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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

MSTL Re-Start Phase 1.5 Project Final Report

This document provides an overview of re-start efforts at Sandia National Laboratories (SNL), National Solar Thermal Test Facility (NSTTF), for the SNL Molten Salt Test Loop (MSTL). MSTL is one of the world’s only industrial-scale molten salt test systems, capable of testing commercial-scale thermal hydraulic equipment at an industrial scale, required for confident bankability of products. This work was facilitated as part of the Phase 1 re-start effort for facilitating forensics assessments to inform final refurbishments and upgrades costs and schedule information for revitalizing MSTL for use during a separate Phase 2 effort. This work was facilitated to further de-risk a Phase 2 effort pertaining to the tank and the pump, which were considered during Phase 1 to be high-risk items for a successful re-start. Impact from a successful re-start will allow SNL and other industrial molten salt systems companies, such as those in the Market Utilization Report provided in the Phase 1 submission package. An objective of this document is to also ensure longevity of utilization of MSTL after re start.

14 SOLAR ENERGY↗
DOE OSTI2023

Crystalline versus Glassy Nature of Iron Phosphate Waste Forms Subjected to Different Slow Cooling Curves

This report provides experimental details and associated results on the elemental distributions (compositions), crystalline/amorphous phase distributions, and microstructures for iron phosphate reference materials (DPF5-336) made with different cooling curves and starting from different temperatures (i.e., 1050°C and 1200°C). The primary goal of this work was to evaluate the properties of the DPF5- 336 reference material after it was melted and cooled at different rates to simulate the cooling profile of different types of canisters. Crystal fractions across the SCC#2, SCC#3, and SCC#5 samples were all similar ranging in crystal content of 35.66–41.14 mass% with amorphous fractions being the balance (64.34–58.86 mass%, respectively). This shows that the heat treatment profile did not seems to greatly affect either the total crystal content or the phase distributions. The quenched sample was almost completely amorphous (99.55 mass%) with very small peaks identified as Li 3 Fe 2 (PO 4 ) 3 whereas the SCC-treated materials showed peaks for what appear to be ten separate phases present in various concentrations. Another goal of these experiments was to see how the phase distribution affected chemical durability of these waste forms, but that information is being collected at Argonne National Laboratory and will be published in a separate report

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2023

Mixed-Polarity Copolymers Based on Ethylene Oxide and Cyclic Carbonate: Insights into Li-Ion Solvation and Conductivity

Here, this study investigates the relationship between polarity and ionic conductivity in random and block copolymer electrolytes comprising highly flexible oligo(ethylene oxide) methyl ether methacrylate (OEM) and highly polar but glassy glycerol carbonate methacrylate (GCMA) monomers, blended with either lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) or lithium triflate. Interestingly, the high polarity of GCMA did not significantly enhance ionic dissociation, and the random copolymers (POEM-r-PGCMA) showed similar or lower ionic conductivities than the POEM homopolymer. Further analysis revealed that Li + only interacts with OEM and its counterion, not with GCMA. The less-intermixed and weakly phase-separated block copolymer (POEM-b-PGCMA) exhibited even lower conductivities than the random copolymer. Our results suggest that Li + solvation occurs only in the POEM-rich phase and that the larger PGCMA regions, depleted of Li + , disrupt long-range ion transport. These findings provide valuable insights into the design of polymer electrolytes and how segmental mobility and functional groups with contrasting polarities affect ion transport.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Phase Behavior and Salt Partitioning in Polyelectrolyte Complex Coacervates

Polyelectrolyte complexes are omnipresent both in nature and in the technological world, including nucleotide condensates, biological marine adhesives, food stabilizers, encapsulants, and carriers for gene therapy. However, the true phase behavior of complexes, resulting from associative phase separation of oppositely charged polyelectrolytes, remains poorly understood. Here in this study, we rely on complementary experimental and simulation approaches to create a complete quantitative description of the phase behavior of polyelectrolyte complexes that represents a significant advance in our understanding of the underlying physics of polyelectrolyte complexation. Experiments employing multiple approaches with model polyelectrolytes oppositely charged polypeptides poly(L-lysine) and poly(D,Lglutamic acid) of matched chain lengths led to phase diagrams with compositions of the complex and the supernatant that were in excellent agreement with simulation results. Contrary to the widely accepted theory for complexation, we found preferential partitioning of salt ions into the supernatant phase. Additionally, the salt partitioning into the supernatant phase was found to initially increase and then decrease on increasing the salt concentrations, manifesting as a distinct minimum in the salt partition coefficients. These trends were shown by simulations to be strongly influenced by the excluded volume interactions in the complex phase, which were not accounted for in their entirety in earlier theories. Finally, we believe the comprehensive data we present will be conducive to the development of an accurate physical theory for polyelectrolyte complexation with predictive capabilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1982

