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DOE OSTI2024

Block copolymer self-assembly derived mesoporous magnetic materials with three-dimensionally (3D) co-continuous gyroid nanostructure

Magnetic nanomaterials are gaining interest for their many applications in technological areas from information science and computing to next-generation quantum energy materials. While magnetic materials have historically been nanostructured through techniques such as lithography and molecular beam epitaxy, there has recently been growing interest in using soft matter self-assembly. In this work, a triblock terpolymer, poly(isoprene-block-styrene-block-ethylene oxide) (ISO), is used as a structure directing agent for aluminosilicate sol nanoparticles and magnetic material precursors to generate organic–inorganic bulk hybrid films with co-continuous morphology. After thermal processing into mesoporous materials, results from a combination of small angle X-ray scattering (SAXS) and scanning electron microscopy (SEM) are consistent with the double gyroid morphology. Nitrogen sorption measurements reveal a type IV isotherm with H1 hysteresis, and yield a specific surface area of around 200 m 2 g −1 and an average pore size of 23 nm. The magnetization of the mesostructured material as a function of applied field shows magnetic hysteresis and coercivity at 300 K and 10 K. Comparison of magnetic measurements between the mesoporous gyroid and an unstructured bulk magnetic material, derived from the identical inorganic precursors, reveals the structured material exhibits a coercivity of 250 Oe, opposed to 148 Oe for the unstructured at 10 K, and presence of remnant magnetic moment not conventionally found in bulk hematite; both of these properties are attributed to the mesostructure. This scalable route to mesoporous magnetic materials with co-continuous morphologies from block copolymer self-assembly may provide a pathway to advanced magnetic nanomaterials with a range of potential applications.

Chemistry↗

DOE OSTI2024

A Reactor Scale-Up Methodology from Lab-Scale to Pilot-Scale Operations: Numerical Modeling of THFA Dehydration to DHP in Packed-Bed Reactors

This manuscript discusses developing a model-based scale-up methodology for a successful technology transfer of gas-phase catalytic reactors from a lab-scale to a pilot-scale operation. The manuscript demonstrates the methodology for gas-phase dehydration of tetrahydrofurfuryl alcohol (THFA) to dihydropyran (DHP) process over commercial Al 2 O 3 catalysts. A two-dimensional reactor model was developed using COMSOL Multiphysics 6.1 software. The model solves heat and mass transport equations in bed-scale and particle scales simultaneously. This powerful feature enables accurate prediction of the heat and mass transfer limitations in pilot-scale reactors, if any exists. Further, the model uses isothermal lab-scale experimental data to derive and validate the reaction chemistry, flow fields and boundary conditions. The model was then scaled-up to project conversion, selectivity, yield and formation rate of DHP in a pilot-scale reactor. The results highlight the complex nature of chemistry, heat, and mass transfer effects in lab-scale and pilot-scale reactors. The model results inform the possible operational limitations of the pilot-scale reactor and design strategies to improve process efficiency. Although the scale-up approach is explained through the THFA dehydration process, the methodology is applicable to any catalytic packed-bed reactor models for a successful process scale-up.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

The cosmic-ray positron excess and its imprint in the Galactic gamma-ray sky

Abstract We study the origin of the positron excess observed in the local cosmic-ray spectrum at high energies, and relate it to the cosmic rays and gamma-ray emission across the entire Galaxy. In particular, we explore the hypothesis of a single, dominant source accountable for primary electron-positron pairs. Since we are agnostic about the physical nature of the underlying source population, we consider four models that are representative of young pulsars, old stars (as a tracer of millisecond pulsars), and annihilating dark matter particles. In the dark matter hypothesis, we consider both a cored and a cuspy model for the halo in the Milky Way. Then, we compare the associated gamma-ray sky maps withFermi-LAT data. We find that the emission arising from pulsar wind nebulae is fairly concentrated near the mid plane, and therefore additional cosmic-ray sources must be invoked to explain the emission at the center of the Galaxy. If the local positron excess were mainly due to millisecond pulsars, inverse Compton scattering by the particles injected would naturally account for a non-negligible fraction of the central gamma-ray emission. The same process would lead to a tension for a standard NFW dark matter profile, exceeding the gamma-ray data by almost a factor of 2 in some regions of the Galaxy. Although the results for an isothermal, cored profile are in agreement with these data, the cross section needed in both cases is around 2 orders of magnitude above the thermal cross-section, disfavouring the dark matter interpretation.

