Microgravity Investigation of Supercooled Fragile Liquid Metal Oxides
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Microgravity Investigation of Supercooled Fragile Liquid Metal Oxides
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Richard Weber↗
Measuring the Density, Viscosity, and Surface Tension of Molten Titanates Using Electrostatic Levitation in Microgravity
Rare earth and barium titanates are useful as ferroelectric, dielectric, and optical materials. Measurements of their thermophysical properties in the liquid state can help guide melt processing technologies for their manufacture and advance understanding of fragile liquids' behavior and glass formation. Here, we report the density, thermal expansion, viscosity, and surface tension of molten BaTiNsub>2 O 5 , BaTi 4 O 9 , and 83TiO 2 -17RE 2 O 3 (RE = La or Nd). Measurements were made using electrostatic levitation and droplet oscillation techniques in microgravity, which provide access to quiescent liquid droplets and deep supercooling of 510–815 K below the equilibrium melting points. Densities were measured over 900–2400 K. Viscosities were similar for all four compositions, increasing from ∼10 mPa s near 2100 K to ∼30 mPa s near 1750 K. Surface tensions were 450–490 dyn cm −1 for the rare earth titanates and 383–395 dyn cm−1 for the barium titanates; surface tensions of all compositions had small or negligible temperature dependence over 1700–2200 K. For solids recovered after melt quenching, x-ray microtomography revealed the fracture mechanics in crystalline products and minimal internal porosity in glass products, likely arising from entrapped gas bubbles. Internal microstructures were generally similar for products processed either in microgravity or in a terrestrial aerodynamic levitator.
Stephen K Wilke↗
On the location of the maximum homogeneous crystal nucleation temperature
Detailed considerations are given to the location of the temperature of maximum homogeneous nucleation as predicted by classical nucleation theory. It is shown quite generally that this maximum temperature, T-asterisk, must occur above the Kauzmann temperature and that the T-asterisk is such that T-asterisk is greater than T(m)/3, where T(m) is the melting temperature. Also, it is demonstrated tha T-asterisk may be considered to be approximately dependent upon two parameters: gamma, the ratio of the difference in specific heat between the crystal and liquid divided by the entropy of fusion, and E, a reduced activation energy for viscous flow. The variation of T-asterisk with these parameters is described. The relationship of the relative location of T-asterisk to the glass transition temperature, is discussed too. This discussion is couched within the framework of the strong and fragile liquid notion introduced by Angell (1981) and coworkers. Finally, the question of the ultimate limits to the undercooling of liquid metals is considered and its relationhsip to computations of the maximum nucleation temperature in such systems.
Weinberg, Michael C.↗
Correlation of the fragility of metallic liquids with the high temperature structure, volume, and cohesive energy
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A. K. Gangopadhyay↗
Microgravity Studies of Liquid-Liquid Phase Transitions in Alumina-Yttria Melts
The scientific objective of this research is to increase the fundamental knowledge base for liquid- phase processing of technologically important oxide materials. The experimental objective is to define conditions and hardware requirements for microgravity flight experiments to test and expand the experimental hypotheses that: 1. Liquid phase transitions can occur in undercooled melts by a diffusionless process. 2. Onset of the liquid phase transition is accompanied by a large change in the temperature dependence of melt viscosity. Experiments on undercooled YAG (Y3A15012)- and rare earth oxide aluminate composition liquids demonstrated a large departure from an Arrhenian temperature dependence of viscosity. Liquid YAG is nearly inviscid at its 2240 K melting point. Glass fibers were pulled from melts undercooled by ca. 600 K indicating that the viscosity is on the order of 100 Pans (1000 Poise) at 1600 K. This value of viscosity is 500 times greater than that obtained by extrapolation of data for temperatures above the melting point of YAG. These results show that the liquids are extremely fragile and that the onset of the highly non-Arrhenian viscosity-temperature relationship occurs at a temperature considerably below the equilibrium melting point of the solid phases. Further results on undercooled alumina-yttria melts containing 23-42 mole % yttrium oxide indicate that a congruent liquid-liquid phase transition occurs in the undercooled liquids. The rates of transition are inconsistent with a diffusion-limited process. This research is directed to investigation of the scientifically interesting phenomena of polyamorphism and fragility in undercooled rare earth oxide aluminum oxide liquids. The results bear on the technologically important problem of producing high value rare earth-based optical materials.
