Development of Ionic Liquid Based Epoxies for Carbon Fiber Composite Cryogenic Tanks
No abstract available
Grugel, R. N.↗
Engineering topics
Kaukler, W. F.
Publications and source records attributed to Kaukler, W. F..
Task-Specific Ionic Liquids for Mars Exploration (Green Chemistry for a Red Planet)
Ionic Liquids (ILs) are organic salts with low melting points that are liquid at or near room temperature. The combinations of available ions and task-specific molecular designability make them suitable for a huge variety of tasks. Because of their low flammability, low vapor pressure, and stability in harsh environments (extreme temperatures, hard vacuum) they are generally much safer and "greener" than conventional chemicals and are thus suitable for a wide range of applications that support NASA exploration goals. This presentation describes several of the ongoing applications that are being developed at MSFC.
Karr, L. J.↗
Solid-Liquid Interface Characterization Hardware: Advanced Technology Development (ATD)
This ATD has the goal of enabling the integration of three separate measurement techniques to characterize the solid-liquid interface of directionally solidified materials in real-time. Arrays of film-based metal thermocouple elements are under development along with compact Seebeck furnaces suitable for interfacing with separately developed X-ray Transmission Microscopes. Results of applying film arrays to furnace profiling are shown, demonstrating their ability to identify a previously undetected hardware flaw in the development of a second-generation compact furnace. Results of real-time furnace profiling also confirmed that the compact furnace design effectively isolates the temperature profiles in two halves of the furnace, a necessary feature. This isolation had only been inferred previously from the characteristics of Seebeck data reported. Results from a 24-thermocouple array successfully monitoring heating and isothermal cooling of a tin sample are shown. The importance of non-intrusion by the arrays, as well as furnace design, on the profiling of temperature gradients is illustrated with example measurements. Further developments underway for effectively combining all three measurements are assessed in terms of improved x-ray transmission, increased magnification, integral arrays with minimum intrusion, integral scales for velocity measurements and other features being incorporated into the third generation Seebeck furnace under construction.
Peters, Palmer N.↗
A Real Time Investigation of Morphological Evolution During Solidification of Different Alloy Systems
Solidification phenomenon which occur at the solid/liquid (s/I) interface play a major role in the determination of structure and hence the technologically important properties of a casting. However, metals being opaque, conclusions related to several important phenomenon such as boundary layer thickness, morphological evolution, and eutectic and cell spacing are deduced from quenching experiments and subsequent post solidification metallographic analysis. Consequently, limited information is obtained about the dynamics of the process. This paper will discuss the recent efforts at the Space Science Laboratory, NASA Marshall Space Flight Center, to view and quantify in-situ and in real time the dynamics of the solidification process and to measure interfacial undercooling. First, a high resolution x-ray transmission microscope (XTM) has been developed to monitor fundamental interfacial phenomena during directional solidification of metals and alloys. The XTM operates in the range of 10-100 KeV and through projection is capable of achieving magnification of up to 16OX. Secondly, an innovative collapsible furnace has been designed to quantify interfacial undercooling by measuring the temperature of a moving s/I interface in reference to a fixed s/l interface. This measurement technique is non-intrusive in nature and is based on the Seebeck principle. In this paper real time results obtained to characterize the dynamics of irregular eutectic spacing will be presented. As an example fiber to lamella or plate transition in the Al-Al2Au eutectic system will be discussed. Further, a resolution limit of 25 micron has permitted viewing in real time morphological instability and cellular growth in Al-Au and Al-Ag systems. Simultaneously, a systematic investigation has been carried out to measure interfacial undercooling for Pb-1 wt.% Sn at and near the marginal stability regime. In conjunction with the XTM observations this study attempts to validate existing relationships between undercooling and growth velocity during plane front growth, marginal stability regime, and stable cellular growth.
Sen, S.↗
Numerical Modeling and In-Situ Observations of the Dynamics of the Solid/Liquid Interface Morphology During Directional Solidification of Alloys
The departure from interface planarity and the subsequent evolution to a periodic array of cells or dendrites is a fundamental process that characterizes most microstructures in solidified alloys. The growing demand for high quality alloys and semiconductor crystals requires a precise methodology to predict and subsequently control both the interface morphology and the distribution of impurities, additives, and phases in the grown crystal. Apart from its practical significance, the study of morphological evolution has also been viewed as a means to unearth a general paradigm for pattern formation in nature. A previously developed 2D numerical model for the solid/liquid interface tracking has been further refined and used to simulate the time-evolution of the perturbations on the interface. The dynamics of the local growth velocity, interface undercooling and solute concentration at the interface has been theoretically predicted by means of the numerical model for Al-Cu and Pb-Sn alloys. The model shows that perturbations with a wavelengths, lambda greater than a critical wavelength lambda(sub c) continue to grow in time whereas perturbations with lambda < lambda(sub c) cease to propagate. The model further predicts that under certain conditions perturbation can also propagate along the interface. Comparison of these predictions with existing theories of pattern formation and experimental results will be discussed.
