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NASA NTRS2005

Morphological Evolution of Directional Solidification Interfaces in Microgravity: An Analysis of Model Experiments Performed on the International Space Station

A series of experiments performed using the Pore Formation and Mobility Investigation (PFMI) apparatus within the glovebox facility (GBX) on board the International Space Station (ISS) has provided video images of the morphological evolution of a three-dimensional interface in a diffusion controlled regime. The experimental samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with "alloys" of succinonitrile (SCN) and water in an atmosphere of nitrogen at 450 millibar pressure. The compositions of the samples processed and analyzed are 0.25,0.5 and 1.0 wt% water. 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 !3pace Flight Center. During the experiments, the sample was first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. Following the melt back, the interface was allowed to stabilize before translation is initiated. The temperatures in the sample were monitored by six in situ thermocouples and the position is monitored by an optical linear encoder. For the experiments performed and analyzed, the gradients ranged from 2.5 - 3.3 K/mm and the initial pulling velocities ranged from 0.7 micron per second to 1 micron per second with subsequent transition velocities of up to 100 microns per second. The data provided by the PFMI for analysis includes near-real-time (NRT) video captured on the ground during the experiment runs, ISS Video Tape Recorder (VTR) data dumped from the VTR at the end of the experiment run and recorded on the ground, telemetry data including temperature and position measurements, and limited flight HI-8 tapes in 2 camera views of experiment runs for which tapes have been returned to the investigators from ISS. Because of limited down mass from the ISS, the majority of the initial analysis has been performed using the NRT and VTR video data but will be supplemented with the HI-8 video as it becomes available. hardware and procedures required to prepare samples for correlation to flight samples is described. Using this ground-based system, a series of experiments have been performed for direct comparison with the flight data. The results of these comparisons as well as implications to future microgravity experiments are presented and discussed. A ground-based thin-sample directional solidification system as well as all associated

Strutzenberg, Louise L.↗

NASA NTRS2005

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

In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. 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 is carried with the macro-flow of the weld metal. By using CT images, a 3-dimensional (3D) image of the lead flow pattern can be reconstructed. CT imaging was found to be 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 NTRS2004

Advanced SiC/SiC Ceramic Composites For Gas-Turbine Engine Components

NASA Glenn Research Center (GRC) is developing a variety of advanced SiC/SiC ceramic composite (ASC) systems that allow these materials to operate for hundreds of hours under stress in air at temperatures approaching 2700 F. These SiC/SiC composite systems are lightweight (approximately 30% metal density) and, in comparison to monolithic ceramics and carbon fiber-reinforced ceramic composites, are able to reliably retain their structural properties for long times under aggressive gas-turbine engine environments. The key for the ASC systems is related first to the NASA development of the Sylramic-iBN Sic fiber, which displays higher thermal stability than any other SiC- based ceramic fibers and possesses an in-situ grown BN surface layer for higher environmental durability. This fiber is simply derived from Sylramic Sic fiber type that is currently produced at ATK COI Ceramics (COIC). Further capability is then derived by using chemical vapor infiltration (CVI) and/or polymer infiltration and pyrolysis (PIP) to form a Sic-based matrix with high creep and rupture resistance as well as high thermal conductivity. The objectives of this study were (1) to optimize the constituents and processing parameters for a Sylramic-iBN fiber reinforced ceramic composite system in which the Sic-based matrix is formed at COIC almost entirely by PIP (full PIP approach), (2) to evaluate the properties of this system in comparison to other 2700 F Sylramic-iBN systems in which the matrix is formed by full CVI and CVI + PIP, and (3) to examine the pros and cons of the full PIP approach for fabricating hot-section engine components. A key goal is the development of a composite system with low porosity, thereby providing high modulus, high matrix cracking strength, high interlaminar strength, and high thermal conductivity, a major property requirement for engine components that will experience high thermal gradients during service. Other key composite property goals are demonstration at high temperatures of high environmental resistance and high creep resistance, which in turn will result in long component life. Data are presented from a variety of laboratory tests on simple two-dimensional panels that examine these properties and compare the performance of the optimized full PIP system with those of the full CVI and CVI + PIP hybrid systems. Underlying mechanisms for performance differences in the various systems are discussed. Remaining issues for further property enhancement and for application of the full PIP approach for engine components are also discussed, as well as on-going approaches at NASA to solve these issues.

