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NASA NTRS2024

Microgravity Effects on Nonequilibrium Melt Processing of Neodymium Titanate: Thermophysical Properties, Atomic Structure, Glass Formation and Crystallization

The relationships between materials processing and structure can vary between terrestrial and reduced gravity environments. As one case study, we compare the nonequilibrium melt processing of a rare-earth titanate, nominally 83TiO 2 -17Nd 2 O 3 , and the structure of its glassy and crystalline products. Density and thermal expansion for the liquid, supercooled liquid, and glass are measured over 300–1850 °C using the Electrostatic Levitation Furnace (ELF) in microgravity, and two replicate density measurements were reproducible to within 0.4%. Cooling rates in ELF are 40–110 °C s −1 lower than those in a terrestrial aerodynamic levitator due to the absence of forced convection. X-ray/neutron total scattering and Raman spectroscopy indicate that glasses processed on Earth and in microgravity exhibit similar atomic structures, with only subtle differences that are consistent with compositional variations of ~2 mol. % Nd 2 O 3 . The glass atomic network contains a mixture of corner- and edge-sharing Ti-O polyhedra, and the fraction of edge-sharing arrangements decreases with increasing Nd 2 O 3 content. X-ray tomography and electron microscopy of crystalline products reveal substantial differences in microstructure, grain size, and crystalline phases, which arise from differences in the melt processes.

thermophysical properties↗
NASA NTRS2017

Organic Matter in Extraterrestrial Water-Bearing Salt Crystals

Introduction: Direct samples of early Solar System fluids are present in two thermally-metamorphosed ordinary chondrite regolith breccias (Monahans (1998) [H5] and Zag [H3-6]), which were found to contain brine-bearing halite (NaCl) crystals that have been added to the regolith of an S-type asteroid following asteroidal metamorphism [1, 2]. The brine-bearing halite grains were proposed to be formed on an icy C-type asteroids (possibly Ceres), and transferred to an S-type asteroid via cryovolcanic event(s) [3]. A unique aspect of these halites is that they contain abundant organic rich solid inclusions hosted within the halites alongside the water inclusions. Methods: We analyzed in detail the compositions of the organic solids and the amino acid content of the halite crystals with two-step laser desorption/laser ionization mass spectrometry (L(sup 2) MS), Raman spectroscopy, X-ray absorption near edge structure (XANES), nanoscale secondary ion mass spectrometry (NanoSIMS), and ultra-performance liquid chromatography fluorescence detection and quadrupole time of flight hybrid mass spectrometry (UPLC-FD/QToF-MS). Results and Discussion: The L(sup 2) MS results show signatures of low-mass polyaromatic hydro-carbons (PAHs) indicated by sequences of peaks separated by 14 atomic mass units (amu) due to successive addition of methylene (CH2) groups to the PAH skeletons [4]. Raman spectra of the micron-sized solid inclusions of the halites indicate the presence of abundant and highly variable organic matter that include a mixture of short-chain aliphatic compounds and macromolecular carbon. C-XANES analysis identified C-rich areas with peaks at 285.0 eV (aromatic C=C) and 286.6 eV (vinyl-keto C=O). However, there is no 1s-sigma* exciton peak (291.7 eV) that is indicative of the development of graphene structure [5], which suggests the organics were synthesized cold. Na-noSIMS analyses show C-rich and N-rich areas that exhibit similar isotopic values with that of the IOM in the unweathered CR chondrites and less metamorphosed meteorites [6], and are moderately enriched in N-15 (delta N-15 = 106.1-164.5 per mille). The total amino acid distribution and abundance of the Zag matrix (approximately 1,940 parts per billion [ppb]) is comparable to other ordinary chondrites (60-3,330 ppb) [7, 8]. While the Zag matrix is gamma-ABA and EACA-deficient, the halite is shown to exhibit an opposite trend and is almost depleted in amino acids. The striking difference in the amino acid contents between the halite and matrix indicates their separate synthetic origins. Conclusion: Abundant, primitive, and highly-diverse N-15-rich organic compounds were detected in brine-water bearing halite crystals that were synthesized on a cryovolcanically-active asteroid. Our study suggests that the asteroidal parent body where the halite precipitated, potentially Ceres, is a host to abundance large variety organic precursors. Insoluble organic matter and amino acids can be synthesized from similar organic precusors under hydrous conditions [9].We envision that similar organic synthetic processes could have occurred on Ceres that synthesized organic solids as well as biologically relevant molecules.

