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DOE OSTI2021

A Theoretical Model for Computing Freezing Point Depression of Lithium-Ion Battery Electrolytes

Reliable prediction of freezing point depression in liquid electrolytes will accelerate the development of improved Li-ion batteries which can operate in low temperature environments. In this work we establish a computational methodology to calculate activity coefficients and liquidus lines for battery-relevant liquid electrolytes. Electronic structure methods are used in conjuction with classical molecular dynamics simulations and theoretical expressions for Born solvation energy, ion-atmosphere effects from Debye-Hückel theory and solvent entropic effects. The framework uses no a priori knowledge beyond neat solvent properties and the concentration of salt. LiPF 6 in propylene carbonate (PC), LiPF 6 in dimethyl carbonate (DMC) and LiClO 4 in DMC are investigated up to 1 molal with accuracy better than 3 °C when compared to experimental freezing point measurements. Finally, we find that the difference in freezing point depression between the propylene carbonate-based electrolyte and the dimethyl carbonate electrolytes originates from the difference in the solvent dielectric constant.

25 ENERGY STORAGE↗

DOE OSTI2021

Active virus-host interactions at sub-freezing temperatures in Arctic peat soil

Abstract Background Winter carbon loss in northern ecosystems is estimated to be greater than the average growing season carbon uptake and is primarily driven by microbial decomposers. Viruses modulate microbial carbon cycling via induced mortality and metabolic controls, but it is unknown whether viruses are active under winter conditions (anoxic and sub-freezing temperatures). Results We used stable isotope probing (SIP) targeted metagenomics to reveal the genomic potential of active soil microbial populations under simulated winter conditions, with an emphasis on viruses and virus-host dynamics. Arctic peat soils from the Bonanza Creek Long-Term Ecological Research site in Alaska were incubated under sub-freezing anoxic conditions with H 2 18 O or natural abundance water for 184 and 370 days. We sequenced 23 SIP-metagenomes and measured carbon dioxide (CO 2 ) efflux throughout the experiment. We identified 46 bacterial populations (spanning 9 phyla) and 243 viral populations that actively took up 18 O in soil and respired CO 2 throughout the incubation. Active bacterial populations represented only a small portion of the detected microbial community and were capable of fermentation and organic matter degradation. In contrast, active viral populations represented a large portion of the detected viral community and one third were linked to active bacterial populations. We identified 86 auxiliary metabolic genes and other environmentally relevant genes. The majority of these genes were carried by active viral populations and had diverse functions such as carbon utilization and scavenging that could provide their host with a fitness advantage for utilizing much-needed carbon sources or acquiring essential nutrients. Conclusions Overall, there was a stark difference in the identity and function of the active bacterial and viral community compared to the unlabeled community that would have been overlooked with a non-targeted standard metagenomic analysis. Our results illustrate that substantial active virus-host interactions occur in sub-freezing anoxic conditions and highlight viruses as a major community-structuring agent that likely modulates carbon loss in peat soils during winter, which may be pivotal for understanding the future fate of arctic soils' vast carbon stocks.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Micro-spectroscopic and freezing characterization of ice-nucleating particles collected in the marine boundary layer in the eastern North Atlantic

Abstract. Formation of atmospheric ice plays a crucial role in the microphysical evolution of mixed-phase and cirrus clouds and thus climate. How aerosol particles impact ice crystal formation by acting as ice-nucleating particles (INPs) is a subject of intense research activities. To improve understanding of atmospheric INPs, we examined daytime and nighttime particles collected during the Aerosol and Cloud Experiments in the Eastern North Atlantic (ACE-ENA) field campaign conducted in summer 2017. Collected particles, representative of a remote marine environment, were investigated for their propensity to serve as INPs in the immersion freezing (IMF) and deposition ice nucleation (DIN) modes. The particle population was characterized by chemical imaging techniques such as computer-controlled scanning electron microscopy with energy-dispersive X-ray analysis (CCSEM/EDX) and scanning transmission X-ray microscopy with near-edge X-ray absorption fine-structure spectroscopy (STXM/NEXAFS). Four major particle-type classes were identified where internally mixed inorganic–organic particles make up the majority of the analyzed particles. Following ice nucleation experiments, individual INPs were identified and characterized by SEM/EDX. The identified INP types belong to the major particle-type classes consisting of fresh sea salt with organics or processed sea salt containing dust and sulfur with organics. Ice nucleation experiments show IMF events at temperatures as low as 231 K, including the subsaturated regime. DIN events were observed at lower temperatures of 210 to 231 K. IMF and DIN observations were analyzed with regard to activated INP fraction, ice-nucleation active site (INAS) densities, and a water activity-based immersion freezing model (ABIFM) yielding heterogeneous ice nucleation rate coefficients. Observed IMF and DIN events of ice formation and corresponding derived freezing rates demonstrate that the marine boundary layer aerosol particles can serve as INPs under typical mixed-phase and cirrus cloud conditions. The derived IMF and DIN parameterizations allow for implementation in cloud and climate models to evaluate predictive effects of atmospheric ice crystal formation.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