H. M. Yun↗

NASA NTRS2005

Tracing Material Flow Paths in Friction Stir Welds

Heat and mechanical work are coupled in the friction stir welding process. The process variables are RPM, translational weld speed, and downward plunge force. The strain-temperature history of a metal element at each point on the cross-section of the weld is determined by the process variables plus the individual flow path taken by the particular filament of metal flowing around the tool and ending on flat point. The strain-temperature history determines the properties of a metal element on the weld cross-section. The strain-temperature history is carefully controlled in metal processes where direct control is feasible. Indirect estimates of the flow paths and the strain-temperature histories of filaments comprising friction stir welds can be made from a model, if the model is good enough. This paper describes marker studies of flow path geometries for various process parameters. Observed geometries are compared with geometries estimated from models.

Sanders, Johnny↗

NASA NTRS2006

Evolution and Control of 2219 Aluminum Microstructural Features Through Electron Beam Freeform Fabrication

The layer-additive nature of the electron beam freeform fabrication (EBF3) process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

NASA NTRS2006

Development of Laser Fabricated Ti-6Al-4V

Laser Engineered Net Shaping (LENS) depositions with Ti-6Al-4V gas-atomized powder were accomplished at five different temperatures, ranging from 30 to 400 C, imposed on the base plate. These base plate temperatures were employed in an effort to relieve stresses which develop during the deposition. Warpage of the base plate was monitored. Only a slight decline in warpage was observed as the base plate temperature was increased. Results indicate that substrate temperatures closer to the stress relief minimum of 480 C would relieve deposition stresses, though process parameters would likely need to be modified to compensate for the higher base plate temperature. The compositions of the as-received powder and the LENS deposited material were chemically analyzed. The oxygen content of the LENS material was 0.154 wt.% which is less than the maximum impurity limit of 0.2 percent for commercial Ti-6Al-4V alloys, but is over the limit allowed in ELI grade (0.13 percent). The level of oxygen in the commercial base plate used was only 0.0635 percent. Tensile specimens were machined from the LENS deposited material and tested in tension at room temperature. The ultimate and yield tensile stresses of the LENS material were about 1200 and 1150 MPa respectively, which is about 20 percent higher than the strengths of wrought Ti-6Al-4V. The higher strength of the LENS material was due to its fine structure and high oxygen content. The LENS deposits were not fully dense; voids were frequent at the interfaces between deposited layers. These dispersed sheets of voids were parallel to the longitudinal axis of the resulting tensile specimens. Apparently there was sufficient continuous, fully dense material longitudinally to enable the high strengths. Ductility was low in the LENS material. Percent elongation at failure in the LENS material was near 4 percent, which is less than half of what is usually expected from Ti-6Al-4V. The low ductility was caused by high oxygen levels, and the presence of voids. It is likely that the relatively high scan speeds used in our depositions contributed to the lack of full density in our LENS material.

deGroh, Henry C., III↗

NASA NTRS2006

Aerosol-Assisted Chemical Vapor Deposited Thin Films for Space Photovoltaics

Copper indium disulfide thin films were deposited via aerosol-assisted chemical vapor deposition using single source precursors. Processing and post-processing parameters were varied in order to modify morphology, stoichiometry, crystallography, electrical properties, and optical properties in order to optimize device-quality material. Growth at atmospheric pressure in a horizontal hot-wall reactor at 395 C yielded best device films. Placing the susceptor closer to the evaporation zone and flowing a more precursor-rich carrier gas through the reactor yielded shinier, smoother, denser-looking films. Growth of (112)-oriented films yielded more Cu-rich films with fewer secondary phases than growth of (204)/(220)-oriented films. Post-deposition sulfur-vapor annealing enhanced stoichiometry and crystallinity of the films. Photoluminescence studies revealed four major emission bands (1.45, 1.43, 1.37, and 1.32 eV) and a broad band associated with deep defects. The highest device efficiency for an aerosol-assisted chemical vapor deposited cell was 1.03 percent.