Guynes, Buddy↗
Liquid Between Macromolecules in Protein Crystals: Static Versus Dynamics
Protein crystals are so fragile that they often can not be handled by tweezers. Indeed, measurements of the Young modulus, E, of lysozyme crystals resulted in E approx. equals 0.1 - 1 GPa, the lower figures, 0.1 - 0.5 GPa, being obtained from triple point bending of as-grown and not cross-linked crystals sitting in solution. The bending strength was found to be approx.10(exp -2) E. On the other hand, ultrasound speed and Mandelstam-Raman-Brilloin light scattering experiments led to much higher figures, E approx. equals 2.7 GPa. The lower figures for E were found from static or low frequency crystal deformations measurements, while the higher moduli are based on high frequency lattice vibrations, 10(exp 7) - 10(exp 10) 1/s. The physical reason for the about an order of magnitude discrepancy is in different behavior of water filling space between protein molecules. At slow lattice deformation, the not-bound intermolecular water has enough time to flow from the compressed to expanded regions of the deformed crystal. At high deformation frequencies in the ultra- and hypersound waves, the water is confined in the intermolecular space and, on that scale, behaves like a solid, thus contributing to the elastic crystal moduli. In this case, the reciprocal crystal modulus is expected to be an average of the water protein and water compressibilities (reciprocal compressibilities): the bulk modulus for lysozyme is 26 GPa, for water it is 7 GPa. Anisotropy of the crystal moduli comes from intermolecular contacts within the lattice while the high frequency hardness comes from the bulk of protein molecules and water bulk moduli. These conclusions are based on the analysis of liquid flow in porous medium to be presented.
Chernov, A. A.↗
Coal pump development phase 3
Techniques for achieving continuous coal sprays were studied. Coazial injection with gas and pressure atomization were studied. Coal particles, upon cooling, were found to be porous and fragile. Reactivity tests on the extruded coal showed overall conversion to gases and liquids unchanged from that of the raw coal. The potentials for applications of the coal pump to eight coal conversion processes were examined.
Kushida, R. O.↗
Research on High Temperature Ceramic Insulation for Electrical Conductors
Three methods for applying ceramic coatings to wires were examined in depth and a fourth (chemical vapor deposition) was studied briefly. CVD coatings were not reported in the thesis because it was realized early in the study that the deposition rate of the coatings was too slow to be used in a commercial process. Of the methods reported in the thesis, slurry coating was the most promising. This method consists of slowly drawing a platinum wire through a thixotropic slurry of alumina in a vehicle composed of polyvinyl butyral, methyl ethyl ketone, and toluene. The coatings produced by this method were continuous and free of cracks after sintering. The sintered coatings crack when the wire is bent around sharp corners, but most of the coating remains in place and still provides electrical insulation between the wire and any metallic structure to which the wire may be attached. The coating thickness was 0.61 mm (16 micrometers). The electrical resistivity of the intact coating was 340 M-Ohm-cm at 800 C and 23 M-Ohm-cm at 1050 C. Therefore, these coatings more than meet the electrical requirements for use in turbine engines. Although adherence of the coating to the wire was generally excellent, a problem was noted in localized areas where the coating flaked off. Further work will be needed to obtain good coating adherence along the entire length of the wire. The next most promising coatings were made by electrophoretic deposition (EPD) of Al2O3 onto platinum wires, using mixtures of ethanol and acetone as the suspending liquid. These EPD coatings were made only on short lengths of wire because the coating is too fragile to allow spooling of the wire. The worst coatings were those made by electrophoretic deposition from aqueous suspensions. Continuous slurry coating of wire was achieved, but due to lack of suitable equipment, the wire had to be cut into short lengths for sintering.
