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NASA NTRS2004

Interaction of Porosity with a Planar Solid/Liquid Interface

In this article, an investigation of the interaction between gas porosity and a planar solid/liquid (SL) interface is reported. A two-dimensional numerical model able to accurately track sharp SL interfaces during solidification of pure metals and alloys is proposed. The finite-difference method and a rectangular undeformed grid are used for computation. The SL interface is described through the points of intersection with the grid lines. Its motion is determined by the thermal and solute gradients at each particular point. Changes of the interface temperature because of capillarity or solute redistribution as well as any perturbation of the thermal and solute field produced by the presence of non-metallic inclusions can be computed. To validate the model, the dynamics of the interaction between a gas pore and a solidification front in metal alloys was observed using a state of the art X-ray transmission microscope (XTM). The experiments included observation of the distortion of the SL interface near a pore, real-time measurements of the growth rate, and the change in shape of the porosity during interaction with the SL interface in pure Al and Al-0.25 wt pct Au alloy. In addition, porosity-induced solute segregation patterns surrounding a pore were also quantified.

Catalina, Adrian V.↗
NASA NTRS2005

Reproducible Crystal Growth Experiments in Microgravity Science Glovebox at the International Space Station (SUBSA Investigation)

Solidification Using a Baffle in Sealed Ampoules (SUBSA) is the first investigation conducted in the Microgravity Science Glovebox (MSG) Facility at the International Space Station (ISS) Alpha. 8 single crystals of InSb, doped with Te and Zn, were directionally solidified in microgravity. The experiments were conducted in a furnace with a transparent gradient section, and a video camera, sending images to the earth. The real time images (i) helped seeding, (ii) allowed a direct measurement of the solidification rate. The post-flight characterization of the crystals includes: computed x-ray tomography, Secondary Ion Mass Spectroscopy (SIMS), Hall measurements, Atomic Absorption (AA), and 4 point probe analysis. For the first time in microgravity, several crystals having nearly identical initial transients were grown. Reproducible initial transients were obtained with Te-doped InSb. Furthermore, the diffusion controlled end-transient was demonstrated experimentally (SUBSA 02). From the initial transients, the diffusivity of Te and Zn in InSb was determined.

Ostrogorsky, A.↗
NASA NTRS2005

The Pore Formation and Mobility Investigation: A Case Study for Conducting Research on the International Space Station in Support of Exploration

The Pore Formation and Mobility Investigation (PFMI) is being conducted in the Microgravity Science Glovebox (MSG) aboard the International Space Station (ISS) with the goal of understanding bubble generation and interactions during controlled directional solidification processing. Through the course of the experiments, beginning in September 2002, a number of key factors pertinent to solidification processing of materials in a microgravity environment have been directly observed, measured, and modeled. Though most experiments ran uninterrupted, on four separate occasions malfunctions to the PFMI hardware and software were experienced that required crew intervention, including in-space repair. Fortunately, each repair attempt was successful and restored the PFMI apparatus to a fully functional condition. Based on PFMI results and lessons learned, the intent of this presentation is to draw attention to the role ISS experiments/hardware can play in providing insight to potential fabrication processing techniques and repair scenarios that might arise during long duration space transport and/or on the lunar/Mars surface.

Grugel, R. N.↗
NASA NTRS2005

Three-System Isotopic of Lunar Norite 78238: Rb-Sr Results

The duration of lunar magma ocean (LMO) crystallization is poorly constrained (Fig. 1). Three techniques employed to determine the age of LMO solidification are 1) dating ferroan anorthosites (FANs), thought to be primary cumulates from the LMO, 2) calculating model ages for KREEP, the most incompatible element enriched material that remained after approx.99.5% of the LMO crystallized [1], and 3) constraining the age of the oldest KREEP-rich magnesium suite (Mg-suite) or alkali suite rock. Dating FANs is difficult because the samples are essentially monomineralic and contain low abundances of many elements used in isotopic dating. In addition, the young ages determined for some FANs may be related to impact metamorphism, potentially making FANs non-ideal for dating the age of LMO crystallization (e.g., [2]). Model ages for KREEP formation are dependent on the assumptions of the initial isotopic composition and parent/daughter ratio of the source. However, lunar rocks are susceptible to isotopic resetting and volatile element loss during shock, and are therefore unlikely to yield consistent model LMO crystallization ages (e.g., [3]). Rocks from the Mg-suite contain KREEP, indicating that they formed after LMO crystallization, and have old ages that indicate they formed almost immediately after the LMO crystallized (Fig. 1). Therefore, precisely dating the oldest Mg-suite rock is a promising way to constrain the age of LMO solidification.

