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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.
A constitutive theory is presented for representing the anisotropic viscoplastic behavior of high temperature alloys that posses directional properties resulting from controlled grain growth or solidification. The theory is an extension of a viscoplastic model that was applied in structural analyses involving isotropic metals. Anisotropy is introduced through the definition of a vector field that identifies a preferential (solidification) direction at each material point. Following the development of a full multiaxial theory, application is made to homogeneously stressed elements in pure shear and to a uniaxially stressed rectangular block in plane stress with the stress direction oriented at an arbitrary angle with the material direction. It is shown that an additional material parameter introduced to characterize the degree of anisotropy can be determined on the basis of simple creep tests.
Studies of the effects of gravitation on the behavior of fluids and the shapes of materials for the years 1977-1982 are reviewed, with a focus on ground-based research which complements and gives direction to experimentation in the reduced-gravity environment of space. Fluid-behavior topics discussed include crystal growth from melts and from vapor, dendritic solidification and casting, multiphase alloy solidification, electrophoresis, convection behavior, and special heat-flow considerations characteristic of the space environment. With regard to solids, such subjects as containerless positioning technology and its applications (in glass preparation, liquid drop and shell studies, nucleation experiments, and measurements of fundamental properties of molten reactants), liquid floating zones, solid self-deformation, and sedimentation and buoyancy effects are considered and illustrated.
A change in thermal conductivity associated with melting or solidification can have a profound influence on the isotherms near the solidification interface if the material is being directionally solidified in an ampoule whose walls carry a substantial portion of the heat. This analysis was prompted by a recent discovery that the thermal conductivity of Hg(1-x)CD(x)Te increased dramatically as the material is heated above the solidus curve. An illustrative example is shown in which the sample is approximated as an infinite cylinder with constant but diffferent thermal properties in the solid and melt. The boundary conditions are fixed on the surface by a conductive ampoule in a two-zone Bridgman furnace with an adiabatic region separating the two zones. The effect of the adiabatic zone in this case is to intensify the curvature of the interface rather than to lessen it.
Deviation in controlled-rod eutectic morphology anticipated for diffusion only crystal growth characterized at low solidification velocities. Naturally induced, gravity-related convective instabilities result in nonalined irregularly dispersed fibers or platelets. Lower solidification limit for controlled growth Bi/Mn alloys is 1 centimeter/ hour.
Numerical and analytical solutions are presented for the temperature and concentration distributions during the solidification of a binary liquid alloy slab. The slab is taken to be of a finite depth but infinite in the horizontal direction. The solidification process is started by withdrawing a fixed amount of heat from the lower surface of the slab. The upper surface of the slab is subjected to both radiation and convective conditions. The solution gives the concentration and temperature profiles and the interface position as a function of time. Due to the smallness of the mass diffusion coefficient in the solid, the numerical solution method breaks down whenever the ratio of the diffusivities in the solid and the liquid falls below a certain value. An analytical method is developed which gives accurate solution for any value of the diffusivity ratio.