Astronomy & Astrophysics↗

NASA NTRS1970

Detection and identification of benthic communities and shoreline features in Biscayne Bay

Progress made in the development of a technique for identifying and delinating benthic and shoreline communities using multispectral imagery is described. Images were collected with a multispectral scanner system mounted in a C-47 aircraft. Concurrent with the overflight, ecological ground- and sea-truth information was collected at 19 sites in the bay and on the shore. Preliminary processing of the scanner imagery with a CDC 1604 digital computer provided the optimum channels for discernment among different underwater and coastal objects. Automatic mapping of the benthic plants by multiband imagery and the mapping of isotherms and hydrodynamic parameters by digital model can become an effective predictive ecological tool when coupled together. Using the two systems, it appears possible to predict conditions that could adversely affect the benthic communities. With the advent of the ERTS satellites and space platforms, imagery data could be obtained which, when used in conjunction with water-level and meteorological data, would provide for continuous ecological monitoring.

Kolipinski, M. C.↗

NASA NTRS1972

Transient-forced convection film boiling on an isothermal flat plate.

Development of a new approach for the solution of transient-forced convection film boiling on an isothermal flat plate using the boundary layer model. The similarity variables are used to convert the governing partial differential equations to ordinary ones. The results of numerical solutions of these ordinary equations indicate that the transient process can be classified as one-dimensional conduction, intermediate, and the steady-state regions. The time required for the one-dimensional conduction and the time necessary to attain a steady-state condition are obtained. The use of local similarity approximations for the intermediate regime facilitates prediction of complete boundary layer growth. Using the ratio of time at any instant to the steady-state time as abscissa, the curves representing the boundary layer growth can be merged into a single mean curve within 5%. Further, the analysis shows that the average rate of heat transfer during transient is 50 to 100% higher than those at steady state. The average rate of vapor convected away is 10 to 15% lower than at steady state while the average rate of accumulation to form the vapor layer is 1 to 14 times larger.

Nagendra, H. R.↗

NASA NTRS1973

Isothermal and cyclic oxidation at 1000 and 1100 deg C of four nickel-base alloys: NASA-TRW VIA, B-1900, 713C, and 738X

The isothermal and cyclic oxidation resistance of four cast Ni-base gamma + gamma prime alloys, NASA-TRW Via, B-1900, 713C, and 738X, was determined in still air at 1000 and 1100 C. The oxidation process was evaluated by specific sample weight change with time, sample thickness change, X-ray diffraction of the scales, and sample metallography. The behavior is discussed in terms of the Cr, Al, and refractory metal contents of the alloys.

Barrett, C. A.↗

NASA NTRS1977

A strategy for analysis of thermal decomposition of polymeric materials

Some analytical methods developed in flammability research are reviewed. Computerized analytical systems are used to separate, identify, and quantify components of complex mixtures of low-boiling volatiles, high-boiling volatiles, and solid residues resulting from pyrolysis, oxidative degradation, and flaming combustion processes. To demonstrate the procedure for determining a material's response to a thermal flux administered under dynamic conditions, the treatment of data is reported for samples of an aromatic polyamide fabric which were degraded under isothermal conditions of 550 C following a dynamic heating rate of 100 C/min from ambient to final temperature.

Einhorn, I. N.↗

NASA NTRS1993

System integration and demonstration of adhesive bonded high temperature aluminum alloys for aerospace structure, phase 2

Adhesive bonding materials and processes were evaluated for assembly of future high-temperature aluminum alloy structural components such as may be used in high-speed civil transport aircraft and space launch vehicles. A number of candidate high-temperature adhesives were selected and screening tests were conducted using single lap shear specimens. The selected adhesives were then used to bond sandwich (titanium core) test specimens, adhesive toughness test specimens, and isothermally aged lap shear specimens. Moderate-to-high lap shear strengths were obtained from bonded high-temperature aluminum and silicon carbide particulate-reinforced (SiC(sub p)) aluminum specimens. Shear strengths typically exceeded 3500 to 4000 lb/in(sup 2) and flatwise tensile strengths exceeded 750 lb/in(sup 2) even at elevated temperatures (300 F) using a bismaleimide adhesive. All faceskin-to-core bonds displayed excellent tear strength. The existing production phosphoric acid anodize surface preparation process developed at Boeing was used, and gave good performance with all of the aluminum and silicon carbide particulate-reinforced aluminum alloys investigated. The results of this program support using bonded assemblies of high-temperature aluminum components in applications where bonding is often used (e.g., secondary structures and tear stoppers).

