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NASA NTRS1999

Identification of Gravity-Related Effects on Crystal Growth From Melts With an Immiscibility Gap

This work involves an experimental-numerical approach to study the effects of natural and Marangoni convections on solidification of single crystals from a silicate melt with a liquid-liquid immiscibility gap. Industrial use of crystals grown from silicate melts is becoming increasingly important in electronic, optical, and high temperature structural applications. Even the simplest silicate systems like Al203-SiO2 have had, and will continue to have, a significant role in the development of traditional and advanced ceramics. A unique feature of crystals grown from the silicate systems is their outstanding linear electro-optic properties. They also exhibit exceptionally high optical rotativity. As a result, these crystals are attractive materials for dielectric, optical, and microwave applications. Experimental work in our laboratory has indicated that directional solidification of a single crystal mullite appears to be preceded by liquid-liquid phase separation in the melt. Disruption of the immiscible state results in crystallization of a two phase structure. There is also evidence that mixing in the melt caused by density-driven convection can significantly affect the stability of the immiscible liquid layers and result in poly-crystalline growth. On earth, the immiscible state has only been observed for small diameter crystals grown in float zone systems where natural convection is almost negligible. Therefore, it is anticipated that growth of large single crystals from silicate melts would benefit from microgravity conditions because of the reduction of the natural convective mixing. The main objective of this research is to determine the effects of transport processes on the phase separation in the melt during growth of a single crystal while addressing the following issues: (1) When do the immiscible layers form and are they real?; (2) What are the main physical characteristics of the immiscible liquids?; and (3) How mixing by natural or Marangoni convection affects the stability of the phase separated melt.

Kassemi, M.↗

NASA NTRS1986

Low gravity containerless processing of immiscible gold rhodium alloys

Under normal one-g conditions immiscible alloys segregate extensively during solidification due to sedementation of the more dense of the immiscible liquid phases. However, under low-g conditions it should be possible to form a dispersion of the two immiscible liquids and maintain this dispersed structure during solidification. Immiscible (hypermonotectic) gold-rhodium alloys were processed in the Marshall Space Flight Center 105 meter drop tube in order to investigate the influence of low gravity, containerless solidification on their microstructure. Hypermonotectic alloys composed of 65 atomic % rhodium exhibited a tendency for the gold rich liquid to wet the outer surface of the containerless processed samples. This tendency led to extensive segregation in several cases. However, well dispersed microstructures consisting of 2 to 3 micron diameter rhodium-rich spheres in a gold-rich matrix were produced in 23.4 atomic % rhodium alloys. This is one of the best dispersions obtained in research on immiscible alloy-systems to data.

Andrews, J. Barry↗

NASA NTRS1992

Solidification in immiscible systems: The influence of processing conditions on resulting microstructures

Research carried out over the past two decades in which attempts have been made to produce desirable microstructures in immiscible alloys is reviewed. Factors affecting the formation of desirable microstructures in immiscible alloys are addressed and some of the techniques that have been successful in controlling these factors in order to produce useful structures are discussed. Some of the intended applications of these alloys require a dispersion of one phase in the other, while other applications favor the use of aligned, fibrous microstructures with continuity of both phases. The microstructures obtained in immiscible alloys are often strongly influenced by processing conditions. Perhaps the most well known effect is gravity induced sedimentation of the denser immiscible phase during solidification. This difficulty with sedimentation led to low gravity processing in attempts to produce dispersed microstructures. However, experimentation under low gravity conditions soon revealed that many other factors, including wetting of the crucible walls and surface tension driven flows, often resulted in complete separation and coalescence of the two immiscible phases. The production of aligned fibrous microstructures in hypermonotectic alloys appears to be even more difficult than the formation of a dispersion. Here, in addition to sedimentation and crucible wetting, convective and interfacial instabilities must be considered as well. Calculation of the limits of stability during directional solidification were carried out but require experimental verification.