Chan, Q. H. S.↗
NASA NTRS1983

Rapid solidification of highly undercooled alloy droplets

Experimental work is described on undercooling and structure of tin-lead droplets emulsified in oil. The droplets, predominantly in the size range of 10-20 microns, were cooled at rates ranging from about 0.04 K/sec to 1,000,000 K/sec. The higher cooling rates were obtained by a newly developed technique of quenching the emulsified droplets in a cold liquid. Measured undercoolings (at the lower cooling rates) ranged up to about 100 C. Structures obtained depended strongly on undercooling, cooling rate before nucleation, droplet size, alloy composition and the rate of heat extraction after nucleation.

Chu, M. G.↗
NASA NTRS1961

Semi-Annual Report: October 15, 1961

Investigations are proposed involving an experimental and theoretical program designed to investigate various properties of the structure of helium both in its atomic form and in the aggregates of the liquid and solid states. The key to the possibilities of performing the experiments lies in the relatively weak electric fields existing in liquid and solid helium and the possibility of producing external fields almost comparable with the internal fields. It is proposed to examine a) the melting pressure curve for helium as a function of electric field b) the dielectric constant of helium as a function of pressure and electric field c) in future, the effect of electric fields on the lambda transition. From the results of these experiments one would expect to be able to gather at least corroborative evidence on a) the crystal structure of solid helium on b) the effect of the Van der Waal interaction of the electric polarizability of helium, c) the possibility of producing helium molecules d) the effective volume available to helium atoms in the liquid and possibly e) the effect of particle interactions on the Bose-Einstein condensation.

HELIUM↗
NASA NTRS1983

Radiant heating tests of several liquid metal heat-pipe sandwich panels

Integral heat pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich construction, were conceived as a means of alleviating thermal stress problems in the Langley Scramjet Engine. Test panels which utilized two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and a liquid metal working fluid (either sodium or potassium) were tested by radiant heating at various heat load levels. The heat pipe panels reduced maximum temperature differences by 31 percent with sodium working fluid and 45 percent with potassium working fluid. Results indicate that a heat pipe sandwich panel is a potential, simple solution to the engine thermal stress problem. Other interesting applications of the concept include: cold plates for electronic component and circuit card cooling, radiators for large space platforms, low distortion large area structures (e.g., space antennas) and laser mirrors.

Camarda, C. J.↗
NASA NTRS1974

Method of repairing discontinuity in fiberglass structures

Damaged fiberglass structures are repaired by substantially filling the irregular surfaced damaged area with a liquid, self-curing resin, preferably an epoxy resin mixed with chopped fiberglass, and then applying to the resin surface the first of several woven fiberglass swatches which has stitching in a zig-zag pattern parallel to each of its edges and a fringe of warp and fill glass fibers about the edges outward of the stitching. The method is especially applicable to repair of fiberglass rocket engine casings and is particularly advantageous since it restores the repaired fiberglass structure to substantially its original strength without any significant changes in the geometry or mass of the structure.

Gelb, L. L.↗
NASA NTRS1988

Materials and structures for hypersonic vehicles

Hypersonic vehicles are envisioned to require, in addition to carbon-carbon and ceramic-matrix composities for leading edges heated to above 2000 F, such 600 to 1800 F operating temperature materials as advanced Ti alloys, nickel aluminides, and metal-matrix composited; These possess the necessary low density and high strength and stiffness. The primary design drivers are maximum vehicle heating rate, total heat load, flight envelope, propulsion system type, mission life requirements and liquid hydrogen containment systems. Attention is presently given to aspects of these materials and structures requiring more intensive development.

