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NASA NTRS2003

Toward Understanding Pore Formation and Mobility during Controlled Directional Solidification in a Microgravity Environment Investigation (PFMI)

The generation and inclusion of detrimental porosity, e.g., pipes and rattails can occur during controlled directional solidification processing. The origin of these defects is generally attributed to gas evolution and entrapment during solidification of the melt. On Earth, owing to buoyancy, an initiated bubble can rapidly rise through the liquid melt and pop at the surface; this is obviously not ensured in a low gravity or microgravity environment. Clearly, porosity generation and inclusion is detrimental to conducting any meaningful solidification-science studies in microgravity. Thus it is essential that model experiments be conducted in microgravity, to understand the details of the generation and mobility of porosity, so that methods can be found to eliminate it. In hindsight, this is particularly relevant given the results of the previous directional solidification experiments conducted in Space. The current International Space Station (ISS) Microgravity Science Glovebox (MSG) investigation addresses the central issue of porosity formation and mobility during controlled directional solidification processing in microgravity. The study will be done using a transparent metal-analogue material, succinonitrile (SCN) and succinonitrile-water 'alloys', so that direct observation and recording of pore generation and mobility can be made during the experiments. Succinonitrile is particularly well suited for the proposed investigation because it is transparent, it solidifies in a manner analogous to most metals, it has a convenient melting point, its material properties are well characterized and, it has been successfully used in previous microgravity experiments. The PFMI experiment will be launched on the UF-2, STS-111 flight. Highlighting the porosity development problem in metal alloys during microgravity processing, the poster will describe: (i) the intent of the proposed experiments, (ii) the theoretical rationale behind using SCN as the study material for porosity generation and migration and, (iii) the experimental protocol for the investigation of the effects of the processing parameters. Photographs of the flight experimental hardware, and the novel sample ampoule, will be exhibited. The experimental apparatus will be described in detail and a summary of the scientific objectives will be presented.

Grugel, Richard N.↗
NASA NTRS2003

Pore Formation and Mobility Investigation (PPMI): Description and Initial Analysis of Experiments Conducted aboard the International Space Station

Flow visualization experiments during the controlled directional melt back and re-solidification of succinonitrile (SCN) and SCN-water mixtures were conducted using the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) aboard the International Space Station. The study samples were initially 'cast' on earth under 450 millibar of nitrogen into 1 cm ID glass sample tubes approximately 30 cm in length, containing 6 in situ thermocouples. During the Space experiments, the processing parameters and flow visualization settings are remotely monitored and manipulated from the ground Telescience Center (TSC). The ground solidified 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. Bubbles of different sizes are seen to initiate at the melt interface and, upon release from the melting solid, translate at different speeds in the temperature field ahead of them before coming to rest. Over a period of time these bubbles dissolve into the melt. The gas-laden liquid is then directionally solidified in a controlled manner, generally starting at a rate of 1 micron /sec. Observation and preliminary analysis of bubble formation and mobility in pure SCN samples during melt back and the subsequent structure resulting during gas generation upon re-solidification are presented and discussed.

Grugel, R. N.↗
NASA NTRS2002

Pore Formation and Mobility Investigation (PFMI): Description and Initial Analysis of Experiments Conducted aboard the International Space Station

Flow visualization experiments during the controlled directional melt back and re-solidification of succinonitrile (SCN) and SCN-water mixtures were conducted using the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) aboard the International Space Station. The study samples were initially "cast" on earth under 450 millibar of nitrogen into 1 cm ID glass sample tubes approximately 30 cm in length, containing 6 in situ thermocouples. During the Space experiments, the processing parameters and flow visualization settings are remotely monitored and manipulated from the ground Telescience Center (TSC). The ground solidified 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. Bubbles of different sizes are seen to initiate at the melt interface and, upon release from the melting solid, translate at different speeds in the temperature field ahead of them before coming to rest. Over a period of time these bubbles dissolve into the melt. The gas-laden liquid is then directionally solidified in a controlled manner, generally starting at a rate of 1 micron /sec. Observation and preliminary analysis of bubble formation and mobility in pure SCN samples during melt back and the subsequent structure resulting during gas generation upon re-solidification are presented and discussed.