Andrews, J. Barry↗

NASA NTRS1979

Plagiogranites as late-stage immiscible liquids in ophiolite and mid-ocean ridge suites - An experimental study

A study of relationships between basic and acidic rocks was made by fractionating primitive basalt at low pressure anhydrous conditions at various fugacities. Fractionally crystallized basalt became increasingly enriched in iron which became silicate liquid immiscible, producing Fe-enriched basaltic and granitic liquids. The latter is similar to plagiogranites found in mid-oceanic rift (MOR) regions, showing that silicate liquid immiscibility could be the petrogenic process which produces plagiogranites in some MOR regions and ophiolites. The major problem in considering plagiogranites as products of silicate liquid immiscibility is absence of any description of the Fe-enriched conjugate liquid in the ophiolite or MOR literature, and the identification of this magma is essential for a definite case of silicate liquid immiscibility.

Dixon, S.↗

NASA NTRS1988

Effects of crucible wetting during solidification of immiscible Pb-Zn

Many industrial uses for liquid phase miscibility gap alloys are proposed. However, the commercial production of these alloys into useful ingots with a reasonable amount of homogeneity is arduous because of their immiscibility in the liquid state. In the low-g environment of space gravitational settling forces are abated, thus solidification of an immiscible alloys with a uniform distribution of phases becomes feasible. Elimination of gravitational settling and coalescence processes in low-g also makes possible the study of other separation and coarsening mechanisms. Even with gravitational separation forces reduced, many low-g experiments have resulted in severely segregated structures. The segregation in many cases was due to preferential wetting of the crucible by one of the immiscible liquids. The objective was to analyze the wetting behavior of Pb-Zn alloys on various crucible materials in an effort to identify a crucible in which the fluid flow induced by preferential wetting is minimized. It is proposed that by choosing the crucible for a particular alloy so that the difference in surface energy between the solid and two liqud phases is minimized, the effects of preferential wetting can be diminished and possibly avoided. Qualitative experiments were conducted and have shown the competitive wetting behavior of the immiscible Pb-Zn system and 13 different crucible materials.

Degroh, Henry C., III↗

NASA NTRS1989

Effects of crucible wetting during solidification of immiscible Pb-Zn alloys

Many industrial uses for liquid phase miscibility gap alloys are proposed. However, the commercial production of these alloys into useful ingots with a reasonable amount of homogeneity is arduous because of their immiscibility in the liquid state. In the low-g environment of space gravitational settling forces are abated, thus solidification of an immiscible alloy with a uniform distribution of phases becomes feasible. Elimination of gravitational settling and coalescence processes in low-g also makes possible the study of other separation and coarsening mechanisms. Even with gravitational separation forces reduced, many low-g experiments have resulted in severely segregated structures. The segregation in many cases was due to preferential wetting of the crucible by one of the immiscible liquids. The objective was to analyze the wetting behavior of Pb-Zn alloys on various crucible materials in an effort to identify a crucible in which the fluid flow induced by preferential wetting is minimized. It is proposed that by choosing the crucible for a particular alloy so that the difference in surface energy between the solid and two liquid phases is minimized, the effects of preferential wetting can be diminished and possibly avoided. Qualitative experiments were conducted and have shown the competitive wetting behavior of the immiscible Pb-Zn system and 13 different crucible materials.

De Groh, H. C., III↗

NASA NTRS1989

The nature and barium partitioning between immiscible melts - A comparison of experimental and natural systems with reference to lunar granite petrogenesis

Elemental partitioning between immiscible melts has been studied using experimental liquid-liquid Kds and those determined by analysis of immiscible glasses in basalt mesostases in order to investigate lunar granite petrogenesis. Experimental data show that Ba is partitioned into the basic immiscible melt, while probe analysis results show that Ba is partitioned into the granitic immiscible melt. It is concluded that lunar granite of significant size can only occur in a plutonic or deep hypabyssal environment.

Neal, C. R.↗

NASA NTRS1999

Wetting Characteristics of Immiscibles

Early microgravity experiments with immiscible alloys were usually carried out with the intent of forming dispersed microstructures. By processing under microgravity conditions, the main mechanism leading to gross phase separation could be eliminated. However, analysis of flight samples revealed a separated structure where the minor phase was present along the outer surface, while the major phase was present in the center. The Wetting Characteristics of Immiscibles (WCI) project, which flew aboard the USMP-4 (United States Microgravity Payload) mission in November of 1997, was designed to gain insight into the mechanisms causing segregation of these alloys. This investigation utilized an immiscible transparent organic alloy system and a transparent container in order to facilitate direct observation of the separation process. A range of immiscible alloy compositions was utilized in order to obtain variations in the minor and major phases present and observe the influence on the segregation processes. A small composition range was found where the minor liquid phase perfectly wet the cell gasket. Unexplained observations were made at the extremes of the composition range.

