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NASA NTRS2003

Analysis of Radial Segregation in Directionally Solidified Hg(0.89)Mn(0.11)Te

Bridgman growth experiments were performed on Hg(0.89)Mn(0.11)Te (MMT) to determine the extent of radial Manganese segregation during directional solidification. MMT crystals were directionally solidified at rates of 0.09 and 0.18 p d s and in axial thermal gradients of 83 and 68"C/cm. Wavelength Dispersive Spectroscopy (WDS) and Fourier Transform Infra-Red (FTIR) analytical techniques were used to determine the radial homogeneity in all boules and the deflection of the solid-liquid interface (SLI) in two boules that were rapidly quenched after 5 to 6 cm of directional solidification. For all growth runs, the measured radial coinpositional variations were on the order of 0.01 molar percent MnTe in the steady state region of growth. Comparison of the measured radial compositional results of the crystals to predicted values in the diffusion-limited regime indicate a strong influence of convection near the solid-liquid interface. This conclusion is supported by the weak influence of the translation rates and axial thermal gradients utilized in this study upon radial compositional homogeneity.

Price, M. W.↗

NASA NTRS2003

Bubble Formation and Transport during Microgravity Materials Processing: Model Experiments on the Space Station

Flow Visualization experiments on the controlled melting and solidification of succinonitrile were conducted in the glovebox facility of the International Space Station (ISS). The experimental samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with pure succinonitrile (SCN) under 450 millibar of nitrogen. Porosity in the samples arose from natural shrinkage, and in some cases by direct insertion of nitrogen bubbles, during solidification of the liquid SCN. The samples were processed in the Pore Formation and Mobility Investigation (PFMI) apparatus that is placed in the glovebox facility (GBX) aboard the ISS. Experimental processing parameters of temperature gradient and translation speed, as well as camera settings, were remotely monitored and manipulated from the ground Telescience Center (TSC) at the Marshall Space Flight Center. During the experiments, the sample is first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. The temperatures in the sample are monitored by six in situ thermocouples. Real time visualization of the controlled directional melt back shows bubbles of different sizes initiating at the melt interface and, upon dislodging from the melting solid, migrating at different speeds into the temperature field ahead of them, before coming to rest. The thermocapillary flow field set up in the melt, ahead of the interface, is dramatic in the context of the large bubbles, and plays a major role in dislodging the bubble. A preliminary analysis of the observed bubble formation and mobility during melt back and its implication to future microgravity experiments is presented and discussed.

Grugel, R. N.↗

NASA NTRS2004

Materials Processing in Space: Model Experiments aboard the International Space Station

Direct observation of fluid flow, bubble movement and solidification during controlled melting and solidification of succinonitrile were conducted in the glovebox facility of the International Space Station (ISS). The samples were processed in the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) on board the ISS. Experimental processing parameters of temperature gradient and translation speed, as well as camera settings, were remotely monitored and manipulated from the ground Telescience Center (TSC) at the Marshall Space Flight Center. Real time visualization of the controlled directional melt back and resolidification reveals a number of microgravity dependent phenomena otherwise masked by Earth s gravity. These and some initial analysis of the observed events is presented.

Grugel, Richard↗

NASA NTRS2003

Development of Aerogel Molds for Metal Casting Using Lunar and Martian Regolith

In the last few years NASA has set new priorities for research and development of technologies necessary to enable long-term presence on the Moon and Mars. Among these key technologies is what is known as in situ resource utilization, which defines all conceivable usage of mineral, liquid, gaseous, or biological resources on a visited planet. In response to this challenge, we have been focusing on developing and demonstrating the manufacturing of a specific product using Lunar and Martian soil simulants (i.e., a mold for the casting of metal and alloy parts) which will be an indispensable tool for the survival of outposts on the Moon and Mars. In addition, our purpose is to demonstrate the feasibility of using mesoporous materials such as aerogels to serve as efficient casting molds for high quality components in propulsion and other aerospace applications. The first part of the project consists of producing aerogels from the in situ resources available in Martian and Lunar soil. The approach we are investigating is to use chemical processes to solubilize silicates using organic reagents at low temperatures and then use these as precursors in the formation of aerogels for the fabrication of metal casting molds. One set of experiments consists of dissolving silica sources in basic ethylene glycol solution to form silicon glycolates. When ground silica aerogel was used as source material, a clear solution of silicon glycolate was obtained and reacted to form a gel thus proving the feasibility of this approach. The application of this process to Lunar and Martian simulants did not result in the formation of a gel; further study is in progress. In the second method acidified alcohol is reacted with the simulants to form silicate esters. Preliminary results indicate the presence of silicon alkoxide in the product distillation. However, no gel has been obtained so further characterization is ongoing. In the second part of the project, the focus has been on developing a series of aerogel plates suitable for thin plate metal casting and ingot metal castings. The influence of aerogels on thin wall metal castings was studied by placing aerogel plates into the cavities of thin sections of resin bonded sand molds. An 1 based commercial alloy ( 356) containing 7 percent Si was poured into these molds. Post-solidification studies provide evidence that aerogel inserts significantly reduce the cooling rate during solidification. The advantage of a lower rate using aerogel inserts was reflected in the reduction of casting defects such as shrinkage porosity. Quantitative results support the hypothesis that using aerogels as a mold material can offer definite advantages when used as casting thin sections. As a separate effort, silica aerogel with cylindrical cavities have been prepared and will be evaluated for casting commercial alloys.

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NASA NTRS2003

The Role of Convection and Growth Competition on Phase Selection in Microgravity

For a wide range of compositions, Fe-Cr-Ni alloys can solidify by a two-step process: a metastable solid forms first, subsequently transforming into the stable solid phase. This two-step solidification produces a profoundly different microstructure, and therefore different properties, in the final solid. The delay time between the two steps of the solidification process varies from microseconds to seconds. This delay time is a strong function of composition and a weak function of the undercooling of the melt below the metastable liquidus. From the results obtained during the MSL-1 mission and in ground based electrostatic levitation testing at NASA MSFC, we know that convection also has a significant effect on the delay time. By examining the effect of convection on delay time over a wide range of convection, for several different alloys, we can gain a better understanding and better control of the microstructural evolution and final structure of stainless steel alloys. MSFC provides ESL for ground-based testing in a low-convection state, and the numerical modeling that enables estimation of the convection levels under the different process conditions.

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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

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.↗