Catalina, Adrian V.↗
Measurement of Interfacial Undercooling in a Dilute Pb-Sn Alloy Near the Regime of Morphological Instability
The solid/liquid (s/1) interfacial Seebeck technique was used to measure interfacial undercooling in a Pb-1 wt.% Sn alloy. For plane front solidification an undercooling in the range of 0.54-0.57C was recorded. However, for growth velocities between 6 to 15 micron/s the undercooling, increased with increase in velocity. 'Tbis is in contradiction to the theoretical predictions based on growth at the extremum condition. A modified analytical expression was developed based on the maro,,inal stability criterion to predict undercooling for growth velocities immediately over the limit of morphological stability. Between 6 to 15 microns/s the trend predicted by this modified expression is in qualitative agreement with the experimental results. This model is more consistent with the analysis of Venugopal and Kirkaldy which states that the extremum condition criterion is not applicable in the marginal stability regime. At higher growth velocities between 20 and 50 microns/s where stable cellular growth is expected the undercooling, decreased with increase in velocity. The predictions of Burden and Hunt based on extremum criterion agree reasonably well with the experimental results in this velocity range. Finally, the importance of non-equilibrium phase diagram parameters such as partition coefficient and liquidus slope were also evaluated using the experimental undercooling results obtained in this investigation.
Sen, S.↗
Optimization of the Processing Parameters of High Temperature Superconducting Glass-Ceramics: Center Director's Discretionary Fund Final Report
A number of promising glass forming compositions of high Tc superconducting Ba-Sr-Ca-Cu-O (BSCCO) materials were evaluated for their glass-ceramic crystallization ability. The BSCCO ceramics belonging to the class of superconductors in the Ba-Sr-Ca-Cu-O system were the focus of this study. By first forming the superconducting material as a glass, subsequent devitrification into the crystalline (glass-ceramic) superconductor can be performed by thermal processing of the glass preform body. Glass formability and phase formation were determined by a variety of methods in another related study. This study focused on the nucleation and crystallization of the materials. Thermal analysis during rapid cooling aids in the evaluation of nucleation and crystallization behavior. Melt viscosity is used to predict glass formation ability.
Ethridge, E. C.↗
Laser welding in space
Autogenous welds in 304 stainless steel were performed by Nd-YAG laser heating in a simulated space environment. Simulation consists of welding on the NASA KC-135 aircraft to produce the microgravity and by containing the specimen in a vacuum chamber. Experimental results show that the microgravity welds are stronger, harder in the fusion zone, have deeper penetration and have a rougher surface rippling of the weld pool than one-g welds. To perform laser welding in space, a solar-pumped laser concept that significantly increases the laser conversion efficiency and makes welding viable despite the limited power availability of spacecraft is proposed.
Kaukler, W. F.↗
Cellular solidification in a monotectic system
Succinonitrile-glycerol, SN-G, transparent organic monotectic alloy is studied with particular attention to cellular growth. The phase diagram is determined, near the monotectic composition, with greater accuracy than previous studies. A solidification interface stability diagram is determined for planar growth. The planar-to-cellular transition is compared to predictions from the Burton, Primm, Schlichter theory. A new technique to determine the solute segregation by Fourier transform infrared spectroscopy is developed. Proposed models that involve the cellular interface for alignment of monotectic second-phase spheres or rods are compared with observations.
Kaukler, W. F.↗
Electrical properties of Al-In-Sn alloys directionally solidified in high and low gravitational fields
The Al-In-Sn alloys were directionally solidified in the NASA KC-135 aircraft which flies a series of parabolas to generate high (high-g) and low (low-g) gravity forces parallel to the longitudinal growth axis. Thus, for a given sample, successive sections can be identified which were solidified in high-g and low-g. Measurements of the electronic properties of the samples reveal that: the resistivity of the low-g sections is larger (about a factor of 10) than that of the high-g sections; the low-g sections behave conductively like a semi-metal, while the high-g sections are essentially metallic; and both high-g and low-g sections are superconducting but the superconducting transition temperature of the low-g sections is 1 K higher than that of the high-g sections.
Wu, M. K.↗
The effects of gravity level during directional solidification on the microstructure of hypermonotectic Al-In-Sn alloys
Five hypermonotectic Al-In-Sn compositions were directionally solidified in a Bridgman-type furnace at normal gravity and during aircraft low-gravity maneuvers. The tendency of the Al-30In alloy to form an indium-rich band at the start of unidirectional growth (SUG) made it difficult to study the integration of L sub 2 into the solidification interface. Hypermonotectic compositions closer to monotectic slightly hypermonotectic caused only a partial band on L sub 2 to form at SUG and allowed the study of such variables as gravity, composition, and monotectic dome height on integration of excess L sub 2 into the solid plus L sub 2 interface. It was found that formation of aligned composite structures for the Al-In-Sn system is not only a function of G and R but also of the degree to which the composition varies from monotectic. Most of the aligned fibrous structures formed from hypermonotectic Al-In-Sn had spacings that were of the order of irregular fibrous structures reported for on monotectic Al-In-Sn. The spacings for the large fibers and aligned globules found for ground and low-gravity processed Al-In-18-Sn-22, respectively, were significantly larger than the others measured and were of the order expected for cell spacings under the growth conditions utilized. It was found that the integration into the solidification front of excess L sub 2 in low gravity was a function of the Sn composition of the alloy.
