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DOE OSTI2025

4D Observations of the initiation of abnormal grain growth in commercially pure Ni

Abnormal grain growth (AGG), where a small fraction of grains grow faster than others, is critical to predict because it can significantly impact material properties. However, the mechanism behind AGG remains unclear. In this study, laboratory-based x-ray diffraction contrast tomography (LabDCT) is employed to non-destructively track the 3D microstructural evolution of high-purity nickel during the onset of AGG at 800 °C. The initial microstructure state is used to test hypothesized microstructure predictors of the initiation of AGG. The change in grain size was not related to the initial grain size or normalized integral mean curvature. Additionally, the grain boundary energy distributions of abnormal grains were indistinguishable from those of control groups exhibiting normal grain growth. However, the grains that later became abnormal exhibit large areas of asymmetric tilt boundaries that were previously found to be fast. This 3D microstructure dataset is useful to investigate new hypotheses for the initiation of AGG.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Elucidating the phase transformations and grain growth behavior of O3-type sodium-ion layered oxide cathode materials during high temperature synthesis

Understanding the formation mechanism of layered oxide cathodes via solid-state synthesis is imperative to achieving controllability over their materials properties and electrochemical behaviors. In this work, we investigate the phase and microstructure evolution during the synthesis of NaNi 1/3 Fe 1/3 Mn 1/3 O 2 , a model sodium-ion layered oxide cathode, using a combination of imaging, diffraction, and spectroscopic techniques. We unravel the synthetic mechanistic pathways involved in the high-temperature calcination reaction, as well as elaborate the synthesis-microstructure-performance relationship of this material. The formation of the final layered oxide phase involves a gradual transformation through a sodiated oxyhydroxide intermediate. During the reaction, the precursor dehydration reaction dominates at 250–550 °C, while the major sodiation reaction occurs at 550–850 °C. Alongside multiple stages of phase transformations, the final grain structure formation occurs through the continuous growth of the (003) and (104) facets. During the reaction, Mn acts as the charge-compensating element and exhibits depth-dependent characteristics. When the sodiation reaction dominates over dehydration, the reaction intermediates undergo gradual electronic structure changes with increasing temperature, as indicated by the spectral features of TM3d-O2p hybrid states. Calcination duration is also a critical parameter governing the microstructure, surface reactivity, phase fraction distribution and electrochemical performance of the material. The optimal calcination duration was determined to be 18 hours at 850 °C under the conditions evaluated here. Calcination beyond this duration was found to be detrimental to electrochemical performance due to Na and O loss and heterogeneous sodium distribution throughout the particles. Our work sheds light on the complex crystallographic-chemical-microstructural evolution of sodium ion layered oxide cathodes and provides insight into precisely tuning material properties which are intimately linked to battery performances.

25 ENERGY STORAGE↗

DOE OSTI2023

Spatial and temporal metagenomics of river compartments reveals viral community dynamics in an urban impacted stream

Although river ecosystems constitute a small fraction of Earth’s total area, they are critical modulators of microbially and virally orchestrated global biogeochemical cycles. However, most studies either use data that is not spatially resolved or is collected at timepoints that do not reflect the short life cycles of microorganisms. To address this gap, we assessed how viral and microbial communities change over a 48-hour period by sampling surface water and pore water compartments of the wastewater-impacted River Erpe in Germany. We sampled every 3 hours resulting in 32 samples for which we obtained metagenomes along with geochemical and metabolite measurements. From our metagenomes, we identified 6,500 viral and 1,033 microbial metagenome assembled genomes (MAGs) and found distinct community membership and abundance associated with each river compartment (e.g., Competibacteraceae in surfacewater and Sulfurimonadaceae in pore water). We show that 17% of our viral MAGs clustered to viruses from other ecosystems like wastewater treatment plants and rivers. Our results also indicated that 70% of the viral community was persistent in surface waters, whereas only 13% were persistent in the pore waters taken from the hyporheic zone. Finally, we predicted linkages between 73 viral genomes and 38 microbial genomes. These putatively linked hosts included members of the Competibacteraceae, which we suggest are potential contributors to river carbon and nitrogen cycling via denitrification and nitrogen fixation. Together, these findings demonstrate that members of the surface water microbiome from this urban river are stable over multiple diurnal cycles. These temporal insights raise important considerations for ecosystem models attempting to constrain dynamics of river biogeochemical cycles.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1990

Dynamical effects of annihilation in pair-dominated winds

The steady, spherically symmetric flow of an ideal fluid dominated by photons and ultrarelativistic electron-positron pairs is analyzed. A new wind equation and a set of critical point conditions are obtained which describe the relativistic flow of an annihilation gas in which the flow velocity exceeds the diffusion velocity of the photons. Numerical results are reported which suggest the possible existence of trapped, pure-pair winds driven by the combined pressure of the pairs and the photons. Most of the annihilation occurs below the critical radius in trapped flows, and a substantial fraction of the total energy of the injected pairs is converted into kinetic energy and radiation. Accurate numerical solutions for the flow velocity and the positron loss rate in optically thin, Newtonian winds are obtained, and a useful approximate analytic relation between the positron loss rate and the flow velocity is derived which suggests that a large number of pairs may survive the annihilation region, ultimately escaping the potential well.