Edmundson, J.↗
NASA NTRS2000

Onset of Convection Due to Surface Tension Variations in Multicomponent and Binary Fluid Layers

Under certain conditions, such as in thin liquid films or microgravity, surface tension variations along a free surface can induce convection. Convection onset due to surface tension variation is important to many terrestrial technological processes in addition to microgravity materials processing applications. Examples include coating, drying crystallization, solidification, liquid surface contamination, and containerless processing. In double-diffusive and multicomponent systems, the spatial variations of surface tension are associated with two or more stratifying agencies, respectively. For example, both temperature and species (concentration) gradients are associated with convection in the solidification of binary alloys or salt ponds. The direction of the two (or more) gradients has a profound effect on the nature of the flow at or slightly beyond the onset of convection. Our recent work at the NASA Lewis Research Center focused on characterizing surface-tension-induced onset of convection, often referred to as Marangoni-Benard convection. Exact solutions for the stationary neutral stability of multicomponent fluid layers with interfacial deformation were derived. These solutions also permit the computation of a boundary curve that separates the long and finite wavelength instabilities. Computing points along this boundary using the exact solution (when possible) is more efficient than the typical numerical approaches, such as finite difference or spectral methods. Above the curve, a long wavelength instability was predicted, suggesting that convection would occur principally through one large flow cell in the layer, whereas below the curve, finite wavelength instabilities occur which suggest multiple finite-sized circulation cells. For many common liquids with layer depths greater than 100 mm, finite wave instability is predicted under terrestrial conditions; however, with little exception, long wavelength instability is predicted in microgravity for the identical fluid systems.

Skarda, J. Raymond Lee↗
NASA NTRS2006

The Pore Formation and Mobility Investigation: A Summary of Conducted Research on the International Space Station

The Pore Formation and Mobility Investigation (PFMI) is being conducted in the Microgravity Science Glovebox (MSG) aboard the International Space Station (ISS) with the goal of understanding bubble generation and interactions during controlled directional solidification processing. Through the course of the experiments, beginning in September 2002, a number of key factors pertinent to solidification processing of materials in a microgravity environment have been directly observed, measured, and modeled. Though most experiments ran uninterrupted, on four separate occasions malfunctions to the PFMI hardware and software were experienced that required crew intervention, including in-space repair. Fortunately, each repair attempt was successful and restored the PFMI apparatus to a fully functional condition. Based on PFMI results and lessons learned, the intent of this presentation is to draw attention to the role ISS experiments/hardware can play in providing insight to potential fabrication processing techniques and repair scenarios that might arise during long duration space transport and/or on the lunar/Mars surface.

Grugel, R. N.↗
NASA NTRS2006

Io: Loki Patera as a Magma Sea

We develop a physical model for Loki Patera as a magma sea. We calculate the total volume of magma moving through the Loki Patera volcanic system every resurfacing cycle (approx.540 days) and the resulting variation in thermal emission. The rate of magma solidification at times reaches 3 x 10(exp 6) kg per second, with a total solidified volume averaging 100 cu km per year. A simulation of gas physical chemistry evolution yields the crust porosity profile and the timescale when it will become dense enough to founder in a manner consistent with observations. The Loki Patera surface temperature distribution shows that different areas are at different life cycle stages. On a regional scale, however, there can be coordinated activity, indicated by the wave of thermal change which progresses from Loki Patera's SW quadrant toward the NE at a rate of approx.1 km per day. Using the observed surface temperature distribution, we test several mechanisms for resurfacing Loki Patera, finding that resurfacing with lava flows is not realistic. Only the crustal foundering process is consistent with observations. These tests also discovered that sinking crust has a 'heat deficit' which promotes the solidification of additional magma onto the sinking plate ("bulking up"). In the limiting case, the mass of sinking material can increase to a mass of approx.3 times that of the foundering plate. With all this solid matter sinking, there is a compensating upward motion in the liquid magma. This can be in excess of 2 m per year. In this manner, solid-liquid convection is occurring in the sea.

