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High gradient allows rapid growth rates in directionally-solidified eutectic alloys. Furnace design permits cost reductions in directional solidification process through its increased solidification rates, which reduces melt/mold interaction. It produces structural engineering materials for any application requiring properties directionally-solidified eutectic materials.
Unexpected results from SPAR experiments, directed at obtaining fine dispersions of metal systems that in a 1-g environment tend to segregate very rapidly, were considered. The physical processes occurring in fluid samples, such as the SPAR samples before solidification, were shown to be insufficient to produce a well mixed liquid by the time solidification was initiated. This would result in solidified samples with the type of segregation noted in the SPAR samples. Experimental evidence and analytical arguments are presented.
Experiment objectives, design/operational concepts, and final results are summarized for six materials science experiments conducted during the second space processing applications rocket mission flown by NASA. The individual experiments discussed are: (1) solidification of Pb-Sb eutectic; (2) feasibility of producing closed-cell metal foams; (3) direct observation of dendrite remelting and macrosegregation in castings; (4) agglomeration in immiscible liquids; (5) casting dispersion - strengthened composites at zero gravity; and (6) solidification behavior of Al-In alloys under zero gravity conditions.
The interaction between second-phase particles and crystal-liquid interfaces in the solidification process has been studied in ground-based experiments and experiments under microgravity conditions. An analysis of these data with a view toward the solidification processing of composite materials reveals a pronounced difference between high entropy of fusion and low entropy of fusion matrix materials, as well as a pronounced effect of differences in the thermal conductivity of particles and liquid on the behavior of materials. Effects of liquid viscosity surface topography of the particles, particle chemistry, and overall particle shape examined.
The welding of the nickel base, heat resistant alloys that are used extensively for welded Shuttle engine components revealed solidification cracking characteristics at weld termination points. If not detected and removed, these crater cracks may cause costly component failure. To better understand this characteristic, welding termination techniques were studied and methods developed to eliminate crater cracks. It was determined that weld termination solidification cracking can be eliminated by controlled decrease of welding current, welding voltage, wire feed, and travel speed.
The metallurgical processing experiments on Skylab were chosen to: (1) elucidate the unknown effects of a low gravity environment on certain processes; (2) determine to what extent nongravitational driven flows operate in the processes; and (3) explore the possibilities of containerless solidification. Welding and brazing experiments were conducted to provide an understanding of solidification mechanics in a weightless environment.
The Apollo Soyuz Test Program is described. A modification of the Skylab furnace was developed for the ASTP mission that had a maximum temperature of 1200 C, a programmed cool down to give more uniform growth rates, and a He quench system to shorten the time required to reach allowable touch temperature. The Space Processing Applications Rocket (SPAR) program was initiated to provide some continuity in flight experimentation. Liquid mixing, immiscible alloy solidification, composite materials, bubbles and dispersed particles during solidification, and containerless processing techniques were studied in the SPAR program.
Thermal models detailing the solidification paths for shallow basaltic magma chambers (both open and closed systems) were calculated using finite-difference techniques. The total solidification time for closed chambers are comparable to previously published calculations; however, the temperature-time paths are not. These paths are dependent on the phase relations and the crystallinity of the system, because both affect the manner in which the latent heat of crystallization is distributed. In open systems, where a chamber would be periodically replenished with additional parental liquid, calculations indicate that the possibility is strong that a steady-state temperature interval is achieved near a major phase boundary. In these cases it is straightforward to analyze fractionation models of the basaltic liquid evolution and their corresponding cumulate sequences. This steady thermal fractionating state can be invoked to explain large amounts of erupted basalts of similar composition over long time periods from the same volcanic center and some rhythmically layered basic cumulate sequences.
A susceptibility apparatus to measure superconducting properties of samples made in the MSFC Drop Tube was used to measure the transition temperature (Tc) and susceptibilities of Nb and Nb Ge Alloys prepared in bulk spherical (2-4 mm diameter) form using a 32 m drop tube in which containerless low gravity solidification could take place. Results indicate that a drop tube processing environment was beneficial for increasing the Tc of the superconducting phase of the material over that of arc melted material. The increase in Tc is found to be related to the amount of solidification of the total sample that took place before reaching the bottom of the drop tube. In phase and quadrature phase measurements of the specimen's susceptibility indicated that some improvement in homogeneity takes place in drop tube processing. These phase measurements also indicated little or no shielding of a lower Tc phase by a higher Tc filamentary structure.
The objectives of this work are: to determine if surface tension-driven convection in float zone experiments may be controlled by means of surface films; and if convection can be controlled, determine whether homogeneous solute distributions will be achieved in float zone solidification and whether accurate measurements of liquid diffusion coefficients may be obtained from float zone solidification experiments. Sn was chosen as a model material because it is a group IV element, chemically similar to Si and Ge and its low melting point and low vapor pressure allow Auger spectroscopy to be employed with liquid samples.
