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NASA NTRS1987

Physical properties of immiscible polymers

The demixing of immiscible polymers in low gravity is discussed. Applications of knowledge gained in this research will provide a better understanding of the role of phase segregation in determining the properties of polymer blends made from immiscible polymers. Knowledge will also be gained regarding the purification of biological materials by partitioning between the two liquid phases formed by solution of the polymers polyethylene glycol and dextran in water. Testing of new apparatus for space flight, extension of affinity phase partitioning, refinement of polymer chemistry, and demixing of isopycnic polymer phases in a one gravity environment are discussed.

Harris, J. Milton↗

NASA NTRS1987

Simulating the cooling of an immiscible alloy

A computer program to simulate the cooling of immiscible alloys is described, and the Pb-Zn system is presented as an example. The program permits the user to calculate various compositions of immiscible alloys. Illustrations are presented which depict the sequence of computer-monitor displays generated by the program.

Probst, H. B.↗

NASA NTRS1990

Silicate liquid immiscibility in isothermal crystallization experiments

The role of silicate liquid immiscibility (SLI) in the petrogenesis of lunar granites was investigated in experiments in which four glasses were synthesized from reagent-grade oxides and carbonates with the compositions of two of the sets of coexisting liquids reported by Hess et al. (1975): a KREEP basalt derivative and a mare basalt derivative. Isothermal crystallization experiments showed that SLI is a stable phenomenon in residual lunar liquids saturated with plagioclase, and is likely to produce large compositional separations. The results indicate that controlled-cooling-rate experiments of Rutherford et al. (1974), and Hess et al. (1975, 1978) were substantially correct analogs of the natural process of liquid immiscibility.

Longhi, J.↗

NASA NTRS1991

Why are blue zhamanshinites blue? Liquid immiscibility in an impact melt

A study of the cause of the coloration of blue zhamanshinites, which are glassy impact melt rocks from the Zhamanshin crater in the USSR are reported. It is found that the blue color results from Rayleigh scattering from spherical, 100 nm-diameter inclusions of a separate Ca-Fe-Mg-P-rich silicate glass. These observations can best be explained by the operation of liquid immiscibility in the zhamanshinite melt, and suggest that liquid immiscibility may have a more general role in impactite evolution.

Zolensky, Michael E.↗

NASA NTRS1993

Rare earth element selenochemistry of immiscible liquids and zircon at Apollo 14 - An ion probe study of evolved rocks on the moon

Results are presented of trace-element analyses of three lunar zircons. The major-element and REE compositions were determined using electron microprobes, and a correction was made for zircon for Zr-Si-O molecular interferences in the La to Pr mass region. The three zircons were found to exhibit similar REE abundances and patterns. Results of the analyses confirm earlier studies (Hess et al., 1975; Watson, 1976; Neal and Taylor, 1989) on the partitioning behavior of trace elements in immiscible liquid-liquid pairs. The results also support the postulated importance of silicate liquid immiscibility in the differentiation of the upper mantle and crust of the moon.

Snyder, Gregory A.↗

NASA NTRS1993

Immiscible phase incorporation during directional solidification of hypermonotectics

Solidification processes in immiscible samples were investigated by directly observing the events taking place at the solid-liquid interface during directional solidification. Visualization of these events was made possible through the use of a transparent metal analog system and a temperature gradient stage assembly fitted to an optical microscope. The immiscible transparent analog system utilized was the succinonitrile-glycerol system. This system has been shown to exhibit the same morphological transitions as observed in metallic alloys of monotectic composition. Both monotectic and hypermonotectic composition samples were directionally solidified in order to gain an improved understanding of the manner in which the excess hypermonotectic liquid is incorporated into the solidifying structure. The processing conditions utilized prevented sedimentation of the excess hypermonotectic liquid by directionally solidifying the samples in very thin (13 microns), horizontally oriented cells. High thermal gradient to growth rate ratios (G/R) were used in an effort to prevent constitutional supercooling and the subsequent formation of L(sub 2) droplets in advance of the solidification front during the growth of fibrous composite structures. Results demonstrated that hypermonotectic composites could be produced in samples up to two weight percent off of the monotectic composition by using a G/R ratio greater than or equal to 4.6 x 10(exp 4) C(s)/mm(sup 2) to avoid constitutional supercooling. For hypermonotectic samples processed with G/R ratios below 4.6 x 10(exp 4) C(s)/mm(sup 2), constitutional supercooling occurred and resulted in slight interfacial instability. For these samples, two methods of incorporation of the hypermonotectic liquid were observed and are reported. The correlation between the phase spacing, lambda, and the growth rate, R, was examined and was found to obey a relationship generally associated with a diffusion controlled coupled growth process. For samples with compositions ranging from the monotectic composition up to 2 percent off of the monotectic composition, data indicated that the square of the phase spacing (lambda) varied linearly with the inverse of the growth rate (R).