Kreidler, Eric R.↗
Satellite-Respondent Buoys Identify Ocean Debris
NASA operates a series of Earth-observing satellites, which help scientists learn more about our home planet. Through partnerships with universities and other government agencies, like the National Oceanic and Atmospheric Administration (NOAA), the Space Agency helps scientists around the world capture precise movements of the Earth s crust to learn more about the underground processes related to earthquakes and volcanic eruptions, create accurate assessments of wind resources for future energy use, and preserve endangered species by generating much-needed data about their environments. This work, done primarily from space with satellites using a variety of complex instruments to take readings of the surface below, generates leagues of valuable data that aid scientists on the ground - or in some cases on the water. As much of the Earth is covered in water liquid, frozen, saltwater, or fresh much of NASA s remote sensing work focuses on the oceans and their health. This valuable, mammoth (yet fragile) resource provides insight into the overall health of our planet, as water, in addition to being abundant, is a key ingredient to all known life on Earth. As part of its ocean-observing work, NASA partnered with NOAA and private industry to develop remote sensing technologies for protecting the seas of the North Pacific from a nefarious and pervasive problem: derelict fishing gear.
Source record↗
Metal/Metal Oxide Differential Electrode pH Sensors
Solid-state electrochemical sensors for measuring the degrees of acidity or alkalinity (in terms of pH values) of liquid solutions are being developed. These sensors are intended to supplant older electrochemical pH sensors that include glass electrode structures and reference solutions. The older sensors are fragile and subject to drift. The present developmental solid-state sensors are more rugged and are expected to be usable in harsh environments. The present sensors are based on a differential-electrode measurement principle. Each sensor includes two electrodes, made of different materials, in equilibrium with the solution of interest.
West, William↗
The Non-Destructive Separation of Diverse Astrobiologically Relevant Organic Molecules By Customizable Capillary Zone Electrophoresis and Monolithic Capillary Electrochromatography
The in situ detection of organic molecules in space is key to understanding the variety and the distribution of the building blocks of life, and possibly the detection of extraterrestrial life itself. Gas chromatography mass spectrometry (GC-MS) has been the most sensitive analytical instrument for organic analyses in flight, and was used on missions from NASA’s Viking, Phoenix, Curiosity missions to ESA’s Rosetta space probe. While pyrolysis GC-MS revealed the first organics on Mars, this step alters or degrades certain fragile molecules that are excellent biosignatures including polypeptides, oligonucleotides and polysaccharides, rendering the intact precursors undetectable. We have identified a solution tailored to the detection of biopolymers and other biomarkers by the use of liquid-based capillary electrophoresis and electrochromatography. In this study, we show that a capillary electrochromatography (CEC) approach using monolithic stationary phases with tailor-made surface chemistry can separate and identify various polycyclic aromatic hydrocarbons (PAHs), nucleobases and aromatic acids that could be formed under astrophysically relevant conditions. In order to simulate flyby organic sample capture, we conducted hypervelocity impact experiments which consisted of accelerating peptide-soaked montmorillonite particles to a speed of 5.6 km/sec, and capturing them in an amorphous silica aerogel of 10 and 30 mg/cc bulk density. Bulk peptide extraction from aerogel followed by capillary zone electrophoresis led to the detection of only two stereoisomeric peptide peaks. The recovery rates of each step of the extraction procedure after the hypervelocity impact suggest that major peptide loss occurred during the impact. Our study provides initial exploration of feasibility of this approach for capturing intact peptides, and subsequently detecting candidate biomolecules during flight missions that would be missed by GC-MS alone. As the monolith-based electrochromatography technology could be customized to detect specific classes of compounds as well as miniaturized, these results demonstrate the potential of the instrumentation for future astrobiology-related spaceflight missions.