heat flow↗
NASA NTRS2008

Formation of gamma(sup prime)-Ni3Al via the Peritectoid Reaction: gamma + beta (+ Al2O3)=gamma(sup prime)(+ Al2O3)

The activities of Al and Ni were measured using multi-cell Knudsen effusion-cell mass spectrometry (multi-cell KEMS), over the composition range 8-32 at.%Al and temperature range T=1400-1750 K in the Ni-Al-O system. These measurements establish that equilibrium solidification of gamma(sup prime)-Ni3Al-containing alloys occurs by the eutectic reaction, L (+ Al2O3)=gamma + Beta(+ Al2O3), at 1640 +/- 1 K and a liquid composition of 24.8 +/- 0.2 at.%al (at an unknown oxygen content). The {gamma + Beta (+Al2O3} phase field is stable over the temperature range 1633-1640 K, and gamma(sup prime)-Ni3Al forms via the peritectoid, gamma + Beta (+ Al2O3)=gamma(sup prime) (+ Al2O3), at 1633 +/- 1 K. This behavior is consistent with the current Ni-Al phase diagram and a new diagram is proposed. This new Ni-Al phase diagram explains a number of unusual steady-state solidification structures reported previously and provides a much simpler reaction scheme in the vicinity of the gamma(sup prime)-Ni2Al phase field.

Copeland, Evan↗
NASA NTRS2009

Dewetting and Segregation of Zn-Doped InSb in Microgravity Experiments

In directional solidification, dewetting is characterized by the lack of contact between the crystal and the crucible walls, due to the existence of a liquid meniscus at the level of the solid-liquid interface. This creates a gap of a few tens of micrometers between the crystal and the crucible. One of the immediate consequences of this phenomenon is the dramatic improvement of the quality of the crystal. This improvement is partly due to the modification of the solid-liquid interface curvature and partly to the absence of sticking and spurious nucleation at the crystal-crucible interface. Dewetting has been, commonly observed during the growth of semiconductors in crucibles under microgravity conditions where it appears to be very stable: the gap between the crystal and the crucible remains constant along several centimetres of growth. The physical models of the phenomenon are well established and they predict that dewetting should not occur in microgravity, if sufficient static pressure is imposed on the melt, pushing it towards the crucible. We present the results of InSb(Zn) solidification experiments conducted at the International Space Station (ISS) where, in spite of a spring exerting a pressure on the liquid, partial dewetting did occur. This surprising result is discussed in terms of force exerted .by the spring on the liquid and of possibility that the spring did not work properly. Furthermore, it appears that the segregation of the Zn was not affected by the occurrence of the dewetting. The data suggest that there was no significant interference of convection with segregation of Zn in InSb.

Ostrogorsky, A. G.↗
NASA NTRS2008

Formation of gamma'-Ni3Al via the Peritectoid Reaction: gamma plus beta (+Al2O3) equals gamma'(+Al2O3)

The activities of Al and Ni were measured using multi-cell Knudsen effusion-cell mass spectrometry (multi-cell KEMS), over the composition range 8 - 32 at.%Al and temperature range T = 1400 - 1750 K in the Ni-Al-O system. These measurements establish that equilibrium solidification of gamma'-Ni3Al-containing alloys occurs by the eutectic reaction, L (+ Al2O3) = gamma + beta (+ Al2O3), at 1640 plus or minus 1 K and a liquid composition of 24.8 plus or minus 0.2 at.%Al (at an unknown oxygen content). The {gamma + beta + Al2O3} phase field is stable over the temperature range 1633 - 1640 K, and gamma'-Ni3Al forms via the peritectiod, gamma + beta (+ Al2O3) = gamma'(+ Al2O3), at 1633 plus or minus 1 K. This behavior is inconsistent with the current Ni-Al phase diagram and a new diagram is proposed. This new Ni-Al phase diagram explains a number of unusual steady state solidification structures reported previously and provides a much simpler reaction scheme in the vicinity of the gamma'-Ni3Al phase field.