Becker, Peter A.↗

NASA NTRS1992

Studies on the reactive melt infiltration of silicon and silicon-molybdenum alloys in porous carbon

Investigations on the reactive melt infiltration of silicon and silicon-1.7 and 3.2 at percent molybdenum alloys into porous carbon preforms have been carried out by process modeling, differential thermal analysis (DTA) and melt infiltration experiments. These results indicate that the initial pore volume fraction of the porous carbon preform is a critical parameter in determining the final composition of the raction-formed silicon carbide and other residual phases. The pore size of the carbon preform is very detrimental to the exotherm temperatures due to liquid silicon-carbon reactions encountered during the reactive melt infiltration process. A possible mechanism for the liquid silicon-porous (glassy) carbon reaction has been proposed. The composition and microstructure of the reaction-formed silicon carbide has been discussed in terms of carbon preform microstructures, infiltration materials, and temperatures.

Singh, M.↗

NASA NTRSDate not supplied

NASA Plans for In Situ Resource Utilization (ISRU) Development, Demonstration, and Implementation

The United States (US) National Aeronautics and Space Administration’s (NASA) Artemis Moon to Mars program has four major goals: (1) Returning Americans to the Moon: 1st Woman & 1st Person of Color, (2) Learning to live and work on the Moon, (3) Translating lessons learned so that the United States has capabilities and operational experience for a mission to Mars, and (4) Inspires the next generation of explorers, researchers, scientists, and engineers worldwide. Overarching all of this, the NASA Artemis program also continues to follow Space Policy Directive One (SPD-1) which directs the US to lead an innovative and sustainable exploration program with commercial and international partners. A major objective to achieve the Artemis program goals and SPD-1 is to understand and characterize the resources that exist at these destinations, and to learn how to utilize these resources for sustained human exploration and the commercialization of space. This ability, commonly known as In Situ Resource Utilization (ISRU), involves any hardware or operation that harnesses and utilizes local resources to create products and services for robotic and human explo-ration. The NASA ISRU program is focused on the production of mission consumables and com-modities to enable sustained human exploration, such as rocket propellants, life support consuma-bles, fuel cell reactants, feedstock for manufacturing and construction, and nutrients for food and plant growth. In particular, propellants make up a significant fraction of the mass launched from Earth, are critical to mission success, and can reduce the cost for reusable transportation. Important for enabling long term surface stays, greater independence from Earth, and growing lunar infra-structure are the abilities to perform construction and manufacturing from in situ-derived metals and materials to create and expand on the infrastructure and reduce the logistical resupply needed for sustained surface and space operations. To achieve these ISRU capabilities, NASA, in partner-ship with industry, academia, and international partners has initiated a multi-faceted program which involves (i) Determining Customer Needs (Type and Quantity of Commodities), (ii) supporting ground Development of Hardware and Systems until Ready for Lunar Flight, (iii) utilize Commer-cial Lunar Payload Services (CLPS) flights to fly resource assessment missions with the Science Mission Directorate (SMD), and public-private partnership (PPP) ISRU demonstrations of critical technologies and processes, and (iv) performing commercial-led end-to-end ‘Pilot’ Plant production of commodities and demonstration of usage at a scale and duration that minimizes or eliminates risk for full implementation of ISRU-derived commodities in mission critical applications. This paper will discuss the technologies, mission studies, and accomplishments achieved to date for the ISRU multi-faceted program, and plans for continued ground development and flight missions to reduce the risk of full ISRU implementation.