Andrews, J. Barry↗

NASA NTRS1998

A Study of Undercooling Behavior Of Immiscible Metal Alloys in the Absence of Crucible-Induced Nucleation

The purpose of this study is to investigate the question: Would eliminating the crucible eliminate the wall-induced nucleation of one of the liquid phases in an immiscible alloy and result in undercooling of the liquid into the metastable region thereby producing significant differences in the separation process and the microstructure upon solidification. Another primary objective of this research is to study systems with a metastable miscibility gap and to directly determine the metastable liquid miscibility gap by undercooling experiments. Nucleation and growth of droplets in these undercooled metallic liquid-liquid mixtures is also being studied. Results of this investigation indicate that containerless processing of immiscibles may not promote the undercooling of the single-phase liquid into the metastable region. Although no recalescence event was observed for this liquid-liquid transition, undercooling did occur across the miscibility gap for the solidification of the Ti phase that eventually separated.

Robinson, Michael B.↗

NASA NTRS2000

Solidification Processing of Immiscible Liquids in the Presence of Applied Ultrasonic Energy

Uniform microstructural development during solidification of immiscible liquids on Earth is hampered by inherent density differences between the phases. Microgravity processing minimizes settling but segregation still occurs due to gravity independent wetting and coalescence phenomena. Experiments with the transparent organic, metal analogue, succinonitrile-glycerol system were conducted in conjunction with applied ultrasonic energy. The processing parameters associated with this technique have been evaluated in view of optimizing dispersion uniformity. Experimental results to evaluate microstructural phase distributions, based on other liquid-liquid immiscibility systems, will also be presented.

Kim, Shinwood↗

NASA NTRS2000

Characterizing the Use of Ultrasonic Energy in Promoting Uniform Microstructural Dispersions in Immiscible Mixtures

Gravity driven separation and preferential wetting precludes uniform microstructural distributions during solidification processing of immiscible, liquid-liquid mixtures. Historically, it is, however, established that liquid/liquid suspensions can be established and maintained by utilizing ultrasound. Following a brief introduction the results of experiments on immiscible mixtures subjected to ultrasonic energy during solidification processing will be compared and evaluated in view of a recently developed mathematical model. The presentation continues by discussion of scaling the model to commercial viability and concludes with the implications of such processing in a microgravity environment.

Grugel, R. N.↗

NASA NTRS2001

Characterizing the Use of Ultrasonic Energy in Promoting Uniform Microstructural Dispersions in Immiscible Mixtures

Grugel, R. N.↗

NASA NTRS1974

Immiscible materials and alloys

Only immiscible materials which involve a fluid phase have a potential advantage when considered for space processing. Processing of such systems at low gravity can lead to a material which is very homogeneous and contains a finely dispersed mixture of phases. Materials with such structures may exhibit potentially useful properties for such applications as superconductors, dispersion-strengthened materials, superplastic materials, permanent magnets, etc. These conclusions have resulted from review of past efforts in the field of low-g processing of materials containing a liquid phase miscibility gap and from present efforts dealing with such systems. These studies have concentrated on precipitation of liquid droplets in a host liquid during cooling through the miscibility gap. This effort has been to study the agglomeration of the droplets both experimentally and through computer simulation in order to understand the mechansism involved and to deduce the effect of gravity on the droplet distribution and resulting structure of the solidified material. The agglomeration mechanisms treated in detail are those due to diffusional growth and collision processes caused by Stokes on convection current-induced droplet migration.

Markworth, A. J.↗

NASA NTRS1974

Preparation and metallurgical properties of low gravity processed immiscible materials

Initial experiments conducted during the Apollo 14 mission demonstrated that unique dispersions of immiscible materials could be obtained by processing in a low gravity environment. Subsequently, seven metallic systems have been processed in three NASA facilities: the drop tower at MSFC, the M-512 facility on board a KC-135 aircraft and the M-518 furnace on board Skylab. All couples were solidified from the liquid while in a low gravity environment, with one gravity processed specimens as controls. Metallographic examination demonstrated that the specimens processed in a low gravity environment exhibited a more uniform dispersion and microstructure than the one gravity processed controls.