Copland, Evan↗
NASA NTRS2012

Dendrite Array Disruption by Bubbles during Re-melting in a Microgravity Environment

As part of the Pore Formation and Mobility Investigation (PFMI), Succinonitrile Water alloys consisting of aligned dendritic arrays were re-melted prior to conducting directional solidification experiments in the microgravity environment aboard the International Space Station. Thermocapillary convection initiated by bubbles at the solid-liquid interface during controlled melt back of the alloy was observed to disrupt the initial dendritic alignment. Disruption ranged from detaching large arrays to the transport of small dendrite fragments at the interface. The role of bubble size and origin is discussed along with subsequent consequences upon reinitiating controlled solidification.

Grugel, Richard N.↗
NASA NTRS2012

Depth and Differentiation of the Orientale Melt Lake

Impact melt emplacement and evolution in lunar multi-ring basins is poorly understood since impact melt deposits in basins are generally buried by mare basalt fill and obscured by subsequent impact cratering. The relatively young Orientale basin, which is only partially flooded with mare basalt, opens a rare window into basin-scale impact melts. We describe the geology of impact melt-related facies in Orientale and suggest that the central depression of Orientale may represent a solidified impact melt lake that vertically subsided shortly after basin formation due to solidification and cooling. We use Lunar Orbiter Laser Altimeter (LOLA) data to measure the depth (approx. 1.75 km) and diameter (approx 350 km) of this central depression. If all the observed subsidence of the central depression is due to solidification and cooling, the melt lake should be approx 12.5-16 km deep, far more voluminous (approx 106 km3) than the largest known differentiated igneous intrusions on Earth. We investigate the possibility that the Orientale melt lake has differentiated and model 1) the bulk composition of the melt lake, 2) the operation of melt mixing in the melt lake, and 3) the chemical evolution of the resulting liquids on the An-Fo-Qz ternary in order to predict the lithologies that might be present in the solidified Orientale melt lake. Finally, we consider the possible significance of these lithologies.

Vaughan, W. M.↗
NASA NTRS2012

Real Time In Situ Observations of Equiaxed Dendrite Coherency in Al-Cu Alloys Using High-Brilliance, 3rd Generation Synchrotron Sources

In the last decade synchrotron X-ray sources have fast become the tool of choice for performing in-situ high resolution imaging during alloy solidification. This paper presents the results of an experimental campaign carried out at the European Synchrotron Radiation Facility, using a Bridgman furnace, to monitor phenomena during solidification of Al-Cu alloys - specifically the onset of equiaxed dendrite coherency. Conventional experimental methods for determining coherency involve measuring the change in viscosity or measuring the change in thermal conductivity across the solidifying melt Conflicts arise when comparing the results of these experimental techniques to find a relationship between cooling rate and coherency fraction. It has been shown that the ratio of average velocity to the average grain diameter has an inversely proportional relationship to coherency fraction. In-situ observation therefore makes it possible to measure these values directly from acquired images sequences and make comparisons with published results.

Murphy, Andrew G.↗
NASA NTRS2012

Studies of Thermophysical Properties of Metals and Semiconductors by Containerless Processing Under Microgravity

Electromagnetic levitation under microgravity provides unique opportunities for the investigation of liquid metals, alloys and semiconductors, both above and below their melting temperatures, with minimized disturbances of the sample under investigation. The opportunity to perform such experiments will soon be available on the ISS with the EML payload which is currently being integrated. With its high-performance diagnostics systems EML allows to measure various physical properties such as heat capacity, enthalpy of fusion, viscosity, surface tension, thermal expansion coefficient, and electrical conductivity. In studies of nucleation and solidification phenomena the nucleation kinetics, phase selection, and solidification velocity can be determined. Advanced measurement capabilities currently being studied include the measurement and control of the residual oxygen content of the process atmosphere and a complementary inductive technique to measure thermophysical properties.