Falcone, Anthony↗

DOE OSTI2024

High Temperature, Isothermal Growth Promotes Close Packing and Thermal Stability in DNA-Engineered Colloidal Crystals

Here, we report a strategy to accelerate the synthesis and increase the crystallinity of colloidal crystals engineered with DNA. Specifically, by holding the DNA-modified Au particle building blocks above the T m of the individual nanoparticle building blocks, but slightly below the T m of the anticipated colloidal crystal during the assembly process, crystallinity is increased, and enthalpically-favored phases with high degrees of facet registration are observed. We studied the utility of this approach with systems for which the commonly adopted slow-cooling approach yielded primarily amorphous aggregates. In particular, we used it to synthesize high-volume fraction colloidal crystals from large (80 nm) anisotropic nanoparticles (cubes and rhombic dodecahedra) with short (<14 nm) DNA designed to restrict the degrees of freedom for the DNA bonds and maintain the anisotropy of the particle building block. Small-angle X-ray scattering and electron microscopy studies show that the crystalline phases synthesized via this method are more thermally stable than their corresponding aggregate phases, likely due to an increased number of DNA-DNA bonds between particles. Crystal size tunability (between 0.5 and 15 µm edge lengths) and epitaxial growth were demonstrated using this strategy by modulating the NaCl concentration in tandem with previously synthesized colloidal crystal nuclei. Taken together, this isothermal strategy provides a route to deliberately crystallize a wide variety of anisotropic colloidal materials and expands the phase space accessible to nanoparticles modified with DNA.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1989

Numerical studies of convective heat transfer in an inclined semiannular enclosure

Natural convection heat transfer in a two-dimensional differentially heated semiannular enclosure is studied. The enclosure is isothermally heated and cooled at the inner and outer walls, respectively. A commercial software based on the SIMPLER algorithm was used to simulate the velocity and temperature profiles. Various parameters that affect the momentum and heat transfer processes were examined. These parameters include the Rayleigh number, Prandtl number, radius ratio, and the angle of inclination. A flow regime extending from conduction-dominated to convection-dominated flow was examined. The computed results of heat transfer are presented as a function of flow parameter and geometric factors. It is found that the heat transfer rate attains a minimum when the enclosure is tilted about +50 deg with respect to the gravitational direction.

Wang, Lin-Wen↗

NASA NTRS1989

Numerical studies of convective heat transfer in an inclined semi-annular enclosure

Wang, L.-W.↗

NASA NTRS1994

Hydrographic section across the Kuroshio near 35 deg N, 143 deg E

A closely spaced conductivity-temperature-depth/hydrographic section was conducted off the east coast of Japan in July 1992. The southeastward section crossed the Japan Trench and the Kuroshio in the vicinity of the Kashima 1 seamount. Vertical sections of temperature, salinity, density, oxygen, and nutrients are discussed in conjunction with the movement and interleaving of water masses. Complicated vertical and horizontal mixings of water masses are inferred from the temperature and salinity relationships. Mixing processes are patchy and not continuous beneath the front. Warm, salty water found beneath the Kurishio may result from upward mixing of water from intermediate depths. The main axis of the Kurishio, indicated by the 14 C isotherm at 200 m, is at 35.7 deg N, 142.6 deg E, about 20 km from the north wall surface thermal front. Geostrophic speeds exceed 170 cm/s at the surface; volume transport through the section is 81 x 10(exp 6) cu m/s.

Teague, W. J.↗

NASA NTRS1999

The Thermal Structure of Triton's Middle Atmosphere

The atmospheric structure of Triton in the altitude range 25-150 kilometers shows an unexpectedly steep thermal gradient of 0.26 K per kilometer above 50 kilometer altitude, with a nearly isothermal profile below. The upper part of the profile can be explained by downward conduction of heat deposited by magnetospheric electrons and solar UV. However, the atmospheric temperature below 50 kilometers is too cold for identified radiative processes to dispose of the inferred heat flux (0.0012 erg per square centimeter per second) from the upper atmosphere. This implies that either the atmosphere is not in a steady state and/or an unidentified cooling mechanism is at work in the altitude range 25-50 kilometers. When extrapolated to the surface, the inversion results yield a pressure of 19.0 sup (+1.8) sub (-1.5), mubar, about 5mubar greater than that observed by Voyager.