Countercurrent distribution of biological cells

It is known that the addition of phosphate buffer to two polymer aqueous phase systems has a strong effect on the partition behavior of cells and other particles in such mixtures. The addition of sodium phosphate to aqueous poly(ethylene glycol) dextran phase systems causes a concentration-dependent shift in binodial on the phase diagram, progressively lowering the critical conditions for phase separation as the phosphate concentration is increased. Sodium chloride produces no significant shift in the critical point relative to the salt-free case. Accurate determinations of the phase diagram require measurements of the density of the phases; data is presented which allows this parameter to be calculated from polarimetric measurements of the dextran concentrations of both phases. Increasing polymer concentrations in the phase systems produce increasing preference of the phosphate for the dextran-rich bottom phase. Equilibrium dialysis experiments showed that poly(ethylene glycol) effectively rejected phosphate, and to a lesser extent chloride, but that dextran had little effect on the distribution of either salt. Increasing ionic strength via addition of 0.15 M NaCl to phase systems containing 0.01 M phosphate produces an increased concentration of phosphate ions in the bottom dextran-rich phase, the expected effect in this type of Donnan distribution.

Source record↗
DOE OSTI2014

Fine structure of Fe-Co-Ga and Fe-Cr-Ga alloys with low Ga content

Investigation of Ga influence on the structure of Fe-Cr and Fe-Co alloys was performed with the use of {sup 57}Fe Mössbauer spectroscopy and X-ray diffraction methods. In the alloys of the Fe-Cr system, doping with Ga handicaps the decomposition of solid solutions, observed in the binary alloys, and increases its stability. In the alloys with Co, Ga also favors the uniformity of solid solutions. The analysis of Mössbauer experiments gives some grounds to conclude that if, owing to liquation, clusterization, or initial stages of phase separation, there exist regions enriched in iron, some amount of Ga atoms prefer to enter the nearest surroundings of iron atoms, thus forming binary Fe-Ga regions (or phases)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Thermodynamic coarsening arrested by viscous fingering in partially miscible binary mixtures

We view the evolution of binary mixtures far from equilibrium, and demonstrate that the interplay between phase separation and hydrodynamic instability can arrest the Ostwald ripening process characteristic of nonflowing mixtures. We describe a model binary system in a Hele-Shaw cell using a phase-field approach with explicit dependence of both phase fraction and mass concentration. When the viscosity contrast between phases is large (as is the case for gas and liquid phases), an imposed background flow leads to viscous fingering, phase branching, and pinch off. This dynamic flow disorder limits phase growth and arrests thermodynamic coarsening. Because of this, the system reaches a regime of statistical steady state in which the binary mixture is permanently driven away from equilibrium.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA NTRS2020

NASA Exploration Systems & Habitation (X-Hab)Academic Innovation Challenge 2020: Microgravity Gas/Liquid Separator for the CO2 Revitalization System Final Report