Reger, J. L.↗

NASA NTRS1974

The behavior of immiscible liquids in space

A demonstration experiment (TV102) was performed on the Skylab 4 mission to illustrate the behavior of immiscible liquids of different densities in zero-gravity. The purpose of the experiment was to determine the rate of coalescence of two well-characterized liquids, Krytox 143 AZ oil and water, after the liquids were finely dispersed by shaking. An analysis of the video-taped data and 35mm color transparencies indicates that all investigated emulsions were stable with only a small amount of observed coalescence for at least 10 hours after mixing, whereas the fluids in the ground-control case separated completely in 10 seconds. This experiment indicates that the coalescence rate was at least .000003 times smaller on Skylab than on earth.

Lacy, L. L.↗

NASA NTRS1975

Study on processing immiscible materials in zero gravity

An experimental investigation was conducted to evaluate mixing immiscible metal combinations under several process conditions. Under one-gravity, these included thermal processing, thermal plus electromagnetic mixing, and thermal plus acoustic mixing. The same process methods were applied during free fall on the MSFC drop tower facility. The design is included of drop tower apparatus to provide the electromagnetic and acoustic mixing equipment, and a thermal model was prepared to design the specimen and cooling procedure. Materials systems studied were Ca-La, Cd-Ga and Al-Bi; evaluation of the processed samples included the morphology and electronic property measurements. The morphology was developed using optical and scanning electron microscopy and microprobe analyses. Electronic property characterization of the superconducting transition temperatures were made using an impedance change-tuned coil method.

Reger, J. L.↗

NASA NTRS1974

Indications of fluid immiscibility in glass from West Clearwater Lake impact crater, Quebec, Canada

Glass from the West Clearwater Lake hypervelocity impact crater contains numerous spheroids, 10 to 500 microns across, which appear to have formed at high temperatures as fluids immiscible in the enclosing melt. The spheroids are distinguished from small, normal, largely void gas vesicles, which are also present, by being completely filled in all cases; by having fillings which vary in composition from spheroid to spheroid, even between spheroids in close association; and by indications that the present fillings are representative of the contents present before the matrix melt chilled. Most of the spheroids are classified petrographically into three types. The preservation of spheroids in the West Clearwater Lake glass is attributed mainly to the position of the glass masses within the breccias lining the crater floor. It is considered that the glass in this location did not achieve free flight but, as part of a large mass, cooled relatively slowly through the high temperature regime in which the spheroids were generated, and then, when detached, chilled rapidly to preserve a record of this transient stage in their history.

Dence, M. R.↗

NASA NTRS1976

Studies on immiscible alloys

To illustrate the behavior of immiscible liquids of different densities in zero-gravity and to determine the rate of coalescence like droplets, a demonstration experiment was performed on the Skylab 4 mission. Dispersions of oil-in-water and of water-in-oil were prepared by the astronauts and their appearance photographed over a time span of 10 hours. The experiment indicated that all emulsions were stable over this period and that the coalescent rate was at least 3 times 10 to the 5th power times smaller on Skylab than on earth. The recorded melting of a cylindrical piece of ice on Skylab 3 is used to study the mode of heat transfer for the latent heat of melting in low-gravity.

Otto, G.↗

NASA NTRS1976

Experimental development of processes to produce homogenized alloys of immiscible metals, phase 3

An experimental drop tower package was designed and built for use in a drop tower. This effort consisted of a thermal analysis, container/heater fabrication, and assembly of an expulsion device for rapid quenching of heated specimens during low gravity conditions. Six gallium bismuth specimens with compositions in the immiscibility region (50 a/o of each element) were processed in the experimental package: four during low gravity conditions and two under a one gravity environment. One of the one gravity processed specimens did not have telemetry data and was subsequently deleted for analysis since the processing conditions were not known. Metallurgical, Hall effect, resistivity, and superconductivity examinations were performed on the five specimens. Examination of the specimens showed that the gallium was dispersed in the bismuth. The low gravity processed specimens showed a relatively uniform distribution of gallium, with particle sizes of 1 micrometer or less, in contrast to the one gravity control specimen. Comparison of the cooling rates of the dropped specimens versus microstructure indicated that low cooling rates are more desirable.

Reger, J. L.↗

NASA NTRS1977

Microgravity studies in the liquid phase immiscible system, aluminum-indium

As part of a study to understand the influence of gravity, cooling rate and composition on the structure of liquid phase immiscible materials, two alloys, Al-40 wt % In and Al-70 wt % In were thermally treated on the SPAR II rocket flight. The treatments involved homogenization at a temperature above the miscibility gap and then rapid cooling through the miscibility gap followed by complete solidification. The last two steps were performed while acceleration levels were less than 4 x 10 to the -5th g. The flight alloys produced unexpected results. Instead of fine uniform structures, the alloys consisted of a macroscopically sized aluminum-rich central region surrounded by indium-rich metal.

Gelles, S. H.↗