A new method for operating a continuous-flow diffusion chamber to investigate immersion freezing: assessment and performance study

Abstract. Glaciation in mixed-phase clouds predominantly occurs through the immersion-freezing mode where ice-nucleating particles (INPs) immersed within supercooled droplets induce the nucleation of ice. Model representations of this process currently are a large source of uncertainty in simulating cloud radiative properties, so to constrain these estimates, continuous-flow diffusion chamber (CFDC)-style INP devices are commonly used to assess the immersion-freezing efficiencies of INPs. This study explored a new approach to operating such an ice chamber that provides maximum activation of particles without droplet breakthrough and correction factor ambiguity to obtain high-quality INP measurements in a manner that previously had not been demonstrated to be possible. The conditioning section of the chamber was maintained at −20 ∘C and water relative humidity (RHw) conditions of 113 % to maximize the droplet activation, and the droplets were supercooled with an independently temperature-controlled nucleation section at a steady cooling rate (0.5 ∘C min−1) to induce the freezing of droplets and evaporation of unfrozen droplets. The performance of the modified compact ice chamber (MCIC) was evaluated using four INP species: K-feldspar, illite-NX, Argentinian soil dust, and airborne soil dusts from an arable region that had shown ice nucleation over a wide span of supercooled temperatures. Dry-dispersed and size-selected K-feldspar particles were generated in the laboratory. Illite-NX and soil dust particles were sampled during the second phase of the Fifth International Ice Nucleation Workshop (FIN-02) campaign, and airborne soil dust particles were sampled from an ambient aerosol inlet. The measured ice nucleation efficiencies of model aerosols that had a surface active site density (ns) metric were higher but mostly agreed within 1 order of magnitude compared to results reported in the literature.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

A new method for operating a continuous flow diffusion chamber to investigate immersion freezing: assessment and performance study

Glaciation in mixed-phase clouds predominately occurs through the immersion freezing mode where ice nucleating particles (INPs) immersed within supercooled droplets induce nucleation of ice. Currently, model representations of this process are a large source of uncertainty in simulating cloud radiative properties, and to constrain these estimates, continuous flow diffusion chamber (CFDC)-style INP devices are commonly used to assess the immersion freezing efficiencies of INPs. In this study, a new approach was explored to operating such an ice chamber that provides maximum activation of particles without droplet breakthrough and correction factor ambiguity to obtain high-quality INP measurements in a manner that has not been demonstrated as possible previously. The conditioning section of the chamber was maintained at ~ –20 °C and water relative humidity (RH w ) ~ 113 % conditions to maximize the droplet activation, and the droplets were supercooled with an independently temperature-controlled nucleation section at a steady cooling rate (0.5 °C min –1 ) to induce the freezing of droplets and evaporation of unfrozen droplets. The performance of the modified ice chamber was evaluated using four INP species: K-feldspar, illite-NX, Argentinian soil dust, and airborne arable dust that had shown ice nucleation over a wide span of supercooled temperatures. Dry dispersed and size-selected K-feldspar particles were generated in the laboratory. Illite-NX and soil dust particles were sampled during the second phase of the Fifth International Ice Nucleation Workshop (FIN-02) campaign, and airborne arable dust particles were sampled from the aerosol inlet located on the rooftop of the laboratory. The measured ice nucleation efficiencies of model aerosols with a surface active site density (n s ) metric were higher, but mostly agreed within one order of magnitude compared to literature results.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1971

Modification of physical properties of freeze-dried rice

Freeze cycling process consists of alternately freezing and thawing precooked rice for two cycles, rice is then frozen and freeze-dehydrated in vacuum sufficient to remove water from rice by sublimitation. Process modifies rice grain structure and porosity, enabling complete rehydration in one minute in hot water.

Huber, C. S.↗

NASA NTRS1979

Design and evaluation of aircraft heat source systems for use with high-freezing point fuels

The objectives were the design, performance and economic analyses of practical aircraft fuel heating systems that would permit the use of high freezing-point fuels on long-range aircraft. Two hypothetical hydrocarbon fuels with freezing points of -29 C and -18 C were used to represent the variation from current day jet fuels. A Boeing 747-200 with JT9D-7/7A engines was used as the baseline aircraft. A 9300 Km mission was used as the mission length from which the heat requirements to maintain the fuel above its freezing point was based.