Grugel, R. N.↗
NASA NTRS2002

Development Of A Novel Discontinuously-Reinforced Aluminum For Space Applications

Discontinuously-reinforced aluminum (DRA) has been used in aerospace structures such as Ventral Fins and Fan Exit Guide Vanes owing to its superior specific stiffness, specific strength, wear resistance, and thermal resistance as compared to the unreinforced aluminum alloys. In order to reduce engine weight, DRA materials are now being considered for space applications. Higher specific strength at ambient and cryogenic temperatures is one of the main requirements in certain rocket applications. The commercial DRA materials use 6xxx and 2xxx precipitation hardened aluminum alloys as matrices which have limited strengths. Therefore, an aluminum alloy which can provide significantly higher ambient and cryogenic strengths is required. In this paper, a novel aluminum alloy based on Al-Sc-X composition with improved ambient and cryogenic temperature strengthening capability is proposed. In addition, this alloy showed promise for improved strength at elevated temperature. The monolithic alloy and the composite with 15 volume percent SiC and B4C particles were processed using a powder metallurgy approach. The influence of processing parameters on the microstructures and mechanical properties of the monolithic and composite materials is discussed. The alloy showed very high strength and moderate ductility. The influence of hydrogen on the properties of monolithic and composite materials is discussed. The thermal stability of these materials is also evaluated. The strength of the material is discussed in terms of solid solution strengthening, Orowan strengthening, and antiphase boundary strengthening models.

Pandey, A. B.↗
NASA NTRS2003

Pore Formation and Mobility Investigation (PFMI): Description and Initial Analysis of Experiments Conducted Aboard the International 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 1D 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 NTRS2003

The Interaction Between an Insoluble Particle and an Advancing Solid/Liquid Interface: Micro-Gravity Experiments and Theoretical Developments

The interaction of an insoluble particle with an advancing solid/liquid interface (SLI) has been a subject of investigation for the past four decades. While the original interest stemmed from geology applications (e.g., frost heaving in soil), researchers soon realized that the complex science associated with such an interaction is relevant to many other scientific fields encompassing metal matrix composites (MMCs), high temperature superconductors, inclusion management in steel, growth of monotectics, and preservation of biological cells. During solidification of a liquid containing an insoluble particle, three distinct interaction phenomena have been experimentally observed: instantaneous engulfment of the particle, continuous pushing, and particle pushing followed by engulfment. It was also observed that for given experimental conditions and particle size there is a critical solidification velocity, V(sub cr), above which a particle is engulfed. During solidification of MMCs pushing leads to particle agglomeration at the grain boundaries and this has detrimental effects on mechanical properties of the casting. Consequently, the process must be designed for instantaneous engulfment to occur. This implies the development of accurate theoretical models to predict V(sub cr), and perform benchmark experiments to test the validity of such models. Although considerable progress has been made in understanding the pushing/engulfment phenomenon (PEP), its quantification in terms of the material and processing parameters remains a focus of research. Since natural convection currents occurring during terrestrial solidification experiments complicate the study of PEP, execution of experiments on the International Space Station (ISS) has been approved and funded by NASA. Extensive terrestrial (1g) experiments and preliminary micro-gravity (mu g) experiments on two space shuttle missions have been conducted in preparation for future experiments on the ISS. The investigated systems included metal-ceramic particles (pure aluminum - zirconia particles) and transparent organic - non-reactive particles (succinonitrile - polystyrene and biphenyl - glass). This paper will discuss the experimental results obtained in both lg and pg conditions and the influence of the natural convection on V(sub cr). A summary of past mathematical models and our recent theoretical developments will also be presented to explain the experimentally observed particle/SLI interaction.