Hepp, Aloysius F.↗

NASA NTRS2006

Structural and Radiation Shielding Properties of a Martian Habitat Material Synthesized From In-Situ Resources

The 2 primary requirements of a Martian habitat structure include sufficient structural integrity and effective radiation shielding. In addition, the capability to synthesize such building materials primarily from in-situ resources would significantly reduce the cost associated with transportation of such materials and structures from earth. To demonstrate the feasibility of such an approach we have fabricated samples in the laboratory using simulated in-situ resources, evaluated radiation shielding effectiveness using radiation transport codes and radiation test data, and conducted mechanical properties testing. In this paper we will present experimental results that demonstrate the synthesis of polyethylene from a simulated Martian atmosphere and the fabrication of a composite material using simulated Martian regolith with polyethylene as the binding material. Results from radiation transport calculations and data from laboratory radiation testing using a 500 MeV/nucleon Fe beam will be discussed. Mechanical properties of the proposed composite as a function of composition and processing parameters will also be presented.

Sen, S.↗

NASA NTRS2006

A Rotating Plug Model of Friction Stir Welding Heat Transfer

A simplified rotating plug model is employed to study the heat transfer phenomena associated with the fiction stir welding process. An approximate analytical solution is obtained based on this idealized model and used both to demonstrate the qualitative influence of process parameters on predictions and to estimate temperatures produced in typical fiction stir welding situations.

Raghulapadu J. K.↗

NASA NTRS2006

Evolution and Control of 2219 Aluminum Microstructural Features through Electron Beam Freeform Fabrication

Electron beam freeform fabrication (EBF3) is a new layer-additive process that has been developed for near-net shape fabrication of complex structures. EBF3 uses an electron beam to create a molten pool on the surface of a substrate. Wire is fed into the molten pool and the part translated with respect to the beam to build up a 3-dimensional structure one layer at a time. Unlike many other freeform fabrication processes, the energy coupling of the electron beam is extremely well suited to processing of aluminum alloys. The layer-additive nature of the EBF3 process results in a tortuous thermal path producing complex microstructures including: small homogeneous equiaxed grains; dendritic growth contained within larger grains; and/or pervasive dendritic formation in the interpass regions of the deposits. Several process control variables contribute to the formation of these different microstructures, including translation speed, wire feed rate, beam current and accelerating voltage. In electron beam processing, higher accelerating voltages embed the energy deeper below the surface of the substrate. Two EBF3 systems have been established at NASA Langley, one with a low-voltage (10-30kV) and the other a high-voltage (30-60 kV) electron beam gun. Aluminum alloy 2219 was processed over a range of different variables to explore the design space and correlate the resultant microstructures with the processing parameters. This report is specifically exploring the impact of accelerating voltage. Of particular interest is correlating energy to the resultant material characteristics to determine the potential of achieving microstructural control through precise management of the heat flux and cooling rates during deposition.

Taminger, Karen M.↗

NASA NTRS2008

Air Flow and Pressure Drop Measurements Across Porous Oxides

This report summarizes the results of air flow tests across eight porous, open cell ceramic oxide samples. During ceramic specimen processing, the porosity was formed using the sacrificial template technique, with two different sizes of polystyrene beads used for the template. The samples were initially supplied with thicknesses ranging from 0.14 to 0.20 in. (0.35 to 0.50 cm) and nonuniform backside morphology (some areas dense, some porous). Samples were therefore ground to a thickness of 0.12 to 0.14 in. (0.30 to 0.35 cm) using dry 120 grit SiC paper. Pressure drop versus air flow is reported. Comparisons of samples with thickness variations are made, as are pressure drop estimates. As the density of the ceramic material increases the maximum corrected flow decreases rapidly. Future sample sets should be supplied with samples of similar thickness and having uniform surface morphology. This would allow a more consistent determination of air flow versus processing parameters and the resulting porosity size and distribution.