This report outlines the efforts of UNT X-Hab Team on a project titled, Microgravity Gas/Liquid Separator for the CO2 Revitalization System. The project is executed as a senior design project during academic year 2019-2020. The X-Hab 2020 Academic Innovation Challenge has selected eleven senior design teams from colleges across the US to demonstrate working prototypes for exploration systems and habitation. UNT has been tasked with the creation of a gas-liquid separator for an air revitalization system. Air revitalization technology has been used to support spaceflight by removing CO2 from enclosed systems in order to maintain breathable air. Solid sorbents such as zeolites or lithium hydroxide have been used in the past for these systems but are difficult to handle in microgravity environments and require a large amount of energy. This challenge aims to demonstrate vortex phase separator (VPS) technology for removing H2O from a CO2 stream. However, VPS technology also has the capability of using liquid sorbents for removing CO2 from an air stream. Further research could be done on liquid sorbents, such as liquid amine, in use with VPS systems. This would potentially be an alternative technology in replacing use of solid sorbents in CO2 removal systems. In 2019, NASA proposed a design that uses a gas/liquid contactor to allow for efficient contact between the two fluid phase. This was integrated into an overall CO2 removal system. The subsystems for gas-liquid separation and storage in NASA’s previous models for CO2 removal system could be replaced with a VPS. Innovative vortex separator technology is expected to allow for high throughput flow and highly efficient CO2 removal compared to other gas-liquid separation technologies. VPS relies on centripetal driven buoyancy forces to form a gas-liquid vortex within a fixed, right circular cylinder. The gas stream enters the separator through a tangential nozzle and breaks into very small bubbles (<<1 mm) resulting in a very large contact surface area for interaction with the liquid stream via energy and mass exchange. VPS technology can handle mismatches in inlet and outlet flow rates and system volume changes through the range of liquid thickness held in the separator (i.e., buffering and accumulating capability), and requires low pressure differences (<5-10 in H2O in most cases) for operation. The X-Hab 2020 team leverages these characteristics to investigate VPS technology as an alternative CO2 removal technology.

Alyssa Sarvadi↗
DOE OSTI2020

Poly(norbornene) anion conductive membranes: homopolymer, block copolymer and random copolymer properties and performance

It has previously been shown that phase-separated block copolymers with non-ion conducting (hydrophobic) blocks and ion conducting (hydrophilic) blocks can form efficient ion conducting channels with high ionic mobility and conductivity. Block copolymers can provide a means for phase segregation and ion channel formation while homopolymers and random copolymers have been shown to have lower ion mobility. In this study, the properties of poly(norbornene) based anion exchange membranes (AEMs) comprising homopolymers, block copolymers, and random copolymers with high ion-exchange capacity (IEC) (3.48–4.55 meq. g -1 ) have been investigated and compared. The polymers were cross-linked with N,N,N',N'-tetramethyl-1,6-hexanediamine before casting the membranes to avoid excessive water swelling due to high water uptake. It was shown that high ionic conductivity can be achieved in both random copolymers and homopolymers even in the absence of microphase-separated structures. For example, the conductivity of a random copolymer was 194 mS cm -1 at 80 °C, which was comparable to the block copolymer, 201 mS cm -1 at 80 °C. The H 2 /O 2 fuel cell performance of random copolymer composite membranes showed a peak power density of 3.05 W cm -2 and peak current density of 7.85 A cm -2 at 80 °C compared to block copolymer membranes (peak power density of 3.21 W cm -2 and peak current density of 8.27 A cm -2 at 80 °C). It is more critical that high water transport be achieved in AEMs than achieving a phase-segregated morphology. Finally, the homopolymer, block copolymer, and random copolymer membranes showed <1.35% degradation after aging in 1 M NaOH at 80 °C for 1000 h.

08 HYDROGEN↗
DOE OSTI2020

Pore-scale evidence of ion exclusion during methane hydrate growth and evolution of hydrate pore-habit in sandy sediments

Hydrate-bearing sediments constitute complex hydrological systems, within which the pore habit of hydrate significantly affects all physical properties. However, there is scarce pore-scale evidence of the evolution of hydrate growth in porous media and the influence of water salinity in the micro-morphology of hydrate. In this paper, we used X-ray computed micro-tomography (CT) to monitor three experiments of methane hydrate growth in sand partially saturated with either NaBr or KI brine under excess-gas conditions. Gas, brine and hydrate are observed to co-exist at the pore-scale during the evolution of hydrate pore-habit towards three-phase equilibrium. The experiments and data analysis reveal that (1) hydrate forms as a porous medium mixed with inclusions of brine and gas, where hydrate and brine evolve gradually into separate phases as hydrate cages exclude salt ions, (2) hydrate growth mobilizes water over fairly long distances resulting in heterogeneous hydrate distribution, and (3) hydrate can exhibit interconnecting pore-habit at local hydrate saturations higher than ~50%, even if grown under excess-gas conditions. The results imply that hydrate micro-morphology and pore habit evolve during hydrate formation and, we suggest, so do the physical properties of hydrate-bearing sediments. Furthermore, our findings provide new insights into the micro-morphology of hydrate and evolution of the properties of hydrate-bearing sediments synthesized in the laboratory and in natural systems.