In situ resource utilization↗

NASA NTRS2023

Numerical Study of Solidification Crack Susceptibility in Novel Refractory Alloy Systems

Calculation of Phase Diagrams (CALPHAD) -based solidification computations, such as Scheil or equilibrium computations, have been utilized to propose crack solidification susceptibility indices (CSSIs) of cracking. These CSSIs have been proposed in order to predict the cracking susceptibility of an alloy in the solidification range, as a function of its solidification fraction and as dependent upon its wt.% elemental composition through the CALPHAD computation & via comparative methods between one composition & the next. Recently Kou at al. have proposed a novel CSSI where the gradient of the e.x. Scheil solidification curve is obtained in the critical solidification cracking region of greater than 0.95 fraction of solid. Therefore, a direct Temperature dependent metric is now available for the prediction, and presumably the control, of solidification cracking. In this TM, the researchers apply this Kou gradient method to refractory alloys for the first time & discuss justification for the approach via Spearman rank correlation with Varestraint cracking test data as well as by comparisons with Thermocalc based vulnerability time CSSI calculations. A Python Pycalphad module example of the approach is provided & can be utilized as an open-source resource that utilizes also open-source available thermodynamical databases, making the CSSI quantitative aspect of ICME more available and freely available to practitioners.

ICME integrated computational materials engineerin↗

NASA NTRSDate not supplied

Mini-Channel Flow Boiling in 1g and μg

Subcooled flow boiling combines complex processes governed by a strong coupling of heat and mass transfer, hydrodynamics, and liquid-vapor transitions. The gravitational body force plays an important role in these processes. By exploiting the latent heat of vaporization, subcooled flow boiling can transfer up to several orders-of-magnitude more heat compared to forced liquid flow. It is widely used in Earth-based thermal equipment to reduce the cost, size, and power required to move heat. Subcooled flow boiling is now considered a promising technology for space applications since it offers a means to control the motion of bubbles near the heated surface and thereby enhance nucleate boiling. However, a lack of data and predictive models on the role that gravity plays in these phenomena hinders the use of flow boiling in a microgravity environment. We will present results of experiments on transients in nucleate boiling that were carried out in the Flow Boiling Module (FBM) on the International Space Station (ISS). The unique ISS FBM ability is to couple large heat loads with flow visualization in testing flow boiling under strict control of experimental conditions in long-duration microgravity. Comparison of results of microgravity experiments with data obtained in a similar setup on the NASA GRC demonstrates the role of gravity in nucleate boiling. The work is supported by the NASA Flight Opportunities program (grant 80NSSC21K0501) and NSF/CASIS program (NSF CBET grants 1832260, 2126461, 2126462).

Two-phase flow and phase transition↗

DOE OSTI2022

Investigation of the OECD/NEA PWR MOX/UO{sub 2} core transient benchmark using a coupled whole core pin-by-pin route in WIMS

This paper investigates the new CAMELOT coupling route developed in WIMS, which uses prepared tabulated cross-sections combined with the flux solver MERLIN module and the integrated sub-channel thermal hydraulics solver ARTHUR module to solve for the coupled core state. This coupling route is applied to the OECD/NEA pressurized water reactor (PWR) core transient benchmark exercise, involving 3-D neutronics and thermal-hydraulics analysis of a full-sized PWR core featuring MOX fuel at various core states, as well as simulating a control rod ejection transient. Analysis of the results for each part of the benchmark demonstrate that the high-resolution pin-by-pin analysis used in WIMS closely matches the other participants in the benchmark, with differences of between 20-200 pcm for k-effective, 1-2.5% RMS difference for assembly-averaged powers, 2-8% difference in rod worth calculations, < 200 ppm for calculations of critical boron concentration, zero difference in delayed neutron fraction calculation and a very close match for power response to the rod ejection transient. This is the first application of the WIMS-CAMELOT approach for the transient analysis of a full-sized reactor and as such further improvements such as reducing computational cost through parallelization, optimisation and memory reduction, are currently in active development. This paper demonstrates the accuracy and flexibility of the CAMELOT coupling route, providing a straightforward and consistent user image that can be easily used for a variety of modelling problems involving coupled neutronics and thermal-hydraulics. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2025

CMI Winter Meeting 2025 Presentation

Lanthanides are important to many technologies including magnets used in high efficiency traction motors. While common in the environment and industrial waste streams, lanthanides are often present at very low concentrations. This work demonstrates synergistic lanthanide recovery from an aqueous magnet leachate to single ppm concentrations using Na2SO4 addition and subsequent DME-FC treatment. It was found that combining DME-FC with low concentrations of Na2SO4 (~0.1 M) results in synergistic isolation of lanthanides while making use of Na2SO4, an excessive byproduct of hydrometallurgical metal production. Combined Na2SO4 + DME reduced lanthanide metal ion's (Pr, Nd, Sm, Gd, Dy, and Ho) solubilities by 1,000 - 25,000x with final concentrations ranging from 2 ppm to 200 ppm. This can be compared to 0.1 M Na2SO4 alone providing a 10 - 200x reduction and DME providing a 100 - 1,500x reduction in lanthanide solubilities. Final solution concentrations of lanthanides were 99.8% lower than what could not be achieved with either individual process. The results also reveal different periodic trends in the solubility reduction for DME and Na2SO4.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗

DOE OSTI2020

Fractionalized Excitations Revealed by Entanglement Entropy

Fractionalized excitations develop in many unusual many-body states such as quantum spin liquids, disordered phases that cannot be described using any local order parameter. Also, because these exotic excitations correspond to emergent degrees of freedom, how to probe them and establish their existence is a long-standing challenge. We present a general procedure to reveal the fractionalized excitations using real-space entanglement entropy in critical spin liquids that are particularly relevant to experiments. Furthermore, we show how to use the entanglement entropy to construct the corresponding spinon Fermi surface. Our work defines a new pathway to establish and characterize exotic excitations in novel quantum phases of matter.

2-dimensional systems↗

DOE OSTI2022

Solvent-driven aqueous separations for hypersaline brine concentration and resource recovery

Solvent-driven separation processes can extract water and high-value minerals from high salinity or contaminated brines, simultaneously reducing the environmental impact of brine disposal and enabling resource recovery. The efficient dewatering of hypersaline brines is essential for the sustainable minimal and zero liquid discharge processing of industrial wastewaters. Fractional crystallization can selectively extract ions from contaminated waste streams, allowing critical materials to be recycled, including transition and lanthanide metals required for renewable energy generation and storage. Mass transfer in solvent-driven water extraction occurs across a liquid–liquid interface, eliminating the scaling and fouling of membrane and heat exchanger surfaces and limiting the need for extensive pretreatment. Solvent-driven fractional crystallization can leverage sequential treatment and control of process conditions to rapidly recover salts without requiring evaporation of water. Despite promising applications, the principles and potential of solvent-driven aqueous separations remain poorly understood. This critical review explores the opportunities presented by solvent-based aqueous separations from the molecular to process scale, evaluating the chemistry of solvation and system design in the broader context of desalination, resource recovery, water softening, and mineral production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2018

Combining Fractional Calorimetry with Statistical Methods to Characterize Thermal Runaway

Thermal management systems designed to handle the impacts of thermal runaway (TR) are key to safe operation of lithium-ion (Li-ion) batteries. Critical factors for optimizing these systems include the total energy released and the fraction of the total energy that is released through the cell casing versus through the ejecta material. A unique calorimeter, designed to characterize said factors, was utilized to examine the TR behavior of a variety of 18650-format Li-ion cells. Statistical methods were implemented to interpret the data.

Walker, William↗

DOE OSTI2020

Applying Constrained Bayesian Optimization to the Design of Critical Experiments

Often when planning a criticality experiment, many design configurations are iteratively investigated with a Monte Carlo transport code. The goal is that the experiment will be optimal with respect to some variable, like the fraction of fissions occurring at a certain energy range, while simultaneously being critical. Unfortunately, the Monte Carlo transport simulations are expensive, which can ultimately limit the number of configurations that can be explored. In this work, we present how Gaussian processes (GPs) can be used as a reduced-order model in a constrained Bayesian optimization (CBO) algorithm to design a criticality experiment. The GPs replace the Monte Carlo transport simulations that explore the design space. The CBO algorithm efficiently identifies new points in the design space to run the Monte Carlo transport code while respecting the criticality constraint. It does so in a manner that both improves the accuracy of the GP and finds the approximate global optimum. We demonstrate the performance of CBO with the design of a Thermal Epithermal eXperiment (TEX) for the criticality safety validation of nuclear waste models of the Hanford Tank Farm.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2021

Scaling of oxygen-methane reacting coaxial jets using x-ray fluorescence to measure mixture fraction