Fox, Dennis S.↗

NASA NTRS2007

Structure-Property Relationships in Porous 3-D Nanostructures as a Function of Preparation Conditions: Isocyanate Cross-Linked Silica Aerogels

Sol-gel derived silica aerogels are attractive candidates for many unique thermal, optical, catalytic, and chemical applications because of their low density and high mesoporosity. However, their inherent fragility has restricted use of aerogel monoliths to applications where they are not subject to any load. We have previously reported cross-linking the mesoporous silica structure of aerogels with di-isocyanates, styrenes or epoxies reacting with amine decorated silica surfaces. These approaches have been shown to significantly increase the strength of aerogels with only a small effect on density or porosity. Though density is a prime predictor of properties such as strength and thermal conductivity for aerogels, it is becoming clear from previous studies that varying the silica backbone and size of the polymer cross-link independently can give rise to combinations of properties which cannot be predicted from density alone. Herein, we examine the effects of four processing parameters for producing this type of polymer cross-linked aerogel on properties of the resulting monoliths. We focus on the results of C-13 CP-MAS NMR which gives insight to the size and structure of polymer cross-link present in the monoliths, and relates the size of the cross-links to microstructure, mechanical properties and other characteristics of the materials obtained.

Meador, Mary Ann B.↗

NASA NTRS2008

Spray Chemical Vapor Deposition of Single-Source Precursors for Chalcopyrite I-III-VI2 Thin-Film Materials

Thin-film solar cells on flexible, lightweight, space-qualified substrates provide an attractive approach to fabricating solar arrays with high mass-specific power. A polycrystalline chalcopyrite absorber layer is among the new generation of photovoltaic device technologies for thin film solar cells. At NASA Glenn Research Center we have focused on the development of new single-source precursors (SSPs) for deposition of semiconducting chalcopyrite materials onto lightweight, flexible substrates. We describe the syntheses and thermal modulation of SSPs via molecular engineering. Copper indium disulfide and related thin-film materials were deposited via aerosol-assisted chemical vapor deposition using SSPs. Processing and post-processing parameters were varied in order to modify morphology, stoichiometry, crystallography, electrical properties, and optical properties to optimize device quality. Growth at atmospheric pressure in a horizontal hotwall reactor at 395 C yielded the best device films. Placing the susceptor closer to the evaporation zone and flowing a more precursor-rich carrier gas through the reactor yielded shinier-, smoother-, and denser-looking films. Growth of (112)-oriented films yielded more Cu-rich films with fewer secondary phases than growth of (204)/(220)-oriented films. Post-deposition sulfur-vapor annealing enhanced stoichiometry and crystallinity of the films. Photoluminescence studies revealed four major emission bands and a broad band associated with deep defects. The highest device efficiency for an aerosol-assisted chemical vapor deposited cell was one percent.

Hepp, Aloysius F.↗

NASA NTRS2008

High Temperature Aerogels in the Al2O3-SiO2 System

Al2O3-SiO2 aerogels are of interest as constituents of thermal insulation systems for use at high temperatures. Al2O3 and mullite aerogels are expected to crystallize at higher temperatures than their SiO2 counterparts, hence avoiding the shrinkages that accompany the formation of lower temperature SiO2 phases and preserving pore structures into higher temperature regimes. The objective of this work is to determine the influence of processing parameters on shrinkage, gel structure (including surface area, pore size and distribution) and pyrolysis behavior.