Seidel, A.↗
NASA NTRS2012

Contribution to "AIAA Aerospace Year in Review" article

The NASA Marshall Space Flight Center Microgravity Science Program is dedicated to promoting our understanding of materials processing by conducting relevant experiments in the microgravity environment and supporting related modeling efforts with the intent of improving ground-based practices. Currently funded investigations include research on dopant distribution and defect formation in semiconductors, microstructural development and transitions in dendritic casting alloys, coarsening phenomena, competition between thermal and kinetic phase formation, and the formation of glassy vs. crystalline material. NASA Microgravity Materials Science Principle Investigators are selected for funding either through a proposal in response to a NASA Research Announcement or by collaborating on a team that has successfully proposed to a foreign space agency research announcement. In the latter case, a US investigator can then apply to NASA for funding through an unsolicited proposal. The International Space Station (ISS) facilities used for the experimental investigations are provided primarily by partnering with foreign agencies and often US investigators are working as a part of a larger team studying a specific area of materials science. Facilities for conducting experiments aboard the ISS include the European Space Agency (ESA) Low Gradient Facility (LGF) and the Solidification and Quench (SQF) modular inserts to the Materials Research Rack/Materials Science Laboratory and are primarily used for controlled solidification studies. The French Space Agency (CNES) provided DECLIC facility allows direct observation of morphological development in transparent materials that solidify analogously to metals. The ESA provided Electro ]Magnetic Levitator (EML) is designed to levitate, melt and then cool samples in order to determine material properties, study nucleation behavior, and document phase transitions. Finally, the Microgravity Science Glovebox (MSG) serves as a onboard facility for supporting the hardware required to conduct a number of smaller, short-term investigations.

Grugel, Richard N.↗
NASA NTRS2012

Primary Dendrite Array Morphology: Observations from Ground-based and Space Station Processed Samples

Influence of natural convection on primary dendrite array morphology during directional solidification is being investigated under a collaborative European Space Agency-NASA joint research program, "Microstructure Formation in Castings of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST)". Two Aluminum-7 wt pct Silicon alloy samples, MICAST6 and MICAST7, were directionally solidified in microgravity on the International Space Station. Terrestrially grown dendritic monocrystal cylindrical samples were remelted and directionally solidified at 18 K/cm (MICAST6) and 28 K/cm (MICAST7). Directional solidification involved a growth speed step increase (MICAST6-from 5 to 50 micron/s) and a speed decrease (MICAST7-from 20 to 10 micron/s). Distribution and morphology of primary dendrites is currently being characterized in these samples, and also in samples solidified on earth under nominally similar thermal gradients and growth speeds. Primary dendrite spacing and trunk diameter measurements from this investigation will be presented.

Tewari, Surendra↗
NASA NTRS2012

Primary Dendrite Array: Observations from Ground-Based and Space Station Processed Samples

Influence of natural convection on primary dendrite array morphology during directional solidification is being investigated under a collaborative European Space Agency-NASA joint research program, Microstructure Formation in Castings of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST). Two Aluminum-7 wt pct Silicon alloy samples, MICAST6 and MICAST7, were directionally solidified in microgravity on the International Space Station. Terrestrially grown dendritic monocrystal cylindrical samples were remelted and directionally solidified at 18 K per centimeter (MICAST6) and 28 K per centimeter (MICAST7). Directional solidification involved a growth speed step increase (MICAST6-from 5 to 50 millimeters per second) and a speed decrease (MICAST7-from 20 to 10 millimeters per second). Distribution and morphology of primary dendrites is currently being characterized in these samples, and also in samples solidified on earth under nominally similar thermal gradients and growth speeds. Primary dendrite spacing and trunk diameter measurements from this investigation will be presented.

Tewari, Surendra N.↗
NASA NTRS2014

NASA MSFC Electrostatic Levitator (ESL) Rapid Quench System

Electrostatic levitation, a form of containerless processing, is an important tool in materials research. Levitated specimens are free from contact with a container; therefore, heterogeneous nucleation on container walls is not possible. This allows studies of deeply undercooled melts. Furthermore, studies of high‐temperature, highly reactive materials are also possible. Studies of the solidification and crystallization of undercooled melts is vital to the understanding of microstructure development, particularly the formation of alloys with unique properties by rapid solidification. The NASA Marshall Space Flight Center (MSFC) Electrostatic Levitator (ESL) lab has recently been upgraded to allow for rapid quenching of levitated materials. The ESL Rapid Quench System uses a small crucible‐like vessel that can be partially filled with a low melting point material, such as a Gallium alloy, as a quench medium. An undercooled sample can be dropped into the vessel to rapidly quench the sample. A carousel with nine vessels sits below the bottom electrode assembly. This system allows up to nine rapid quenches before having to break vacuum and remove the vessels. This new Rapid Quench System will allow materials science studies of undercooled materials and new materials development. In this presentation, the system is described and initial results are presented.

SanSoucie, Michael P.↗