Tenney, Darrel R.↗
NASA NTRS1984

Solidification of highly undercooled Sn-Pb alloy droplets

Experimental work on undercooling and structure of tin-lead droplets emulsified in oil is described. The droplets, predominantly in the size range of 10 to 20 microns, were cooled at rates (just before nucleation) ranging from about 0.1 to 1 million K/s. The higher cooling rates were obtained by a newly developed technique of quenching the emulsified droplets in a cold liquid. Measured undercoolings (at the lower cooling rates) ranged up to about 100 K. Structures obtained depend strongly on undercooling, cooling rate before and after nucleation, and alloy composition. Droplets containing up to 5 wt pct Pb were apparently single phase when undercooled and rapidly quenched. Droplets in the composition range of about 25-90 wt pct Pb solidified dendritically, even at the most rapid quench rates employed, apparently because these alloys undercooled only slightly before nucleation of the primary phase.

Chu, M. G.↗
NASA NTRS2021

Demonstration of Multilayer Insulation, Vapor Cooling of Structure, and Mass Gauging for Large Scale Upper Stages: Structural Heat Intercept, Insulation, and Vibration Evaluation Rig (SHIIVER) Final Report

Testing was completed on the Structural Heat Intercept, Insulation, and Vibration Evaluation Rig (SHIIVER) between August 2019 and January 2020. SHIIVER was designed to be a test bed for the scaling of cryogenic fluid management technologies as applied to large upper stages and long duration in-space stages. The hardware consists of a 4 meter diameter stainless steel tank, structural skirts supporting the tank in the aft direction, and an aluminum forward skirt with vapor cooling channels bolted to it. The initial testing of the SHIIVER hardware was with liquid hydrogen and liquid nitrogen (as a substitute fluid for liquid oxygen and liquid methane) and sought to demonstrate the use of boil-off vapor to intercept heat on a structural skirt, multilayer insulation (MLI) on the tank domes, and the radio frequency mass gauge (RFMG). Testing was completed in four stages: a baseline thermal vacuum test prior to installation of the MLI, a thermal vacuum test after the MLI installation, a reverberant acoustic test, and a subsequent thermal vacuum test to verify that no damage occurred during the reverberant acoustic testing. Each thermal vacuum test with chamber wall at ambient temperature and vacuum level in the 10-6 torr range was conducted continuously between approximately 90% full and 25% full. Test results showed that the vapor cooling reduced the heat load to the tank by approximately 10%, but the boil-off by less than 3% at 50% full with no MLI on the domes. It reduced the heat load to the tank by approximately 10%, but the boil-off was essentially unchanged at 50% full whether or not vapor cooling was operational with MLI on the domes. The MLI reduced the heat load to the tank by approximately 40% at all fill levels, but the boil-off by approximately 25% at 90% full and 45% below 65% full. The RFMG performed well over all fill ranges, and several RF tank modes were used to gauge the mass of fluid in the tank. SHIIVER was then exposed to an acoustic environment of 147 dB OASPL (overall sound pressure level) in a reverberant chamber. The acoustic environment and profile envelopes the upper stage internal acoustic level of several different modern launch vehicles. No structural or thermal performance changes were observed as a result of acoustic testing. Final thermal vacuum testing after the acoustic testing showed no degradation to the MLI due to the acoustic environment as measured via system heat loads.

SHIIVER↗
NASA NTRSDate not supplied

Three-Dimensional In Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions, which shed new light on the selection of dendritic array structures, and on roles of macroscopic curvatures and subgrain boundaries between grains with a small misorientation with respect to the temperature gradient in the spatiotemporal evolution of the primary cellular spacing.