Curreri, P. A.↗
Electrical properties of Al-In-Sn alloys directionally solidified in high and low gravitational fields
The Al-In-Sn alloys were directionally solidified in the NASA KC-135 aircraft which flies a series of parabolas to generate high (high-g) and low (low-g) gravity forces parallel to the longitudinal growth axis. Thus, for a given sample, successive sections can be identified which were solidified in high-g and low-g. Measurements of the electronic properties of the samples reveal that: the resistivity of the low-g sections is larger (about a factor of 10) than that of the high-g sections; the low-g sections behave conductively like a semi-metal, while the high-g sections are essentially metallic; and both high-g and low-g sections are superconducting but the superconducting transition temperature of the low-g sections is 1 K higher than that of the high-g sections.
Curreri, P. A.↗
Crystallization microstructure in transparent monotectic alloys
The surprising funguslike morphology which occurs at the liquid(1)/liquid(2)/solid triple junction in directionally solidifying miscibility gap systems at the monotectic temperature is described. The monotectic temperature in a binary mixture is the one at which two immiscible solutions of the same two components form phases in equilibrium with the solid phase of one of the components. The growth of this morphology is described, and a similarity between it and that of a known crystal growth morphology is pointed out.
Kaukler, W. F.↗
Separation in Binary Alloys
Studies of monotectic alloys and alloy analogs reviewed. Report surveys research on liquid/liquid and solid/liquid separation in binary monotectic alloys. Emphasizes separation processes in low gravity, such as in outer space or in free fall in drop towers. Advances in methods of controlling separation in experiments highlighted.
Frazier, D. O.↗
Surface film effects on drop tube undercooling studies
The effects of various gaseous atmospheric constituents on drop-tube solidified samples of elemental metals were examined from a microstructural standpoint. All specimens were prepared from the purest available elements, so effects of impurities should not account for the observed effects. The drop-tube gas has a definite effect on the sample microstructure. Most dramatically, the sample cooling rate is effected. Some samples receive sufficient cooling to solidify in free fall while others do not, splating at the end of the drop tube in the sample catcher. Gases are selectively absorbed into the sample. Upon solidification gas can become less soluble and as a result forms voids within the sample. The general oxidation/reduction characteristics of the gas also affect sample microstructures. In general, under the more favorable experimental conditions including reducing atmospheric conditions and superheatings, examination of sample microstructures indicates that nucleation has been suppressed. This is indicated by underlying uniform dendrite spacings throughout the sample and with a single dendrite orientation through most of the sample. The samples were annealed yielding a few large grains and single or bi-crystal samples were commonly formed. This was especially true of samples that were inadvertently greatly superheated. This is in contrast with results from a previous study in which surface oxides were stable and contained numerous sites of nucleation. The number of nucleation events depends upon the surface state of the specimen as determined by the atmosphere and is consistent with theoretical expectations based upon the thermodynamic stability of surface oxide films. Oxide-free specimens are characterized by shiny surfaces, with no observable features under the scanning electron microscope at 5000X.
Ethridge, E. C.↗
Variable-Temperature-Gradient Device for Solidification Research
Device for research in solidification and crystal growth allows crystallization of melt observed as occurs. Temperature gradient across melt specimen increased or decreased rapidly while solidification front proceeds at constant speed across sample. Device moves sample at same speed, thereby holding position of liquid/solid interface stationary within field of optical microscope. Device, variabletemperature-gradient microscope stage, used to study crystal growth at constant rate while thermal driving force is varied.
Kaukler, W. F.↗
Reversing Glass Wettability
Treatment reverses wettability of glassware: Liquids that normally wet glass no longer do, and those that do not wet glass are made to do so. Useful in research on container effects in nucleation and growth of secondary phase from solution. Treatment consists of spreading 3 percent (by weight) solution of silicone oil in hexane isomers over glass, drying in air, and curing at 300 degrees C in vacuum for one hour.
Frazier, D. O.↗
Studies of Model Immiscible Systems
The objectives are to use model transparent monotectics to obtain fundamental information applicable to two-phase systems in general, to apply this understanding to materials of interest in the Microgravity Science and Applications program, and to interpret results of flight experimental involving monotectic alloys. A number of model immiscible systems are in use to study various aspects of two-phase behavior within the miscibility gap and during solidification. Particle growth, coalescence and particle motions are under investigation using a holographic microscopy system. The system is capable of working with particle densities up to 10 to the 7th power particles/cubic centimeters through a 100 micron depth and can resolve particles of the order of 2 to 3 micron in diameter throughout the entire cell volume. Particle size, distribution changes with respect to time and temperature are observable from sequential holograms. Initial experiments using diethylene glycol/ethyl salicylate (DEG/ES) have demonstrated the usefulness of the technique. The thermal system controls temperature to at least plus or minus 0.001 K over the course of an experiment. A time-lapse film, made from holograms, of a succinonitrile/water solution shows particle size and number distribution changes with time under isothermal conditions. The observations are consistent with Ostwald ripening theory.
Frazier, D. O.↗