Catalina, Adrian V.↗
NASA NTRS2003

Bubble Formation and Transport during Microgravity Materials Processing: Model Experiments on the International 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 NTRS2003

High Strength Discontinuously Reinforced Aluminum For Rocket Applications

This study presents results on the development of a new aluminum alloy with very high strength and ductility. Five compositions of Al-Mg-Sc-Gd-Zr alloy were selected for this purpose. These alloys were also reinforced with 15 volume percent silicon-carbide and boron-carbide particles to produce Discontinuously Reinforced Aluminum (DRA) materials. Matrix alloys and DRA were processed using a powder metallurgy process. The helium gas atomization produced very fine powder with cellular-dentritic microstructure. The microstructure of matrix alloys showed fine Al3Sc based precipitate which provides significant strengthening in these alloys. DRA showed uniform distribution of reinforcement in aluminum matrix. DRA materials were tested at -320 F, 75 F in air and 7S F in gaseous hydrogen environments and matrix alloys were tested at 75 F in air. DRA showed high strengths in the range of 89-111 ksi (614-697 MPa) depending on alloy compositions and test environments. Matrix alloys had a good combination of strength, 84-89 ksi (579-621 MPa) and ductility, 4.5-6.5%. The properties of these materials can further be improved by proper control of processing parameters.

Pandey, A. B.↗
NASA NTRS2003

Bubble Formation and Transport during Microgravity Materials Processing: Model Experiments on the International 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 NTRS2003

A Dry-Etch Process for Low Temperature Superconducting Transition Edge Sensors for Far Infrared Bolometer Arrays

The next generation of ultra-low power bolometer arrays, with applications in far infrared imaging, spectroscopy and polarimetry, utilizes a superconducting bilayer as the sensing element to enable SQUID multiplexed readout. Superconducting transition edge sensors (TES s) are being produced with dual metal systems of superconductinghormal bilayers. The transition temperature (Tc) is tuned by altering the relative thickness of the superconductor with respect to the normal layer. We are currently investigating MoAu and MoCu bilayers. We have developed a dry-etching process for MoAu TES s with integrated molybdenum leads, and are working on adapting the process to MoCu. Dry etching has the advantage over wet etching in the MoAu system in that one can achieve a high degree of selectivity, greater than 10, using argon ME, or argon ion milling, for patterning gold on molybdenum. Molybdenum leads are subsequently patterned using fluorine plasma.. The dry-etch technique results in a smooth, featureless TES with sharp sidewalls, no undercutting of the Mo beneath the normal metal, and Mo leads with high critical current. The effects of individual processing parameters on the characteristics of the transition will be reported.

Allen, Christine A.↗
NASA NTRS2003

2XXX Aluminum Self Reacting Friction Stir Weld Development

Weld process development are: (1) Execute a two-phased design of experiment (DOE) approach: process DOE to establish rotation and travel speeds and forge load;set-up DOE to establish allowable gap and centerline offset. (2) Determine the effect of process parameters on strength and weld quality: room and -320 deg F tensile testing; metalllurgical and NDE evaluation. (3) Weld quality goals: visual and radiographic acceptable; room temperature ultimate strength.

Brown, Randy J.↗
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

Direct Observation of Controlled Melting and Resolidification of Succinonitrile Mixtures in a Microgravity Environment

In support of the Pore Formation and Mobility Investigation (PFMI) direct observation of experiments on the controlled melting and subsequent resolidification of succinonitrile were conducted in the glovebox facility (GBX) of the International Space Station (ISS). Samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with pure succinonitrile (SCN) and SCN-Water mixtures under 450 millibar of nitrogen. 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. Sample temperatures are monitored by six in situ thermocouples. Real time visualization during melt back revealed bubbles of different sizes initiating at the solid/liquid interface, their release, interactions, and movement into the temperature field ahead of them. Subsequent re-solidification examined planar interface breakdown and the transition to steady-state dendritic growth. A preliminary analysis of the observed phenomena 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 NTRS2002

Plasma-enhanced chemical vapor deposition of multiwalled carbon nanofibers

Plasma-enhanced chemical vapor deposition is used to grow vertically aligned multiwalled carbon nanofibers (MWNFs). The graphite basal planes in these nanofibers are not parallel as in nanotubes; instead they exhibit a small angle resembling a stacked cone arrangement. A parametric study with varying process parameters such as growth temperature, feedstock composition, and substrate power has been conducted, and these parameters are found to influence the growth rate, diameter, and morphology. The well-aligned MWNFs are suitable for fabricating electrode systems in sensor and device development.

