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There are three sets of Japanese containerless experiments. The first is Drop dynamics research. It consists of acoustic levitation and large amplitude drop oscillation. The second is Optical materials processing in an acoustic levitation furnace. And the third is Electrostatic levitator development by two different Japanese companies.
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A program was conducted to develop the technique of space processing for chalcogenide glass, and to define the process and equipment necessary. In the course of this program, successful long term levitation of objects in a 1-g environment was achieved. Glass beads 4 mm diameter were containerless melted and fused together.
A containerless low-gravity environment, produced within a 32 m drop tube apparatus, has been used to undercool and solidify metals, alloys or glasses by eliminating crucible induced nucleation processes. Niobium droplets with diameters in the range of 2 to 5 mm have been undercooled by 525 K which corresponds to the maximum undercooling reported by Turnbull and others on fine dispersions of low melting point metals. Solidification at large undercooling resulted in single crystalline spheres with the formation of interdendritic shrinkage channels on the sample surface rather than interior shrinkage cavities. The grain refinement as observed for Ni samples undercooled and solidified in fused silica crucibles does not occur in free-falling drops of Nb. A calculated solidification speed of undercooled Nb is compared to Ni. A solidification speed of 320 m/s is found for the Nb drops. This solidification speed is greater than or comparable to the solidification speeds calculated in splat cooled samples. Thus, a drop tube apparatus can be useful in the preparation and study of high temperature metastable compounds or alloys in bulk form.
The experimental work performed thus far has resulted in the preparation of new glass compositions not reported heretofore in the open literature. Recent experiments which have resulted in the formation of 1/4-inch-diameter glass samples from two compositions, suggest that containerless melting and cooling as envisioned for space operations is of real technological significance. To date studies of space glasses have by choice been confined to oxide glasses only. It is felt that the applications for such glasses are more readily predictable than for the other materials, and that many of the principles that will evolve from a study of oxide glasses, which can be melted in air, permit a more direct approach to non-oxide materials in the future. The compositions being studied are all very simple in terms of traditional glass practices, none of them containing more than three major constituents. Future efforts should be concerned with more complex compositions, both to cover a broader range of optical properties and to enhance glass-forming tendencies.
With the upper temperature limit of the Ni-based superalloys attained, a new class of materials is required. Intermetallics appear as likely candidates because of their attractive physical properties. With a relatively low density, high thermal conductivity, excellent oxidation resistance, high melting point, and simple crystal structure, nickel aluminide (NiAl) appears to be a potential candidate. However, NiAl is limited in structural applications due to its low room temperature fracture toughness and poor elevated temperature strength. One approach to improving these properties has been through the application of eutectic composites. Researchers have shown that containerless directional solidification of NiAl-based eutectic alloys can provide improvement in both the creep strength and fracture toughness. Although these systems have shown improvements in the mechanical properties, the presence of refractory metals increases the density significantly in some alloys. Lower density systems, such as the carbides, nitrides, and borides, may provide NiAl-based eutectic structure. With little or no information available on these systems, experimental investigation is required. The objective of this research was to locate and develop NiAl-carbide eutectic alloys. Exploratory arc-melts were performed in NiAl-refractory metal-C systems. Refractory metal systems investigated included Co, Cr, Fe, Hf, Mo, Nb, Ta, Ti, W, and Zr. Systems containing carbides with excellent stability (i.e.,HfC, NbC, TaC, TiC, and ZrC) produced large blocky cubic carbides in an NiAl matrix. The carbides appeared to have formed in the liquid state and were randomly distributed throughout the polycrystalline NiAl. The Co, Cr, Fe, Mo, and W systems contained NiAl dendrites with a two-phase interdendritic microconstituent present. Of these systems, the NiAl-Mo-C system had the most promising microstructure for in-situ composites. Three processing techniques were used to evaluate the NiAl-Mo-C system: arc-melting, slow cooling, and containerless directional solidification. Arc-melting provided a wide range of compositions in an economical and simple fashion. The slow cooled ingots provided larger ingots and slower cooling rates than arc-melting. Directional solidification was used to produce in-situ composites consisting of NiAl reinforced with molybdenum carbides.
A simple aerodynamic system which can heat, melt, cool, and solidify (in a containerless fashion) small, roughly spherical (diameter 1.5-4 mm) samples of materials is described. The principal components of the system are an aerodynamic levitation tube and an elliptical radiant heater. The materials processed, i.e., melted and resolidified, in the system include lead and an alkali borosilicate glass. The processing of a glass bead is described. In addition, the physical phenomena which may generate the levitation force in the tube are briefly discussed.
The glass-forming and undercooling ability of PbO-B2O3 melts in the 2PbO.B2O3 to 4PbO.B2O3 composition range were studied. The glass formation propensities were investigated as a function of cooling rate and sample mass. A qualitative investigation of the crystallization process(es) preventing glass formation was made, and it was concluded that under normal circumstances heterogeneous nucleation was the common occurrence. Hence, it was concluded that such compositions are prime candidates for containerless experiments aboard the Space Shuttle.
Scientific experiments conducted in a low-gravity environment make it possible to study effects, such as surface tension-driven flows, which are often masked by buoyancy-driven flows. A summary is provided of several early experiments which demonstrate that unwanted convective flows can be effectively suppressed in experiments conducted in orbiting spacecraft. Possible applications of low-G processing are discussed, taking into account Bridgman growth of solid solution alloy-type semiconductors, Bridgman growth of eutectic systems, and float-zone crystal growth. The control of macrosegregation and phase separation in castings is considered, giving attention also to containerless melting and solidification. A description of experiment facilities and opportunities is provided.