Elliot, J. L.↗

NASA NTRS2002

Splashing Droplets

Current data on droplet breakup is scarce for the sizes and velocities typical of practical applications such as in spray combustion processes and coating processes. While much more representative of practical applications, the small spatial scales and rapid time-scales prevent detailed measurement of the internal fluid dynamics and liquid property gradients produced by impinging upon surfaces. Realized through the extended spatial and temporal scales afforded by a microgravity environment, an improved understanding of drop breakup dynamics is sought to understand and ultimately control the impingement dynamics of droplets upon surfaces in practical situations. The primary objective of this research will be to mark the onset of different 'splashing modes' and to determine their temperature, pressure and angle dependence for impinging droplets representative of practical fluids. In addition, we are modeling the evolution of droplets that do not initially splash but rather undergo a 'fingering' evolution observed on the spreading fluid front and the transformation of these fingers into splashed products. An example of our experimental data is presented below. These images are of Isopar V impacting a mirror-polished surface. They were acquired using a high-speed camera at 1000 frames per second. They show the spreading of a single droplet after impact and ensuing finger instabilities. Normal gravity experimental data such as this will guide low gravity measurements in the 2.2 second drop tower and KC-135 aircraft as available. Presently we are in the process of comparing the experimental data of droplet shape evolution to numerical models, which can also capture the internal fluid dynamics and liquid property gradients such as produced by impingement upon a heated surface. To-date isothermal numerical data has been modeled using direct numerical simulations of representative splashing droplets. The data obtained so far indicates that the present model describes well the droplet wall interactions to a point in time just before splash. Additional information is included in the original extended abstract.

VanderWal, Randall L.↗

DOE OSTI2026

Testing of High S Matrix Glasses to Expand DFHLW Glass Compositional Ranges (Rev.1)

Gaps in glass composition-property data for direct-feed high-level waste (DFHLW) have recently been identified. One such gap is the region of high sulfur solubility since previous, pretreated, high-level wastes contained very little sulfur. Filling this data gap will significantly broaden the range of process flowsheet options including minimal washing and will allow for optimized waste loading in DFHLW glasses. This report summarizes the data collected during the characterization of the DFHLW High S Glass Matrix (HS24). A glass matrix of 50 glass compositions was developed to evenly cover the DFHLW composition region for high sulfur glass. Matrix glasses were designed to expand the composition region outside the current component concentration and property limits so as to reduce uncertainties at the limits. The 50 matrix glasses were fabricated and tested for properties important to the success of DFHLW vitrification including: compositions, canister centerline cooling (CCC) crystallinity and isothermal crystallinity, density, viscosity, electrical conductivity (EC), product consistency test (PCT) response, toxicity, and sulfate solubility. Melter materials corrosion testing is reported elsewhere. These glasses were intentionally designed to have high SO 3 solubilities (0.7 to 2.2 SO 3 wt%) in compositional regions that had not been previously explored. Forty-eight glasses showed the measured SO 3 content retained >80% of the target SO 3 and the densities of all the glasses ranged from 2.49 g·cm -3 to 2.74 g·cm -3 . While the model predicted nepheline formation in 5 glasses, one of the tested 50 CCC glasses formed nepheline, and 35 glasses formed Cr-containing phases such as spinels and eskolaite. Only five glasses were amorphous after CCC treatment where 44 glasses with detectable crystals contained =10 wt% crystals and only one glass had > 10 wt% crystals. None of the glasses exceeded the allowable T 2% for spinel crystal formation at 950 ºC (i.e., no glasses had >2 wt% spinel at 950 ºC) during isothermal crystal fraction tests where 10 glasses showed no crystalline phases at or below 950 ºC. All the glasses (except one which failed being slightly lower than the target) satisfied the SO 3 constraint while 98 glasses did not meet the viscosity constraints and 4 failed the EC constraints. Six quenched (Q) and six CCC glasses failed the Defense Waste Processing Facility (DWPF) Environmental Assessment (EA) glass PCT threshold and 3 Q and 4 CCC failed the PCT design constraint. One glass exceeded the WTP delisting limits for Cr via EPA Method 1311 (i.e., Toxicity Characteristic Leaching Procedure, TCLP). It should be emphasized that some of these glasses were specifically designed to approach or even exceed certain property constraints, as filling data gaps in these regions will provide the greatest benefit for future model development by improving accuracy and reducing uncertainties. These insights will ultimately support the development of more robust glass formulation strategies, enabling higher waste loading, reducing operational risks, and expanding the processing envelope.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Development of Calcined Clay/Calcium Sulfate Blends for Robust Performance of LC3 Concrete

