylglucoside (OG) detergent micelle under a range of instrument conditions on both MS platforms. Increasing the applied collision energy of the FT-ICR collision cell yielded varying degrees of tetramer (97 kDa) liberation from the OG micelles, as well as dissociation into the trimeric (72 kDa) and monomeric (24 kDa) substituents. Tandem-MS on the Q-ToF yielded higher intensity tetramer signal and, depending on the m/z region selected, the observed monomer signal varied in intensity. Precursor ion selection of an m/z range above the expected protein signal distribution, followed by mild collisional activation, is able to efficiently liberate AqpZ with a high S/N ratio. The tetrameric charge state distribution obtained on both instruments demonstrated superpositioning of multiple proteoforms due to varying degrees of N-terminal formylation. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Cryo-based Structural Characterization and Growth Model of Salt Film on Metal

Metal salt films play a critical role in high rate dissolution processes such as within an active pit. However, structural and compositional characterization of salt films is challenging owing to the dynamic nature of the dissolving interface. Here, the salt film formed on SS304 one-dimensional artificial pit surface was directly characterized using flash freezing and cryo-based focused ion beam/scanning electron microscopy. The salt film exhibits a porous structure. Ni is co-located with Fe in the salt film, indicating the formation of co-precipitated salt containing Fe2+ and Ni2+. Additionally, a salt film growth model is presented based on ion transport.

Salt film, Pitting corrosion, Cryogenic, Cryo-FIB/↗
DOE OSTI2024

Characterization of ferredoxins involved in electron transfer pathways for nitrogen fixation implicates differences in electronic structure in tuning 2[4Fe 4S] Fd activity

Ferredoxins (Fds) are small proteins which shuttle electrons to pathways like biological nitrogen fixation. Physical properties tune the reactivity of Fds with different pathways, but knowledge on how these properties can be manipulated to engineer new electron transfer pathways is lacking. Recently, we showed that an evolved strain of Rhodopseudomonas palustris uses a new electron transfer pathway for nitrogen fixation. This pathway involves a variant of the primary Fd of nitrogen fixation in R. palustris, Fer1, in which threonine at position 11 is substituted for isoleucine (Fer1 T11I ). To understand why this substitution in Fer1 enables more efficient electron transfer, we used in vivo and in vitro methods to characterize Fer1 and Fer1 T11I . Electrochemical characterization revealed both Fer1 and Fer1 T11I have similar redox transitions (–480 mV and – 550 mV), indicating the reduction potential was unaffected despite the proximity of T11 to an iron-sulfur (Fe—S) cluster of Fer1. Additionally, disruption of hydrogen bonding around an Fe—S cluster in Fer1 by substituting threonine with alanine (T11A) or valine (T11V) did not increase nitrogenase activity, indicating that disruption of hydrogen bonding does not explain the difference in activity observed for Fer1 T11I . Electron paramagnetic resonance spectroscopy studies revealed key differences in the electronic structure of Fer1 and Fer1 T11I , which indicate changes to the high spin states and/or spin-spin coupling between the Fe—S clusters of Fer1. Finally, our data implicates these electronic structure differences in facilitating electron flow and sets a foundation for further investigations to understand the connection between these properties and intermolecular electron transfer.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2017

Characterization of fission gas bubbles in irradiated U-10Mo fuel

Irradiated U-10Mo fuel samples were prepared with traditional mechanical potting and polishing methods with in a hot cell. They were then removed and imaged with an SEM located outside of a hot cell. The images were then processed with basic imaging techniques from 3 separate software packages. The results were compared and a baseline method for characterization of fission gas bubbles in the samples is proposed. It is hoped that through adoption of or comparison to this baseline method that sample characterization can be somewhat standardized across the field of post irradiated examination of metal fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Characterization of a gamma-ray tracking array: A comparison of GRETINA and Gammasphere using a 60 Co source

In this paper, we provide a formalism for the characterization of the tracking arrays with emphasis on the proper corrections required to extract their photopeak efficiencies and peak-to-total ratios. The methods are first applied to Gammasphere, a well characterized 4pi array based on the principle of Compton suppression, and subsequently to GRETINA. The tracking efficiencies are then discussed and some guidelines as to what clustering angle to use in the tracking algorithm are presented. It was possible, using GEANT4 simulations, to scale the measured efficiencies up to the expected values for the full 4pi implementation of GRETA.

efficiency measurements↗
DOE OSTI2019

Characterization of the Hamamatsu VUV4 MPPCs for nEXO

In this paper we report on the characterization of the Hamamatsu VUV4 (S/N: S13370-6152) Vacuum Ultra-Violet (VUV) sensitive Silicon Photo-Multipliers (SiPMs) as part of the development of a solution for the detection of liquid xenon scintillation light for the nEXO experiment. Various SiPM features, such as: dark noise, gain, correlated avalanches, direct crosstalk and Photon Detection Efficiency (PDE) were measured in a dedicated setup at TRIUMF. SiPMs were characterized in the range 163 K = T = 233 K. At an over voltage of 3.1 ± 0.2 V and at T = 163 K we report a number of Correlated Avalanches (CAs) per pulse in the 1µs interval following the trigger pulse of 0.161±0.005. At the same settings the Dark-Noise (DN) rate is 0.137 ± 0.002 Hz/mm2. Both the number of CAs and the DN rate are within nEXO specifications. The PDE of the Hamamatsu VUV4 was measured for two different devices at T = 233 K for a mean wavelength of 189 ± 7 nm. At 3.6 ± 0.2 V and 3.5 ± 0.2 V of over voltage we report a PDE of 13.4 ± 2.6 % and 11 ± 2%, corresponding to a saturation PDE of 14.8 ± 2.8 % and 12.2±2.3%, respectively. Both values are well below the 24 % saturation PDE advertised by Hamamatsu. More generally, the second device tested at 3.5 ± 0.2 V of over voltage is below the nEXO PDE requirement. The first one instead yields a PDE that is marginally close to meeting the nEXO specifications. This suggests that with modest improvements the Hamamatsu VUV4 MPPCs could be considered as an alternative to the FBKLF SiPMs for the final design of the nEXO detector.

Gallina, G↗
DOE OSTI2024

Godiva IV central cavity neutron environment characterization with threshold neutron detectors

Godiva IV is a cylindrical fast burst reactor comprised of approximately 65 kg of highly enriched uranium that is operated by Los Alamos National Laboratory and sited at the National Criticality Experiments Research Center at the Nevada National Security Site in Nevada in the United States. Godiva IV is typically operated at delayed critical and in the regime spanning from sub-prompt to super-prompt bursts. Godiva IV is used for sample irradiations, criticality safety demonstrations, dosimetry studies, and for studying super-prompt behavior. In preparation for both an upcoming experiment to reduce uncertainties in the prompt fission spectrum for 235U using threshold neutron detectors, and for future research using Godiva IV, it was desired to exercise the process of the selection of threshold neutron detectors/activation foils, radiation metrology, and the subsequent adjustment of the neutron spectrum. For this exercise, nine high purity threshold neutron detectors/activation foils were irradiated in a Godiva IV burst. The foils were then analyzed using a high-purity germanium detector in the NCERC counting laboratory to determine end of irradiation specific activities for available IRDFF-II reactions. This work summarizes the Godiva IV foil irradiation, radiation metrology results, and adjusted neutron spectrum. The results of this exercise ultimately characterized the neutron environment inside the sample irradiation cavity inside Godiva IV to a higher degree than previously performed, informed decisions for the upcoming larger scale experiment, and will inform future neutron spectrum characterizations at NCERC.

Whitman, Nicholas H.↗