Flyby sample return↗
Ceramic Aerogel Composite Materials and Characterization
Aerogels a.k.a "Solid Smoke" are gels with the liquid phase replaced by gas, leaving behind a highly porous material with a nanoscale framework. Due to the porous, nanoscale structure, aerogels have the lowest known density and conductivity of solids. Aerogels have the potential for being a breakthrough material because of their extremely light weight and unique properties. In this paper, we address overcoming their most profound weaknesses: mechanical fragility and very high surface activity, which leads to a lowered sintering temperature. A matrix of ceramic aerogel composite materials was produced to investigate their properties and functionality. Mechanical property measurements and Scanning Electron Micrographs are used to identify trends and structure of these ceramic composite materials. Thermal cycling was used to identify the sintering points of the materials.
White, Susan↗
Risk Reduction Testing of Superconducting Coils for the High Efficiency Megawatt Motor
Second generation high temperature superconducting coils provide a very attractive level of performance for use in the field winding of electric machines for aircraft. Aside from maintaining these coils at cryogenic temperatures, much care must be taken to prevent damaging these relatively fragile materials due to excessive stress. Thermal stresses due to temperature cycling and mechanical stresses due to centrifugal forces are the most critical for the High Efficiency Megawatt Motor. This paper summarizes two test campaigns that were undertaken to reduce the risks posed by these loads. In one campaign, several superconducting coils were fabricated, thermally cycled up to 50~times, and electrically tested in liquid nitrogen to assess the change in superconductivity metrics throughout thermal cycling. In the other campaign, a full-scale superconducting coil was fabricated, a test article was designed to produce a representative stress environment in the coil, the test article and coil were rotated at room temperature up to a speed of 11,800~rpm, and the superconductivity metrics were measured in liquid nitrogen before and after each rotation. The experimental results demonstrate that the superconducting coils manufactured in house can survive both thermal cycling and high speed rotation with no appreciable degradation in superconducting performance.
partially superconducting electric machine↗
Crystallization of amorphous water ice in the solar system
Electron diffraction studies of vapor-deposited water ice have characterized the dynamical structural changes during crystallization that affect volatile retention in cometary materials. Crystallization is found to occur by nucleation of small domains, while leaving a significant part of the amorphous material in a slightly more relaxed amorphous state that coexists metastably with cubic crystalline ice. The onset of the amorphous relaxation is prior to crystallization and coincides with the glass transition. Above the glass transition temperature, the crystallization kinetics are consistent with the amorphous solid becoming a "strong" viscous liquid. The amorphous component can effectively retain volatiles during crystallization if the volatile concentration is approximately 10% or less. For higher initial impurity concentrations, a significant amount of impurities is released during crystallization, probably because the impurities are trapped on the surfaces of micropores. A model for crystallization over long timescales is described that can be applied to a wide range of impure water ices under typical astrophysical conditions if the fragility factor D, which describes the viscosity behavior, can be estimated.
NASA Center ARC↗
A Survey of Alternative Oxygen Production Technologies
Utilization of the Martian atmosphere for the production of fuel and oxygen has been extensively studied. The baseline fuel production process is a Sabatier reactor, which produces methane and water from carbon dioxide and hydrogen. The oxygen produced from the electrolysis of the water is only half of that needed for methane-based rocket propellant, and additional oxygen is needed for breathing air, fuel cells and other energy sources. Zirconia electrolysis cells for the direct reduction of CO2 arc being developed as an alternative means of producing oxygen, but present many challenges for a large-scale oxygen production system. The very high operating temperatures and fragile nature of the cells coupled with fairly high operating voltages leave room for improvement. This paper will survey alternative oxygen production technologies, present data on operating characteristics, materials of construction, and some preliminary laboratory results on attempts to implement each. Our goal is to significantly improve upon the characteristics of proposed zirconia cells for oxygen production. To achieve that goal we are looking at electrolytic systems that operate at significantly lower temperatures, preferably below 31C to allow the incorporation of liquid CO2 in the electrolyte. Our preliminary results indicate that such a system will have much higher current densities and have simpler cathode construction than a porous gas feed electrode system. Such a system could be achieved based on nonaqueous electrolytes or ionic liquids. We are focusing our research on the anode reaction that will produce oxygen from a product generated at the cathode using CO2 as the feed. Operation at low temperatures also will open up the full range of polymer and metal materials, allowing a more robust system design to withstand the rigors of flight, landing, and long term unattended operation on the surface of Mars.