Pasion, A. J.↗

NASA NTRS1979

High-freezing-point fuels used for aviation turbine engines

Broadened-specification aviation fuels could be produced from a greater fraction of crude source material with improvements in fuel supply and price. These fuels, particularly those with increased final boiling temperatures, would have higher freezing temperatures than current aviation turbine fuels. The higher-freezing-point fuels can be substituted in the majority of present commercial flights, since temperature data indicate that in-flight fuel temperatures are relatively mild. For the small but significant fraction of commercial flights where low fuel temperatures make higher freezing-point fuel use unacceptable, adaptations to the fuel or fuel system may be made to accommodate this fuel. Several techniques are discussed. Fuel heating is the most promising concept. One simple system design uses existing heat rejection from the fuel-lubricating oil cooler, another uses an engine-driven generator for electrical heating. Both systems offer advantages that outweigh the obvious penalties.

Friedman, R.↗

NASA NTRS1980

Temperature and flow measurements on near-freezing aviation fuels in a wing-tank model

Freezing behavior, pumpability, and temperature profiles for aviation turbine fuels were measured in a 190-liter tank chilled to simulate internal temperature gradients encountered in commercial airplane wing tanks. When the bulk of the fuel was above the specification freezing point, pumpout of the fuel removed all fuel except a layer adhering to the bottom chilled surfaces, and the unpumpable fraction depended on the fuel temperature near these surfaces. When the bulk of the fuel was at or below the freezing point, pumpout ceased when solids blocked the pump inlet, and the unpumpable fraction depended on the overall average temperature.

Friedman, R.↗

NASA NTRS1980

Temperature and flow measurements on near-freezing aviation fuels in a wing-tank model

Freezing behavior, pumpability, and temperature profiles for aviation turbine fuels were measured in a 190-liter tank, to simulate internal temperature gradients encountered in commercial airplane wing tanks. Two low-temperature situations were observed. Where the bulk of the fuel is above the specification freezing point, pumpout of the fuel removes all fuel except a layer adhering to the bottom chilled surfaces, and the unpumpable fraction depends on the fuel temperature near these surfaces. Where the bulk of the fuel is at or below the freezing point, pumpout ceases when solids block the pump inlet, and the unpumpable fraction depends on the overall average temperature.

Friedman, R.↗

NASA NTRS1952

A Photographic Study of Freezing of Water Droplets Falling Freely in Air

A photographic technique for investigating water droplets of diameter less than 200 microns falling freely in air at temperatures between 0 C and -50 C has been devised and used to determine: (i) The shape of frozen droplets (2) The occurrence of collisions of partly frozen or of frozen and liquid droplets (3) The statistics on the freezing temperatures of individual free-falling droplets A considerable number of droplets were found to have a nonspherical shape after freezing because of various protuberances and frost growth, and droplet aggregates formed by collision. The observed frequency of collision of partly frozen droplets showed good order of magnitude agreement with the frequency computed from theoretical collection efficiencies. The freezing temperature statistics indicated a general similarity of the data to those obtained for droplets frozen on a metallic surface in previous experiments.

Dorsch, Robert G.↗

NASA NTRS1982

Evaluation of methods for rapid determination of freezing point of aviation fuels

Methods for identification of the more promising concepts for the development of a portable instrument to rapidly determine the freezing point of aviation fuels are described. The evaluation process consisted of: (1) collection of information on techniques previously used for the determination of the freezing point, (2) screening and selection of these techniques for further evaluation of their suitability in a portable unit for rapid measurement, and (3) an extensive experimental evaluation of the selected techniques and a final selection of the most promising technique. Test apparatuses employing differential thermal analysis and the change in optical transparency during phase change were evaluated and tested. A technique similar to differential thermal analysis using no reference fuel was investigated. In this method, the freezing point was obtained by digitizing the data and locating the point of inflection. Results obtained using this technique compare well with those obtained elsewhere using different techniques. A conceptual design of a portable instrument incorporating this technique is presented.