Clathrate hydrate↗
DOE OSTI2013

Phase transitions in the assembly of multivalent signalling proteins

Cells are organized on length scales ranging from angstrom to micrometers. However, the mechanisms by which angstrom-scale molecular properties are translated to micrometer-scale macroscopic properties are not well understood. Here we show that interactions between diverse synthetic, multivalent macromolecules (including multi-domain proteins and RNA) produce sharp liquid-liquid-demixing phase separations, generating micrometer-sized liquid droplets in aqueous solution. This macroscopic transition corresponds to a molecular transition between small complexes and large, dynamic supramolecular polymers. The concentrations needed for phase transition are directly related to the valency of the interacting species. In the case of the actin-regulatory protein called neural Wiskott-Aldrich syndrome protein (N-WASP) interacting with its established biological partners NCK and phosphorylated nephrin1, the phase transition corresponds to a sharp increase in activity towards an actin nucleation factor, the Arp2/3 complex. The transition is governed by the degree of phosphorylation of nephrin, explaining how this property of the system can be controlled to regulatory effect by kinases. The widespread occurrence of multivalent systems suggests that phase transitions may be used to spatially organize and biochemically regulate information throughout biology.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1972

Phase equilibria in fluid mixtures at high pressures: The He-CH4 system

An experimental study of phase equilibria in the He-CH4 system was carried out over the temperature range 95 to 290 K and at pressures to 10,000 atm. The experimental results consist of equilibrium phase composition for twenty-eight isotherms in the region of coexistence of two fluid phases, together with the pressure-temperature trace of the three-phase boundary at which a CH4-rich solid phase is in equilibrium with the two fluid phases. The system exhibits a fluid-fluid phase separation which persists to temperatures and pressures beyond the range of this experiment. These results, together with those recently obtained for other binary systems, provide information about the form of phase diagrams for binary gas mixtures in the region of pressure induced phase transitions at high pressures. These findings are relevant to problems of deep atmosphere and interior structures in the outer planets.

Streett, W. B.↗
NASA NTRS1975

Forced-flow once-through boilers

A compilation and review of NASA-sponsored research on boilers for use in spacecraft electrical power generation systems is presented. Emphasis is on the heat-transfer and fluid-flow problems. In addition to space applications, much of the boiler technology is applicable to terrestrial and marine uses such as vehicular power, electrical power generation, vapor generation, and heating and cooling. Related research areas are discussed such as condensation, cavitation, line and boiler dynamics, the SNAP-8 project (Mercury-Rankine cycle), and conventional terrestrial boilers (either supercritical or gravity-assisted liquid-vapor separation types). The research effort was directed at developing the technology for once-through compact boilers with high heat fluxes to generate dry vapor stably, without utilizing gravity for phase separations. A background section that discusses, tutorially, the complex aspects of the boiling process is presented. Discussions of tests on alkali metals are interspersed with those on water and other fluids on a phenomenological basis.

Stone, J. R.↗
DOE OSTI2015

Non-minimally coupled varying constants quantum cosmologies

We consider gravity theory with varying speed of light and varying gravitational constant. Both constants are represented by non-minimally coupled scalar fields. We examine the cosmological evolution in the near curvature singularity regime. We find that at the curvature singularity the speed of light goes to infinity while the gravitational constant vanishes. This corresponds to the Newton's Mechanics limit represented by one of the vertex of the Bronshtein-Zelmanov-Okun cube [1,2]. The cosmological evolution includes both the pre-big-bang and post-big-bang phases separated by the curvature singularity. We also investigate the quantum counterpart of the considered theory and find the probability of transition of the universe from the collapsing pre-big-bang phase to the expanding post-big-bang phase.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1978

Metallurgical analysis of skylab M552 and M557 samples

The anomalous microstructures on the basis of phase equilibria, liquid/liquid phase separation, and liquid/solid segregation for the Skylab M557 and M552 flight samples were studied. All of the unknown diffraction spectra have been identified. The previously unknown crystal structure of the Zn3Sb2 phase the M577B Experiment was determined. Previously unreported effects due to the near-absence of the hydrostatic pressure head are documented for the M557C samples.