Lueck, Dale E.↗
Zeolite Formation and Weathering Processes in Dry Valleys of Antartica: Martian Analogs
Terrestrial weathering processes in cold-desert climates such as the Dry Valleys of Antarctica may provide an excellent analog to chemical weathering and diagenesis of soils on Mars. Detailed studies of soil development and the chemical and mineralogical alterations occurring within soil columns in Wright Valley, Antarctica show incredible complexity in the upper meter of soil. Previous workers noted the ice-free Dry Valleys are the best terrestrial approximations to contemporary Mars. Images returned from the Pathfinder and Spirit landers show similarities to surfaces observed within the Dry Valleys. Similarities to Mars that exist in these valleys are: mean temperatures always below freezing (-20 C), no rainfall, sparse snowfall-rapidly removed by sublimation, desiccating winds, diurnal freeze-thaw cycles (even during daylight hours), low humidity, oxidative environment, relatively high solar radiation and low magnetic fields . The Dry Valley soils contain irregular distributions and low abundances of soil microorganisms that are somewhat unusual on Earth. Physical processes-such as sand abrasion-are dominant mechanisms of rock weathering in Antarctica. However, chemical weathering is also an important process even in such extreme climates. For example, ionic migration occurs even in frozen soils along liquid films on individual soil particles. It has also been shown that water with liquid-like properties is present in soils at temperatures on the order of approx.-80 C and it has been observed that the percentage of oxidized iron increases with increasing soil age and enrichments in oxidized iron occurs toward the surface. The presence of evaporates is evident and appear similar to "evaporite sites" within the Pathfinder and Spirit sites. Evaporites indicate ionic migration and chemical activity even in the permanently frozen zone. The presence of evaporates indicates that chemical weathering of rocks and possibly soils has been active. Authogenic zeolites have been identified within the soil columns because they are fragile; i.e. they are euhedral, unabraded, and unfractured, strongly suggesting in situ formation. Their presence in Antarctic samples is another indication that diagenic processes are active in cold-desert environments. The presence of zeolites, and other clays along with halites, sulfates, carbonates, and hydrates are to be expected within the soil columns on Mars at the Gusev and Isidis Planitia regions. The presence of such water-bearing minerals beneath the surface supplies one of the requirements to support biological activity on Mars.
Gibson, E. K., Jr.↗
Protective Skins for Aerogel Monoliths
A method of imparting relatively hard protective outer skins to aerogel monoliths has been developed. Even more than aerogel beads, aerogel monoliths are attractive as thermal-insulation materials, but the commercial utilization of aerogel monoliths in thermal-insulation panels has been inhibited by their fragility and the consequent difficulty of handling them. Therefore, there is a need to afford sufficient protection to aerogel monoliths to facilitate handling, without compromising the attractive bulk properties (low density, high porosity, low thermal conductivity, high surface area, and low permittivity) of aerogel materials. The present method was devised to satisfy this need. The essence of the present method is to coat an aerogel monolith with an outer polymeric skin, by painting or spraying. Apparently, the reason spraying and painting were not attempted until now is that it is well known in the aerogel industry that aerogels collapse in contact with liquids. In the present method, one prevents such collapse through the proper choice of coating liquid and process conditions: In particular, one uses a viscous polymer precursor liquid and (a) carefully controls the amount of liquid applied and/or (b) causes the liquid to become cured to the desired hard polymeric layer rapidly enough that there is not sufficient time for the liquid to percolate into the aerogel bulk. The method has been demonstrated by use of isocyanates, which, upon exposure to atmospheric moisture, become cured to polyurethane/polyurea-type coats. The method has also been demonstrated by use of commercial epoxy resins. The method could also be implemented by use of a variety of other resins, including polyimide precursors (for forming high-temperature-resistant protective skins) or perfluorinated monomers (for forming coats that impart hydrophobicity and some increase in strength).
Leventis, Nicholas↗