Five experiments involving the processing of semiconductor materials were performed during the Skylab mission. After discussions on semiconductors and their unique electronic properties, and techniques of crystal growth, these five experiments are presented. Four melt growth experiments were attempted: (1) steady state growth and segregation under zero gravity (InSb); (2) seeded, containerless solidification of InSb; (3) influence of gravity-free solidification on microsegregation; and (4) directional solidification of InSb-GaSb alloys. One vapor growth experiment, crystal growth by vapor transport, was attempted.
Proteins account for 50% or more of the dry weight of most living systems and play a crucial role in virtually all biological processes. Since the specific functions of essentially all biological molecules are determined by their three-dimensional structures, it is obvious that a detailed understanding of the structural makeup of a protein is essential to any systematic research pertaining to it. At the present time, protein crystallography has no substitute, it is the only technique available for elucidating the atomic arrangements within complicated biological molecules. Most macromolecules are extremely difficult to crystallize, and many otherwise exciting and promising projects have terminated at the crystal growth stage. There is a pressing need to better understand protein crystal growth, and to develop new techniques that can be used to enhance the size and quality of protein crystals. There are several aspects of microgravity that might be exploited to enhance protein crystal growth. The major factor that might be expected to alter crystal growth processes in space is the elimination of density-driven convective flow. Another factor that can be readily controlled in the absence of gravity is the sedimentation of growing crystal in a gravitational field. Another potential advantage of microgravity for protein crystal growth is the option of doing containerless crystal growth. One can readily understand why the microgravity environment established by Earth-orbiting vehicles is perceived to offer unique opportunities for the protein crystallographer. The near term objectives of the Protein Crystal Growth in a Microgravity Environment (PCG/ME) project is to continue to improve the techniques, procedures, and hardware systems used to grow protein crystals in Earth orbit.
Containerless methods are sought for bulk crystal growth and epitaxy which thus far are a less visible component of materials science in space efforts. In the opinion of the author, this is an anomaly which ought to be corrected, because container interactions are a major problem in earth bound materials processing, including crystal growth, and can be avoided or at least significantly reduced in space. The space environment is unique in solving some of these problems, e.g., memory effects in the integration of different classes of materials in high resolution multilayer heterostructures by molecular beam epitaxy or organometallic molecular beam epitaxy. Spectroscopic method of noncontact temperature measurements exist that could be developed in this context. The error in the absolute temperature measurement achieved by these techniques decreases with decreasing substrate temperature and supplements pyrometric measurements that are better suited for high temperature measurements.
An electromagnetic furnace is being prepared for flights aboard the Space Shuttle. This apparatus is capable of melting metals and alloys up to 1400 C melting point by induction heating with subsequent solidification of the freely levitated melt without contact with any container. The solidification can be carried out with greatly reduced fields resulting in minimal heating and stirring of the free melt. Sequential specimens can be processed during flight. Several experiments are planned for a series of flights, beginning in 1985 with an undercooling experiment of NiSn alloys. These will be interspersed with detailed studies of fluid flow caused by low and high field levels in order to quantify the corresponding effect upon the solidification process.
The 30 meter and 100 meter drop tubes at the Marshall Space Flight Center offer a unique opportunity to study solidification in a containerless, microgravity environment. Samples are melted in a furnace at the top of the drop tube and solidify during a 4.5 second free fall in the 100 meter drop tube or a 2.6 second free fall in the 30 meter drop tube. The cooling rate obtained in the drop tubes is lower than cooling rates in atomization and splat-quenching processes. Decoupling the rapid solidification process allows the study of the effects of undercooling and recalescence on alloy morphologies. The research therefore has a three-fold purpose. The first is examination of the limits of undercooling of niobium and niobium-base alloys in the drop tube. The second purpose is the observation of microstructures resulting from the solidification of samples at large undercoolings and moderate cooling rates. The third purpose is the observation of metastable phase formation in highly undercooled samples.
During the Skylab mission experiments were conducted concerning the influence of weightlessness on molten metals and the solidification process. It was found that the absence of gravity-induced thermal convection and sedimentation modified the properties of the bulk melt. A metals melting experiment was conducted to study the behavior of metal melted by an electron beam and to evaluate the feasibility of joining metals in space. An exothermic brazing experiment investigated the spreading, mixing, and capillary flow of molten braze material. The containerless melting and solidification of small samples of several metals was studied in another experiment. A description is also given of a study of the directional solidification of solid solution alloys.
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.
Space, in contrast to earth, offers total gravity control and unequaled vacuum, temperature, pressure, and radiation characteristics. In zero-g molecular forces such as cohesion and adhesion become controlling factors even in the largest bulk processes. The absence of relative mass accelerations eliminates the need for support of solid matter. Stability in liquid-solid, liquid-liquid, or liquid-gas mixtures, and the absence of thermal convection is obtained because there is no relative motion in fluids due to differences in density. Applications of these characteristics include liquid-matrix preparation of composites, fine-grain castings, supersaturated alloys, combinations which exhibit liquid-phase immiscibility, the containerless free suspension of materials, surface-tension casting, surface-tension drawing, adhesion casting, and controlled density casting.
The containerless melting of high-purity multicomponent homogeneous gels and gel monoliths offers a unique approach to making ultrapure multicomponent optical glasses in the reduced gravity environment of space. Procedures for preparing and characterizing gels and gel-derived glasses in the system Na2O-B2O3-SiO2 are described. Preparation is based on the polymerization reactions of alkoxysilane with trimethyl borate or boric acid and a suitable sodium compound. The chemistry of the gelling process is discussed in terms of process parameters and the gel compositions. The physicochemical nature of gels prepared by three different procedures was found to be significantly different. Infrared absorption spectra indicate finite differences in the molecular structures of the different gels. The melting of the gel powders and the transformation of porous gel monoliths to transparent 'glass' without melting are described.