Kaihua Ji↗
NASA NTRS1993

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗
NASA NTRS1998

Low Cost Large Core Vehicle Structures Assessment

Boeing Information, Space, and Defense Systems executed a Low Cost Large Core Vehicle Structures Assessment (LCLCVSA) under contract to NASA Marshall Space Flight Center (MSFC) between November 1997 and March 1998. NASA is interested in a low-cost launch vehicle, code named Magnum, to place heavy payloads into low earth orbit for missions such as a manned mission to Mars, a Next Generation Space Telescope, a lunar-based telescope, the Air Force's proposed space based laser, and large commercial satellites. In this study, structural concepts with the potential to reduce fabrication costs were evaluated in application to the Magnum Launch Vehicle (MLV) and the Liquid Fly Back Booster (LFBB) shuttle upgrade program. Seventeen concepts were qualitatively evaluated to select four concepts for more in-depth study. The four structural concepts selected were: an aluminum-lithium monocoque structure, an aluminum-lithium machined isogrid structure, a unitized composite sandwich structure, and a unitized composite grid structure. These were compared against a baseline concept based on the Space Shuttle External Tank (ET) construction. It was found that unitized composite structures offer significant cost and weight benefits to MLV structures. The limited study of application to LFBB structures indicated lower, but still significant benefits. Technology and facilities development roadmaps to prepare the approaches studied for application to MLV and LFBB were constructed. It was found that the cost and schedule to develop these approaches were in line with both MLV and LFBB development schedules. Current Government and Boeing programs which address elements of the development of the technologies identified are underway. It is recommended that NASA devote resources in a timely fashion to address the specific elements related to MLV and LFBB structures.

Hahn, Steven E.↗
NASA NTRS1990

Cloud and boundary layer structure over San Nicolas Island during FIRE

The temporal evolution of the structure of the marine boundary layer and of the associated low-level clouds observed in the vicinity of the San Nicolas Island (SNI) is defined from data collected during the First ISCCP Regional Experiment (FIRE) Marine Stratocumulus Intense Field Observations (IFO) (July 1 to 19). Surface, radiosonde, and remote-sensing measurements are used for this analysis. Sounding from the Island and from the ship Point Sur, which was located approximately 100 km northwest of SNI, are used to define variations in the thermodynamic structure of the lower-troposphere on time scales of 12 hours and longer. Time-height sections of potential temperature and equivalent potential temperature clearly define large-scale variations in the height and the strength of the inversion and periods where the conditions for cloud-top entrainment instability (CTEI) are met. Well defined variations in the height and the strength of the inversion were associated with a Cataline Eddy that was present at various times during the experiment and with the passage of the remnants of a tropical cyclone on July 18. The large-scale variations in the mean thermodynamic structure at SNI correlate well with those observed from the Point Sur. Cloud characteristics are defined for 19 days of the experiment using data from a microwave radiometer, a cloud ceilometer, a sodar, and longwave and shortwave radiometers. The depth of the cloud layer is estimated by defining inversion heights from the sodar reflectivity and cloud-base heights from a laser ceilometer. The integrated liquid water obtained from NOAA's microwave radiometer is compared with the adiabatic liquid water content that is calculated by lifting a parcel adiabatically from cloud base. In addition, the cloud structure is characterized by the variability in cloud-base height and in the integrated liquid water.

Albrecht, Bruce A.↗
NASA NTRS2014

Computational and Experimental Investigation of Li-doped Ionic Liquid Electrolytes: [pyr14][tfsi], [pyr13][fsi], and [EMIM][BF4]

We employ molecular dynamics (MD) simulation and experiment to investigate the structure, thermodynamics, and transport of N-methyl-N-butylpyrrolidinium bis(trifluoromethylsufonyl)imide ([pyr14][TFSI]), N -methyl-N-propylpyrrolidinium bis(fluorosufonyl)imide ([pyr13][FSI]), and 1-ethyl-3-methylimidazolium boron tetrafluoride ([EMIM][BF4]), as a function of Li-salt mole fraction (0.05 xLi+ 0.33) and temperature (298 K T 393 K). Structurally, Li+ is shown to be solvated by three anion neigh- bors in [pyr14][TFSI] and four anion neighbors in both [pyr13][FSI] and [EMIM][BF4], and at all levels of xLi+ we find the presence of lithium aggregates. Pulsed field gradient spin-echo NMR measurements of diffusion and electrochemical impedance spectroscopy measurements of ionic conductivity are made for the neat ionic liquids as well as 0.5 molal solutions of Li-salt in the ionic liquids. Bulk ionic liquid properties (density, diffusion, viscosity, and ionic conductivity) are obtained with MD and show excellent agreement with experiment. While the diffusion exhibits a systematic decrease with increasing xLi+, the contribution of Li+ to ionic conductivity increases until reach- ing a saturation doping level of xLi+ 0.10. Comparatively, the Li+ conductivity of [pyr14][TFSI] is an order of magnitude lower than that of the other liquids, which range between 0.1-0.3 mScm. Our transport results also demonstrate the necessity of long MD simulation runs ( 200 ns) required to converge transport properties at room T. The differences in Li+ transport are reflected in the residence times of Li+ with the anions (Li), which are revealed to be much larger for [pyr14][TFSI] (up to 100 ns at the highest doping levels) than in either [EMIM][BF4] or [pyr13][FSI]. Finally, to comment on the relative kinetics of Li+ transport in each liquid, we find that while the net motion of Li+ with its solvation shell (vehicular) significantly contributes to net diffusion in all liquids, the importance of transport through anion exchange (hopping) increases at high xLi+ and in liquids with large anions.