Mathiprakasam, B.↗

NASA NTRS1982

Response of MnBi-Bi eutectic to freezing rate changes

Reference is made to a study by Fu and Wilcox (1981), which treated theoretically the influence on freezing rate of sudden changes in translation rate in the Bridgman-Stockbarger technique. This treatment is extended here to a linear ramped translation rate and an oscillatory freezing rate. It is found that oscillations above a few hertz are highly damped in small-diameter apparatus. An experimental test is carried out of the theoretical predictions for a sudden change of translation rate. The MnBi-Bi eutectic is solidified with current-induced interface demarcation. The experimental results accord reasonably well with theory if the silica ampoule wall is assumed to either (1) contribute only a resistance to heat exchange between the sample and the furnace wall or (2) transmit heat effectively in the axial direction by radiation. In an attempt to explain the fact that a finer microstructure is obtained in space, MnBi-Bi microstructure is determined when the freezing rate is increased or decreased rapidly. Preliminary results suggest that fiber branching does not occur as readily as fiber termination.

Nair, M.↗

NASA NTRS1990

Radiobrightness of diurnally heated, freezing soil

Freezing and thawing soils exhibit unique radiometric characteristics. To examine these characteristics, diurnal insolation is modeled as one-dimensional heating of a moist soil half-space during a typical fall at a northern Great Plains site. The one-dimensional heat flow equation is nonlinear because both the enthalpy (the change in internal energy with temperature at constant pressure) and the thermal conductivity of freezing soils are nonlinear functions of temperature. The problem is particularly difficult because phase boundaries propagate in time, and because soils, particularly clay-rich soils, freeze over a range of temperatures rather than at 0 C. Diurnal radiobrightness curves at 10.7, 18.0, and 37.0-GHz were computed for each month. The 37.0-GHz radiobrightness best tracks soil surface temperature; the 10.7-37.0-GHz spectral gradient of thawed soils is strongly positive; the spectral gradient of frozen soils is slightly negative; and the midnight-to-noon spectral gradient is shifted by approximately +0.1 K/GHz by diurnal changes in the surface temperature and the thermal gradient. These observations support the use of the scanning multichannel microwave radiometer 37.0-GHz radiobrightness and its 10.7-37.0-GHz spectral gradient as discriminants in a frozen soil classifier for high-latitude prairie.

England, Anthony W.↗

NASA NTRS1992

Atmospheric concentrations of submicron contact-freezing nuclei

Atmospheric concentrations of contact-freezing nuclei were measured using a technique primarily sensitive to submicron aerosol particles. Diffusion and phoretic forces were relied on for the capture of nuclei by supercooled drops of distilled water exposed to the sample air. Nucleus concentrations were deduced from the rate at which the drops were observed to freeze, interpreting that rate on the basis of a theoretical prediction of aerosol capture rate for different assumed sizes of the nuclei. Measurements at Laramie, Wyoming, yielded average concentrations of contact-freezing nuclei of 1.7/L at -15 C and 3.1/L at -18 C for an assumed radius of 0.01 micron for the nucleating particles.

Deshler, Terry↗

NASA NTRS1992

Freezing in confined geometries

Results of detailed structural studies, using elastic neutron scattering, of the freezing of liquid O2 and D2 in porous vycor glass, are presented. The experimental studies have been complemented by computer simulations of the dynamics of freezing of a Lennard-Jones liquid in narrow channels bounded by molecular walls. Results point to a new simple physical interpretation of freezing in confined geometries.

Sokol, P. E.↗

NASA NTRS1993

Freeze-Drying Makes Improved IPN And Semi-IPN Polymers

Novel process developed for production of interpenetrating polymer networks (IPN's) or semi-IPN's with greater fracture toughness and resistance to microcracks. Process controls degree of phase separation in IPN's. In experiment, IPN's and semi-IPN's formed by dissolving constituents in another common solvent in traditional method. Resins and composite materials produced were tested for both traditional and freeze-drying processes. Glass-transition temperatures and data from dynamic mechanical tests of freeze-dried IPN's and semi-IPN's demonstrated freeze-drying process provided much improved IPN's and semi-IPN's.

Pater, Ruth H.↗

NASA NTRS1991

Mechanisms of voids formation during cooldown and freezing of lithium in SP-100 type systems

The mechanisms of void formation during the cooldown and freezing of lithium coolant within the primary loop of SP-100 type systems are investigated. These mechanisms are: (a) homogeneous nucleation, (b) heterogeneous nucleation, (c) normal segregation of helium gas dissolved in liquid lithium, and (d) shrinkage of lithium during freezing. To evaluate the void formation potential due to segregation, a numerical scheme that couples the freezing and mass diffusion processes in both the solid and liquid regions is developed. The results indicated that the formation of He bubbles is unlikely by either homogeneous or heterogeneous nucleation during the cooldown process. However, homogeneous nucleation of He bubbles following the segregation of dissolved He in liquid Lithium ahead of the solid-liquid interface is likely to occur. Results also show that total volume of He void is insignificant when compared to that of shrinkage voids.

Yang, Jae Y.↗