Hurwitz, Frances I.↗

NASA NTRS2008

Microstructural Evolution in Friction Stir Welding of Ti-6Al-4V

Friction stir welding (FSW) is a thermo-mechanical process that utilizes a nonconsumable rotating pin tool to consolidate a weld joint. In the conventional FSW process, the pin tool is responsible for generating both the heat required to soften the material and the forces necessary to deform and combine the weld seam. As such, the geometry of the pin tool is important to the quality of the weld and the process parameters required to produce the weld. Because the geometry of the pin tool is limitless, a reduced set of pin tools was formed to systematically study their effect on the weldment with respect to mechanical properties and resultant microstructure. In this study 0deg, 15deg, 30deg, 45deg, and 60deg tapered, microwave sintered, tungsten carbide (WC) pin tools were used to FSW Ti-6Al-4V. Transverse sections of the weld were used to test for mechanical properties and to document the microstructure using optical microscopy. X-ray diffraction (XRD) was also used to characterize the microstructure in the welds. FSW results for the 45deg and 60deg pin tools are reported in this paper.

Rubisoff, H.↗

NASA NTRS2009

Pin Tool Geometry Effects in Friction Stir Welding

In friction stir welding (FSW) there is significant evidence that material can take one of two different flow paths when being displaced from its original position in front of the pin tool to its final position in the wake of the weld. The geometry of the pin tool, along with the process parameters, plays an important role in dictating the path that the material takes. Each flow path will impart a different thermomechanical history on the material, consequently altering the material microstructure and subsequent weld properties. The intention of this research is to isolate the effect that different pin tool attributes have on the flow paths imparted on the FSWed material. Based on published weld tool geometries, a variety of weld tools were fabricated and used to join AA2219. Results from the tensile properties and microstructural characterization will be presented.

Querin, J. A.↗

NASA NTRS2009

Bond Assembly FOD Zones - A Procedure for Assuring Acceptable Adhesion

Rocket motor components are primarily assembled by adhesion. a) For example, the RSRM (Reusable Solid Rocket Motor - part of the Space Shuttle Boosters) system contains 10,000 sq ft of bondline area. b) Rocket motors contain a variety of adhesive/substrate bond systems c) Bond system performance requirements also vary. To assemble reliable components, ATK Space Systems and customers invest substantial resources to the study of bond assembly processes. a) Surface and adhesion science; b) Adhesive chemistry; c) Process parameters; d) Contamination effects.

Evans, Kurt↗

NASA NTRS2007

Manufacturing Large Membrane Mirrors at Low Cost

Relatively inexpensive processes have been developed for manufacturing lightweight, wide-aperture mirrors that consist mainly of reflectively coated, edge-supported polyimide membranes. The polyimide and other materials in these mirrors can withstand the environment of outer space, and the mirrors have other characteristics that make them attractive for use on Earth as well as in outer space: With respect to the smoothness of their surfaces and the accuracy with which they retain their shapes, these mirrors approach the optical quality of heavier, more expensive conventional mirrors. Unlike conventional mirrors, these mirrors can be stowed compactly and later deployed to their full sizes. In typical cases, deployment would be effected by inflation. Potential terrestrial and outer-space applications for these mirrors include large astronomical telescopes, solar concentrators for generating electric power and thermal power, and microwave reflectors for communication, radar, and short-distance transmission of electric power. The relatively low cost of manufacturing these mirrors stems, in part, from the use of inexpensive tooling. Unlike in the manufacture of conventional mirrors, there is no need for mandrels or molds that have highly precise surface figures and highly polished surfaces. The surface smoothness is an inherent property of a polyimide film. The shaped area of the film is never placed in contact with a mold or mandrel surface: Instead the shape of a mirror is determined by a combination of (1) the shape of a fixture that holds the film around its edge and (2) control of manufacturing- process parameters. In a demonstration of this manufacturing concept, spherical mirrors having aperture diameters of 0.5 and 1.0 m were fabricated from polyimide films having thicknesses ranging from <20 m to 150 m. These mirrors have been found to maintain their preformed shapes following deployment.

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