electrolytes↗
NASA NTRS1983

Radiant heating tests of several liquid metal heat-pipe sandwich panels

Integral heat-pipe sandwich panels, which synergistically combine the thermal efficiency of heat pipes and the structural efficiency of honeycomb sandwich construction, were conceived as a means of alleviating thermal stress problems in the Langley Scramjet Engine. Test panels which utilized two different wickable honeycomb cores, facesheets with screen mesh sintered to the internal surfaces, and a liquid metal working fluid (either sodium or potassium) were tested by radiant heating at various heat-load levels. The heat-pipe panels reduced maximum temperature differences by 31 percent with sodium working fluid and 45 percent with potassium working fluid. Results indicate that a heat-pipe sandwich panel is a potential, simple solution to the engine thermal stress problem. Other interesting applications of the concept include: cold plates for electronic component and circuit card cooling, radiators for large space platforms, low-distortion large area structures (e.g., space antennas) and laser mirrors.

Camarda, C. J.↗
NASA NTRSDate not supplied

Three-dimensional in Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions in polycrystalline samples containing several grains with a small misorientation with respect to the temperature gradient. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions that shed new light on the role of subgrain boundaries in the spatiotemporal evolution of the primary cellular spacing and the selection of dendritic array structures.

Kaihua Ji↗
NASA NTRS1984

Observing atmospheric water in storms with the Nimbus 7 scanning multichannel microwave radiometer

Employing data on integrated atmospheric water vapor, total cloud liquid water and rain rate obtainable from the Nimbus 7 Scanning Multichannel Microwave Radiometer (SMMR), we study the frontal structure of several mid-latitude cyclones over the North Pacific Ocean as they approach the West Coast of North America in the winter of 1979. The fronts, analyzed with all available independent data, are consistently located at the leading edge of the strongest gradient in integrated water vapor. The cloud liquid water content, which unfortunately has received very little in situ verification, has patterns which are consistent with the structure seen in visible and infrared imagery. The rain distribution is also a good indicator of frontal location and rain amounts are generally within a factor of two of what is observed with rain gauges on the coast. Furthermore, the onset of rain on the coast can often be accurately forecast by simple advection of the SMMR observed rain areas.

Katsaros, K. B.↗
NASA NTRS2002

Physics of Colloids in Space: Flight Hardware Operations on ISS

The Physics of Colloids in Space (PCS) experiment was launched on Space Shuttle STS-100 in April 2001 and integrated into EXpedite the PRocess of Experiments to Space Station Rack 2 on the International Space Station (ISS). This microgravity fluid physics investigation is being conducted in the ISS U.S. Lab 'Destiny' Module over a period of approximately thirteen months during the ISS assembly period from flight 6A through flight 9A. PCS is gathering data on the basic physical properties of simple colloidal suspensions by studying the structures that form. A colloid is a micron or submicron particle, be it solid, liquid, or gas. A colloidal suspension consists of these fine particles suspended in another medium. Common colloidal suspensions include paints, milk, salad dressings, cosmetics, and aerosols. Though these products are routinely produced and used, we still have much to learn about their behavior as well as the underlying properties of colloids in general. The long-term goal of the PCS investigation is to learn how to steer the growth of colloidal structures to create new materials. This experiment is the first part of a two-stage investigation conceived by Professor David Weitz of Harvard University (the Principal Investigator) along with Professor Peter Pusey of the University of Edinburgh (the Co-Investigator). This paper describes the flight hardware, experiment operations, and initial science findings of the first fluid physics payload to be conducted on ISS: The Physics of Colloids in Space.

Doherty, Michael P.↗