The interaction of heat, mass, and momentum transport in the floating zone method for growing single crystals from the melt is examined. Methods for detailed numerical simulation of the transport phenomena in a floating zone are developed. Results of the calculations are combined with experiments to determine the effects of solidification induced, surface tension driven, and buoyancy driven convection in establishing dopant redistribution in the melt and the roles of heat transfer in crystal and melt and melt/solid interface shape in determining crystal quality. State of the art finite element techniques were developed for calculating the influence of natural convection in the melt on the shape of a melt/crystal interface and dopant segregation in the crystal. These techniques are demonstrated for solidification by the Bridgman technique. Numerical techniques are developed that calculate the shapes of both the melt/solid and melt/gas interfaces simultaneously with the thermal fields in melt and solid. Models for the fluid flows due to the rotation of the feed and crystal rods are completed and the effects of these flows on dopant segregation are studied, especially in the case of zones longer than can be achieved on Earth.
Developments of particulate metallurgy of alloyed materials where the final products is a fully dense body are discussed. Particulates are defined as powders, flakes, foils, silvers, ribbons and strip. Because rapid solidification is an important factor in particulate metallurgy, all of the particulates must have at least one dimension which is very fine, sometimes as fine as 10 to 50 microns, but move typically up to several hundred microns, provided that the dimension permits a minimum solidification rate of at least 100 K/s.
Investigations of the interactions of heat, mass, and momentum transport in crystal growth from the melt are described. Studies of the mall-scale floating zone process and on a prototype of the vertical Bridgman growth system were emphasized. In both systems detailed numerical calculations are used to dissect the interplay between fluid convection and dopant segregation. These calculations are based on finite element techniques that make feasible the complete solution of solidification problems which include convection. Other numerical methods were developed for solving thermal models of crystal growth processes with melt/gas menisci and for simulating the microscale instabilities in solidification interfaces.
The morphologies and distribution of the MC carbides in Mar-M247 ingot stock and castings were investigated using metallographic, X-ray diffraction and energy-dispersive X-ray analysis techniques. The MC carbides were found to form script structures during solidification. The script structures were composed of three distinct parts. The central cores and elongated arms of the MC carbide script structures had compositions (Ti, Cr, Hf, Ta, W)C and lattice parameters of 4.39 A. The elongated script arms terminated in enlarged, angular "heads". The heads had compositions (Ti, Hf, Ta, W)C and lattice parameters of approximately 4.50 A. The heads had a higher Hf content than the cores and arms. The size of the script structures, as well as the relative amount of head-type to core and arm-type MC carbide, was found to be determined by solidification conditions. No carryover of the MC carbides from the ingot stock to the remelted and cast material was observed.
After a brief historical review of the economics of expendable-booster, commercial-payload operations to date, and a description of the Space Shuttle system's design, operational capabilities, and mission profile, the payload flight assignments, materials processing experiments, and Spacelab I material science experiment are detailed. Among the Materials Processing in Space (MPS) fields for investigation are crystal growth from vapor and solution, the production of magnetic composites and metal foams, laser host glasses and metallic glasses, non-buoyancy-driven convections, unidirectional solidification of eutectics, and the solidification of immiscible alloys. Emphasis is put on the long-term, commercial usefulness of such studies, with attention to historical precedents such as the Skylab, Apollo and Apollo-Soyuz programs.
The groundwork for the use of advanced optical measurement techniques in Space Shuttle materials processing in space (MPS) experiments is being laid in tests, conducted aboard a NASA KC-135 aircraft flying a parabolic trajectory, involving a Mach-Zehnder interferometer and a sideband holographic unit. The two experiments described are (1) the observation of flow during solidification, in which fluid concentration and temperature profiles were measured during unidirectional solidification of a saturated NH4Cl-H2O solution, and (2) the observation of electrodeposition flow, in which interferometry is used to provide quantitative data required in the understanding of electrochemical process transport properties. The free-floating holographic unit was operated in the microgravity environment to both test the practicality of optical systems in such conditions and test the shock and vibration characteristics of the package.
The thirty-two meter drop tube at the Marshall Space Flight Center was used to study the effect of zero gravity containerless processing on the structure and properties of materials. The concept involves the suppression of heterogeneous nucleation of solid in liquid and, therefore, solidification accompanied by large degrees of undercooling. Under these conditions metastable phases can be formed or, at the very least, unique nonequilibrium microstructures (containing equilibrium phases) with unique properties can be produced. The drop tube solidification was applied to niobium base alloys with emphasis on the Nb-Ge binary system in an effort to produce metastable phases with high superconducting transition temperatures in bulk specimens. In the past, only lower Ge alloys (Nb-13 a/o, Nb-18 a/o, and Nb-22 a/o) could be undercooled. Higher Ge alloys (e.g., Nb-25 a/o Ge and Nb-27 a/o Ge) can now be undercooled on a routine basis.
Directional solidification by the Heat Exchanger Method (HEM) is a viable approach for directional solidification of silicon ingots used for terrestrial solar cell applications. Some of the significant advances made during this phase of the program were: ingot size, 34 cm x 34 cm x 17 cm - 45 kg, usable material yield - 90%, solar cell efficiency averaged over the whole ingot - 85% of control CZ (35 kg ingot), very uniform resistivity over the boule, and cycle time for 36 kg ingots - 56 hours. Some of the problems encountered were growth rate decrease with increased ingot height, silicon carbide precipitates, and high dislocation density in HEM material. The silicon carbide is attributed to backstreaming of oil vapors from the vacuum pump; the high dislocation density is associated with the thermal history of the boule.