This report documents the development of robust blends of calcined clays (CCs) with calcium sulfate (gypsum) for application in limestone calcined clay cement (LC3) systems. The U.S. cement industry faces supply chain constraints and high energy intensity, motivating the need for alternative supplementary cementitious materials. Calcined clays are abundant and highly reactive when properly processed, but their variable physical and chemical characteristics can negatively impact hydration balance, rheology, and admixture demand in LC3 concretes. To address this, five calcined clays, two Portland cements, ground limestone, gypsum, and a polycarboxylate dispersant were procured. Isothermal calorimetry and mini-cone flow tests were used to determine sulfate and dispersant demand. Results show that the addition of approximately 6.7% gypsum, relative to the calcined clay weight, consistently balanced sulfate consumption across the LC3 systems studied. Dispersant demand, however, varied significantly with clay source, demonstrating the need for tailored admixture strategies. These findings confirm that supplying CC–gypsum blends directly to concrete producers is a viable approach to overcoming current manufacturing constraints, enabling reliable fresh and hardened performance of LC3 concretes, and supporting broader adoption of calcined clays in the U.S. market.

36 MATERIALS SCIENCE↗

NASA NTRS1971

Transient-forced convection film boiling on an isothermal flat plate

An approach for the solution of transient-forced convection film boiling on an isothermal flat plate using the boundary layer model is developed. The similarity variables are used to convert the governing partial differential equations to ordinary ones. The results of numerical solutions of these ordinary equations indicate that the transient process can be classified as one-dimensional conduction, intermediate, and the steady state regions. The time required for the one-dimensional conduction and the time necessary to attain a steady state condition are obtained. The influence of interfacial shear is seen to be negligible while the Prandtl Number and the ratio (C sub p delta T divided by h sub fg times Pr) have major influence. The use of local similarity approximations for the intermediate regime facilitates prediction of complete boundary layer growth. Using the ratio of time at any instant to the steady state time as abscissa, the curves representing the boundary layer growth can be merged into a single mean curve within 5 percent. Further, the analysis shows that the average rate of heat transfer during transient is 50 to 100 percent higher than those at steady state. The average rate of vapor convected away is 10 to 15 percent lower than at steady state while the average rate of accumulation to form the vapor layer is 1 to 14 times larger. Further, the total heat transferred during transient increases and the evaporation decreases for increasing values of C sub p delta T divided by h sub fg times Pr

Nagendra, H. R.↗

NASA NTRS1999

Boronate affinity adsorption of RNA: possible role of conformational changes

Batch equilibrium adsorption isotherm determination is used to characterize the adsorption of mixed yeast RNA on agarose-immobilized m-aminophenylboronic acid. It is shown that the affinity-enhancing influence of divalent cations depends strongly on the precise nature of the cation used, with barium being far more effective than the conventionally-used magnesium. This adsorption-promoting influence of barium is suggested to arise primarily from ionic influences on the structure and rigidity of the RNA molecule, as the adsorption of ribose-based small molecules is not similarly affected. The substitution of barium for the standard magnesium counterion does not greatly promote the adsorption of DNA, implying that the effect is specific to RNA and may be useful in boronate-based RNA separations. RNA adsorption isotherms exhibit sharp transitions as functions of temperature, and these transitions occur at different temperatures with Mg2+ and with Ba2+. Adsorption affinity and capacity were found to increase markedly at lower temperatures, suggestive of an enthalpically favored interaction process. The stoichiometric displacement parameter, Z, in Ba2+ buffer is three times the value in Mg2+ buffer, and is close to unity.

NASA Discipline Environmental Health↗