Nanotechnology/instrumentation/methods↗
NASA NTRS1986

Cost Risk Analysis Based on Perception of the Engineering Process

In most cost estimating applications at the NASA Langley Research Center (LaRC), it is desirable to present predicted cost as a range of possible costs rather than a single predicted cost. A cost risk analysis generates a range of cost for a project and assigns a probability level to each cost value in the range. Constructing a cost risk curve requires a good estimate of the expected cost of a project. It must also include a good estimate of expected variance of the cost. Many cost risk analyses are based upon an expert's knowledge of the cost of similar projects in the past. In a common scenario, a manager or engineer, asked to estimate the cost of a project in his area of expertise, will gather historical cost data from a similar completed project. The cost of the completed project is adjusted using the perceived technical and economic differences between the two projects. This allows errors from at least three sources. The historical cost data may be in error by some unknown amount. The managers' evaluation of the new project and its similarity to the old project may be in error. The factors used to adjust the cost of the old project may not correctly reflect the differences. Some risk analyses are based on untested hypotheses about the form of the statistical distribution that underlies the distribution of possible cost. The usual problem is not just to come up with an estimate of the cost of a project, but to predict the range of values into which the cost may fall and with what level of confidence the prediction is made. Risk analysis techniques that assume the shape of the underlying cost distribution and derive the risk curve from a single estimate plus and minus some amount usually fail to take into account the actual magnitude of the uncertainty in cost due to technical factors in the project itself. This paper addresses a cost risk method that is based on parametric estimates of the technical factors involved in the project being costed. The engineering process parameters are elicited from the engineer/expert on the project and are based on that expert's technical knowledge. These are converted by a parametric cost model into a cost estimate. The method discussed makes no assumptions about the distribution underlying the distribution of possible costs, and is not tied to the analysis of previous projects, except through the expert calibrations performed by the parametric cost analyst.

Dean, Edwin B.↗
NASA NTRS2004

Computer Tomography 3-D Imaging of the Metal Deformation Flow Path in Friction Stir Welding

In friction stir welding, a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. This solid-state technique has been successfully used in the joining of materials that are difficult to fusion weld such as aluminum alloys. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path is required. Marker studies are the principal method of studying the metal deformation flow path around the FSW pin tool. In our study, we have used computed tomography (CT) scans to reveal the flow pattern of a lead wire embedded in a FSW weld seam. At the welding temperature of aluminum, the lead becomes molten and thus tracks the aluminum deformation flow paths in a unique 3-dimensional manner. CT scanning is a convenient and comprehensive way of collecting and displaying tracer data. It marks an advance over previous more tedious and ambiguous radiographic/metallographic data collection methods.

Schneider, Judy↗
NASA NTRS2005

Low Conductive Thermal Barrier Coatings Produced by Ion Beam Assisted EB-PVD with Controlled Porosity, Microstructure Refinement and Alloying Additions for High Temperature Applications

Various advanced Hafnia-based thermal barrier coatings (TBC) were applied on nickel-based superalloy coupons by electron beam physical vapor deposition. In addition, microstructural modifications to the coating material were made in an effort to reduce the thermal conductivity of the coating materials. Various processing parameters and coating system modifications were made in order to deposit the alloyed TBC with the desired microstructure and thus coating performance, some of which include applying coatings at substrate temperatures of 1150 C on both PtAl and CoNiCrAlY bond coated samples, as well as using 8YSZ as a bond layer. In addition, various characterization techniques including thermal cyclic tests, scanning electron microscopy, x-ray diffraction, thermal conductivity, and reflectivity measurements were performed. Although the coating microstructure was never fully optimized due to funding being cut short, significant reductions in thermal conductivity were accomplished through both chemistry changes (composition) and microstructural modifications.

Wolfe, Douglas E.↗