Stoichiometric mixing length L s of reacting coaxial jet flames is a critical scaling parameter for liquid rocket engine combustors. Previous studies have shown that L s for shear coaxial flames can be scaled like their non-reacting counterparts using a non-dimensional momentum flux ratio J. In addition, stoichiometric mixing lengths of reacting and nonreacting coaxial jets collapse upon a single line by altering J using an effective outer flow gas density. This effective density is calculated from a modified version of the equivalence principle, originally developed by Tacina and Dahm [1, 2] and accounts for the effects of heat release on mixing. However, previous studies also required a second nonphysical scaling constant S c for the reacting jets, which is not predicted by the equivalence principle [3]. It was originally hypothesized that S c is attributed to the limitation of hydroxyl (OH) planar laser-induced fluorescence, which only infers L s . Direct quantitative measurement of conserved scalar fields using conventional optical diagnostics is difficult due to the lack of a tracer that easily fluoresces, survives high temperature oxygen flames, and is not dominated by quenching effects. To measure a conserved scalar field, this work implements x-ray fluorescence of Kr and Ar tracers to obtain quantitative mixture fraction fields. From these mixture fraction fields, stoichiometric mixing lengths for two CH 4 /O 2 flames are calculated and scaled against nonreacting coaxial mixing lengths using the equivalence principle. By directly measuring the stoichiometric mixing length, it is established that the additional constant is a byproduct of the OH measurement technique and the equivalence principle fully captures the scaling. Finally, comparison with high-fidelity simulation of the flame further supports this conclusion. In addition to further strengthening this scaling method, this work represents the first use of x-ray fluorescence to make quantitative conserved scalar measurements in turbulent flames.

33 ADVANCED PROPULSION SYSTEMS↗

DOE OSTI2024

Probing inhomogeneous cuprate superconductivity by terahertz Josephson echo spectroscopy

Abstract Inhomogeneities crucially influence the properties of quantum materials, yet methods that can measure them remain limited and can access only a fraction of relevant observables. For example, local probes such as scanning tunnelling microscopy have documented that the electronic properties of cuprate superconductors are inhomogeneous over nanometre length scales. However, complementary techniques that can resolve higher-order correlations are needed to elucidate the nature of these inhomogeneities. Furthermore, local tunnelling probes are often effective only far below the critical temperature. Here we develop a two-dimensional terahertz spectroscopy method to measure Josephson plasmon echoes from an interlayer superconducting tunnelling resonance in a near-optimally doped cuprate. The technique allows us to study the multidimensional optical response of the interlayer Josephson coupling in the material and disentangle intrinsic lifetime broadening from extrinsic inhomogeneous broadening for interlayer superconducting tunnelling. We find that inhomogeneous broadening persists up to a substantial fraction of the critical temperature, above which this is overcome by the thermally increased lifetime broadening.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1992

Inferring total canopy APAR from PAR bidirectional reflectances and vegetation indices in tallgrass prairie

The fraction of photosynthetically active radiation (PAR) absorbed by a vegetated canopy (APARc) or landscape (APARs) is a critical parameter in climate processes. A grassland study examined: 1) whether APARs can be estimated from PAR bidirectional exitance fractions; and 2) whether APARs is correlated with spectral vegetation indices (SVIs). Data were acquired with a high resolution continuous spectroradiometer at 4 sun angles on grassland sites. APARs was computed from the scattered surface PAR exitance fractions. The nadir APARs value was the most variable diurnally; it provided a good estimate of the average surface APARs at ~95 percent. APARc was best represented by exitance factors between 30-60* forward.

Middleton, Elizabeth M.↗

NASA NTRS1993

Buckling analysis of laminated thin shells in a hot environment

Results are presented of parametric studies to assess the effects of various parameters on the buckling behavior of angle-ply, laminated thin shells in a hot environment. These results were obtained by using a three-dimensional finite element analysis. An angle-ply, laminated thin shell with fiber orientation of (theta/-theta)(sub 2) was subjected to compressive mechanical loads. The laminated thin shell had a cylindrical geometry. The laminate contained T300 graphite fibers embedded in an intermediate-modulus, high-strength (IMHS) matrix. The fiber volume fraction was 55 percent and the moisture content was 2 percent. The residual stresses induced into the laminate structure during the curing were taken into account. Parametric studies were performed to examine the effect on the critical buckling load of the following parameters: cylinder length and thickness, internal hydrostatic pressure, different ply thicknesses, different temperature profiles through the thickness of the structure, and different lay up configurations and fiber volume fractions. In conjunction with these parameters the ply orientation was varied from 0 deg to 90 deg. Seven ply angles were examined: 0 deg, 15 deg, 30 deg, 45 deg, 60 deg, 75 deg, and 90 deg. The results show that the ply angle theta and the laminate thickness had significant effects on the critical buckling load. The fiber volume fraction, the fiber orientations, and the internal hydrostatic pressure had important effects on the critical buckling load. The cylinder length had a moderate influence on the buckling load. The thin shell with (theta/-theta)(sub 2) or (theta/-theta)(sub s) angle-ply laminate had better buckling-load performance than the thin shell with (theta)(sub 4) angle-ply laminate. The temperature profiles through the laminate thickness and various laminates with the different ply thicknesses has insignificant effects on the buckling behavior of the thin shells.

Gotsis, Pascal K.↗