Andrews, J. B.↗

NASA NTRS1974

The electrical properties of low-g processed immiscible alloys

When dispersed or mixed immiscibles are solidified on earth, a large amount of separation of the constituents takes place due to differences in densities. However, when the immiscibles are dispersed and solidified in zero-gravity, density separation does not occur, and unique composite solids can be formed with many new and promising electrical properties. By measuring the electrical resistivity and superconducting critical temperature of zero-g processed Ga-Bi samples, it has been found that the electrical properties of such materials are entirely different from the basic constituents and the ground control samples. The finest dispersions are obtained only in a low-gravity environment. Our results indicate that space-processed immiscible materials may form an entirely new class of electronic materials. The interesting electrical properties of directionally solidified Al-Cu eutectic, a two-component alloy consisting of Al and Al2Cu which was processed on Skylab (M566) are briefly reviewed. The electrical resistivity of directionally solidified eutectics with a lamellar structure are highly anisotropic and have been studied both experimentally and theoretically. The local resistivity of the space-processed samples are compared to a ground control sample and to the expected theoretical results.

Otto, G. H.↗

NASA NTRS1974

The electrical properties of zero-gravity processed immiscibles

Lacy, L. L.↗

NASA NTRS1974

Experimental liquid line of descent and liquid immiscibility for basalt 70017

The paper describes one possible liquid line of descent produced for a high-titanium mare basalt composition through an arbitrarily chosen series of partial equilibrium and fractional crystallization experiments on basalt 70017. The liquid line of descent leading to immiscibility at 994 C is characterized by enrichment of FeO, K2O, SiO2, and MnO and depletion of MgO and TiO2 in the residual liquids. The composition of the residual liquid at the onset of immiscibility is ferrobasaltic, and the initial appearance of immiscible liquids in the form of silica-rich spherules is in the vicinity of plagioclase-liquid contacts. The integrated bulk composition of the areas of finely exsolved liquids indicates that the trend of the liquid line of descent is at a small angle to the tie lines joining the two liquids.

Rutherford, M. J.↗

NASA NTRS1990

Containerless low gravity processing of glass forming and immiscible alloys

Under normal one-g conditions immiscible alloys segregate extensively during solidification due to sedimentation of the more dense of the immiscible liquid phases. Immiscible (hypermonotectic) gold-rhodium alloys were processed in the 100 meter drop tube under low gravity, containerless conditions to determine the feasibility of producing dispersed structures. Three alloy compositions were utilized. Alloys containing 10 percent by volume of the gold-rich hypermonotectic phase exhibited a tendency for the gold-rich liquid to wet the outer surface of the samples. This wetting tendency led to extensive segregation in several cases. Alloys containing 80 and 90 percent by volume of the gold-rich phase possessed completely different microstructures from the 10 percent samples when processed under low-g, containerless conditions. Several samples exhibited microstructures consisting of well dispersed 2 to 3 microns diameter rhodium-rich spheres in a gold-rich matrix.

Andrews, J. Barry↗

NASA NTRS1991

The effect of processing conditions on solidified structures in immiscible systems

The incentive for low-gravity processing of immiscible alloys is usually tied to an attempt to eliminate sedimentation of the more dense immiscible liquid phase during processing. However, many other factors can influence the solidified structure of these alloys. For example, crucible wetting by one of the immiscible liquid phases during normal (non-directional) low-gravity solidification in a container has been shown to often lead to a completely separated structure. For containerless, low-gravity processing, alloy composition has a tremendous affect on the structure formed. During directional solidification, alloy composition, thermal gradient, solidification rate, convective instability and the miscibility gap height of the system all have a major effect on the structures obtained. This paper discusses the conditions necessary for the production of desired microstructures in each of these processing techniques. Examples are shown of samples processed under both desirable and undesirable conditions.