Larson, D. J., Jr.↗
NASA NTRS1985

Optical studies of a binary miscibility gap system

Model transparent fluids are being studied to develop a better understanding of phase separation processes in binary miscibility-gap metal alloys. The model selected for the reported work is diethylene glycol-ethyl salicylate. This system is well characterized with respect to its phase diagram, density, surface and interfacial tensions, viscosity, and other pertinent physical properties. Minority phase growth, coalescence, and droplet motions are observed using holographic microscopy which is capable of recording particle densities up to 10 to the 7th particles/cu cm and is able to resolve particles as small as 2 to 3 microns in diameter throughout the entire volume of the test cell. Sequential holograms allow determination of droplet size distribution changes throughout the total volume with respect to time and temperature. This allows a direct method for testing various theories of droplet growth and ripening phenomena.

Witherow, W. K.↗
DOE OSTI2015

TEM characterization of 14YWT and 12YWT ODS ferritic alloys neutron irradiated at 500C using in-situ helium injection

This report summaries TEM characterization of 14YWT and 12YWT, ODS ferritic alloys with 14 and 12 wt % of Cr respectively, to compare the effect of neutron irradiation with and without concurrent He injection using ISHI. The density and average size of <100>/{100} type dislocation loops are always larger than those of 1/2<111>/{111} type, but this difference is significantly affected by He implantation. The density of dislocation loops of both types ranges from ~1 to 4x1021 m-3 with average size ranging from 5~20 nm. 14YWT has lower density but larger size dislocation loops than 12YWT, while the line dislocation density of 14YWT is 3 times lower than that of 12YWT. Helium bubble densities of both 14YWT and 12YWT are 1.9x1023 m-3, the average He bubbles size of 14YWT and 12YWT are 1.4 and 1.2 nm, respectively. 14YWT exhibits α-α’ phase separation, Y-rich particles and uniformly distributed W. In addition to those features, 12YWT exhibits Y-Ti-O particles (not Y-O rich) and elongated Cr-rich phases.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A Wide Band Gap Polymer with a Deep Highest Occupied Molecular Orbital Level Enables 14.2% Efficiency in Polymer Solar Cells

To simultaneously achieve low photon energy loss ( E loss ) and broad spectral response, the molecular design of the wide band gap (WBG) donor polymer with a deep HOMO level is of critical importance in fullerene-free polymer solar cells (PSCs). Herein, we developed a new benzodithiophene unit, i.e., DTBDT-EF, and conducted systematic investigations on a WBG DTBDT-EF-based donor polymer, namely, PDTB-EF-T. Due to the synergistic electron-withdrawing effect of the fluorine atom and ester group, PDTB-EF-T exhibits a higher oxidation potential, i.e., a deeper HOMO level (ca. –5.5 eV) than most well-known donor polymers. Hence, a high open-circuit voltage of 0.90 V was obtained when paired with a fluorinated small molecule acceptor (IT-4F), corresponding to a low E loss of 0.62 eV. Furthermore, side-chain engineering demonstrated that subtle side-chain modulation of the ester greatly influences the aggregation effects and molecular packing of polymer PDTB-EF-T. With the benefits of the stronger interchain π–π interaction, the improved ordering structure, and thus the highest hole mobility, the most symmetric charge transport and reduced recombination are achieved for the linear decyl-substituted PDTB-EF-T (P2)-based PSCs, leading to the highest short-circuit current density and fill factor (FF). Due to the high Flory–Huggins interaction parameter (χ), surface-directed phase separation occurs in the P2:IT-4F blend, which is supported by X-ray photoemission spectroscopy results and cross-sectional transmission electron microscope images. By taking advantage of the vertical phase distribution of the P2:IT-4F blend, a high power conversion efficiency (PCE) of 14.2% with an outstanding FF of 0.76 was recorded for inverted devices. Lastly, these results demonstrate the great potential of the DTBDT-EF unit for future organic photovoltaic applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