Andrews, J. B.↗

NASA NTRS2013

Compositions of Magmatic and Impact Melt Sulfides in Tissint And EETA79001: Precursors of Immiscible Sulfide Melt Blebs in Shergottite Impact Melts

Immiscible sulfide melt spherules are locally very abundant in shergottite impact melts. These melts can also contain samples of Martian atmospheric gases [1], and cosmogenic nuclides [2] that are present in impact melt, but not in the host shergottite, indicating some components in the melt resided at the Martian surface. These observations show that some regolith components are, at least locally, present in the impact melts. This view also suggests that one source of the over-abundant sulfur in these impact melts could be sulfates that are major constituents of Martian regolith, and that the sulfates were reduced during shock heating to sulfide. An alternative view is that sulfide spherules in impact melts are produced solely by melting the crystalline sulfide minerals (dominantly pyrrhotite, Fe(1-x)S) that are present in shergottites [3]. In this abstract we report new analyses of the compositions of sulfide immiscible melt spherules and pyrrhotite in the shergottites Tissint, and EETA79001,507, and we use these data to investigate the possible origins of the immiscible sulfide melt spherules. In particular, we use the metal/S ratios determined in these blebs as potential diagnostic criteria for tracking the source material from which the numerous sulfide blebs were generated by shock in these melts.

Ross, D. K.↗

NASA NTRS1978

Determination of liquid-phase immiscibility in the lead-zinc system

A number of different techniques in the past have yielded inconsistent equilibrium measurements of immiscibility in the Pb-Zn system above 600 C. Accurate differential thermal analysis (DTA) measurements were performed on well-homogenized samples of high-purity Pb-Zn, and they indicate that the immiscibility curve is higher than previously accepted for Zn compositions between 20 and 70 at. %. The maximum deviations observed correspond to about 20 C. Below 600 C the DTA results agree with previous results.

Trahan, J. F.↗

NASA NTRS1977

Melt immiscibility in Apollo 15 KREEP - Origin of Fe-rich mare basalts

Silicate liquid immiscibility (SLI) is investigated in terms of chemistry and occurrence in two KREEP-rich Apollo 15 basalts. The two samples have different cooling histories but the same composition. In the first sample, SLI occurred at the time of 58% crystallization. In the second sample, SLI occurred after 20% had crystallized. It is noted that SLI could be initiated as soon as plagioclase (out of a total composition which also included zircon, FeS, SiO2, whitlockite, and ilmenite) alone had crystallized. Attention is given to Fe-rich immiscible melts, and it is suggested that SLI may play an important role in the formation of the source regions of Fe-rich mare basalts. The analytical technique used for the assays was an energy dispersive analysis system with a resolution of 167 eV.

Hollister, L. S.↗

NASA NTRS1978

Clast assemblages of possible deep-seated /77517/ and immiscible-melt /77538/ origins in Apollo 17 breccias

Breccia samples 77517 and 77538 are composed of abundant mineral and lithic clasts set in porous, poorly sintered matrices. Clast assemblages in the two rocks are of contrasting composition and origin. Breccia 77517 has Mg-rich olivine and pyroxene and calcic plagioclase clasts, indicating limited, almost exclusively ANT-suite parentage. A significant feature is the presence of an assemblage (aluminous enstatite, forsterite, anorthite, aluminous spinel) corresponding to spinel cataclasite, a rock type of deep-seated (about 60 km) crustal origin. Breccia 77538 contains Fe-rich pyroxene and rather sodic plagioclase clasts, indicative of predominantly KREEP and/or mare derivation. An important feature is the occurrence of high-K and high-Fe lithic clasts whose compositions resemble those of immiscible-melts produced during late-stage magmatic crystallization, and which probably originated via silicate liquid immiscibility in a KREEP or mare basalt magma. Both rocks contain numerous fine-grained breccia clasts which represent material that has been modified by impact processes at or very near the moon's surface.

Warner, R. D.↗

NASA NTRS1985

Diffusion in Immiscible Melts

The objective of this program is to measure the diffusion coefficients for molten Pb in Zn in the immiscible liquid-phase region. Diffusion couples of pure Pb and Zn were prepared using a shear cell. These have been placed in graphite crucibles and encapsulated in stainless steel cartridges and are awaiting the next Materials Experiment Assembly (MEA) flight opportunity. In flight, one couple will be soaked for 40 minutes at 440 deg C (just above the monotectic temperature) and the second couple will be soaked for 40 minutes 820 deg C (just above the consolute temperature). After the soak both samples will be rapidly quenched by flowing He to minimize redistribution of the immiscible phases. Post flight compositional analysis will be accomplished using X-ray fluorescence in the scanning electron microscopy.

Pond, R. B.↗