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NASA NTRS1995

X-ray transmission microscope development

This report covers the third 6 month period, from February 28, 1995 to August 31, 1995, under this contract. The main efforts during this period were the construction of the X-ray furnace, evaluation and selection of the CCD technology for the X-ray camera, solidification experiments with Al alloys and Al-zirconia composites in the prototype furnace, evaluation of specimens for the particle pushing flight experiment - PEPSI, measurements of emitted spectra from X-ray source, testing of the high resolution X-ray test targets, and the establishment of criteria for and selection of peripheral equipment. In addition to these tasks, two presentations were prepared in this period; one for the AIAA Microgravity Symposium and another for the Gordon Conference on Gravitational Effects in Pyisico-Chemical Systems.

Kaukler, William F.↗

NASA NTRS1995

Construction material processed using lunar simulant in various environments

The manufacture of construction materials from locally available resources in space is an important first step in the establishment of lunar and planetary bases. The objective of the CoMPULSIVE (Construction Material Processed Using Lunar Simulant In Various Environments) experiment is to develop a procedure to produce construction materials by sintering or melting Johnson Space Center Simulant 1 (JSC-1) lunar soil simulant in both earth-based (1-g) and microgravity (approximately 0-g) environments. The characteristics of the resultant materials will be tested to determine its physical and mechanical properties. The physical characteristics include: crystalline, thermal, and electrical properties. The mechanical properties include: compressive tensile, and flexural strengths. The simulant, placed in a sealed graphite crucible, will be heated using a high temperature furnace. The crucible will then be cooled by radiative and forced convective means. The core furnace element consists of space qualified quartz-halogen incandescent lamps with focusing mirrors. Sample temperatures of up to 2200 C are attainable using this heating method.

Chase, Stan↗

NASA NTRS1995

Investigation of Advanced Processed Single-Crystal Turbine Blade Alloys

This investigation studied the influence of thermal processing and microstructure on the mechanical properties of the single-crystal, nickel-based superalloys PWA 1482 and PWA 1484. The objective of the program was to develop an improved single-crystal turbine blade alloy that is specifically tailored for use in hydrogen fueled rocket engine turbopumps. High-gradient casting, hot isostatic pressing (HIP), and alternate heat treatment (HT) processing parameters were developed to produce pore-free, eutectic-free microstructures with different (gamma)' precipitate morphologies. Test materials were cast in high thermal gradient solidification (greater than 30 C/cm (137 F/in.)) casting furnaces for reduced dendrite arm spacing, improved chemical homogeneity, and reduced interdendritic pore size. The HIP processing was conducted in 40 cm (15.7 in.) diameter production furnaces using a set of parameters selected from a trial matrix study. Metallography was conducted on test samples taken from each respective trial run to characterize the as-HIP microstructure. Post-HIP alternate HT processes were developed for each of the two alloys. The goal of the alternate HT processing was to fully solution the eutectic gamma/(gamma)' phase islands and to develop a series of modified (gamma)' morphologies for subsequent characterization testing. This was accomplished by slow cooling through the (gamma)' solvus at controlled rates to precipitate volume fractions of large (gamma)'. Post-solution alternate HT parameters were established for each alloy providing additional volume fractions of finer precipitates. Screening tests included tensile, high-cycle fatigue (HCF), smooth and notched low-cycle fatigue (LCF), creep, and fatigue crack growth evaluations performed in air and high pressure (34.5 MPa (5 ksi)) hydrogen at room and elevated temperature. Under the most severe embrittling conditions (HCF and smooth and notched LCF in 34.5 MPa (5 ksi) hydrogen at 20 C (68 F), screening test results showed increases in fatigue life typically on the order of 1OX, when compared to the current Space Shuttle Main Engine (SSME) Alternate Turbopump (AT) blade alloy (PWA 1480).

Peters, B. J.↗

NASA NTRS1995

The origin of the solar wind

The high speed solar wind, which is associated with coronal holes and unipolar interplanetary magnetic field, has now been observed in situ beyond 0.3 a.u. and at latitudes up to 80 degrees. Its important characteristics are that it is remarkably steady in terms of flow properties and composition and that the ions, especially minor species, are favored in terms of heating and acceleration. We have proposed that the high speed wind, with its associated coronal holes, forms the basic mode of solar wind flow. In contrast, the low speed wind is inherently non-stationary, filamentary and not in equilibrium with conditions at the coronal base. It is presumably the result of continual reconfigurations of the force-free magnetic field in the low-latitude closed corona which allow trapped plasma to drain away along transiently open flux tubes. Observations of high speed solar wind close to its source are hampered by the essential heterogeneity of the corona, even at sunspot minimum. In particular it is difficult to determine more than limits to the density, temperature and wave amplitude near the coronal base as a result of contamination from fore- and back-ground plasma. We interpret the observations as indicating that the high speed solar wind originates in the chromospheric network, covering only about 1% of the surface of the sun, where the magnetic field is complex and not unipolar. As a result of small-scale reconnection events in this 'furnace', Alfven waves are generated with a flat spectrum covering the approximate range 10 kHz to 10 Hz. The plasma is likely to be produced as a result of downwards thermal conduction and possibly photoionization at the top of the low density chromospheric interface to the furnace, thus controlling the mass flux in the wind. The immediate source of free (magnetic) energy is in the form of granule-sized loops which are continually carried into the network from the sides. The resulting wave spectrum is such that energy can be efficiently transferred to the ions within a few solar radii of the base of the corona, favoring heavy species and creating stable, fast solar wind.

Axford, W. I.↗

NASA NTRS1996

Parabolic aircraft solidification experiments

A number of solidification experiments have been utilized throughout the Materials Processing in Space Program to provide an experimental environment which minimizes variables in solidification experiments. Two techniques of interest are directional solidification and isothermal casting. Because of the wide-spread use of these experimental techniques in space-based research, several MSAD experiments have been manifested for space flight. In addition to the microstructural analysis for interpretation of the experimental results from previous work with parabolic flights, it has become apparent that a better understanding of the phenomena occurring during solidification can be better understood if direct visualization of the solidification interface were possible. Our university has performed in several experimental studies such as this in recent years. The most recent was in visualizing the effect of convective flow phenomena on the KC-135 and prior to that were several successive contracts to perform directional solidification and isothermal casting experiments on the KC-135. Included in this work was the modification and utilization of the Convective Flow Analyzer (CFA), the Aircraft Isothermal Casting Furnace (ICF), and the Three-Zone Directional Solidification Furnace. These studies have contributed heavily to the mission of the Microgravity Science and Applications' Materials Science Program.

Workman, Gary L.↗

NASA NTRS1997

Potential New Sensor for Use With Conventional Gas Carburizing

Diagnostics developed for in-situ monitoring of rocket combustion environments have been adapted for use in heat treating furnaces. Simultaneous, in-situ monitoring of the carbon monoxide, carbon dioxide, methane, water, nitrogen and hydrogen concentrations in the endothermic gas of a heat treating furnace has been demonstrated under a Space Act Agreement between NASA Lewis, the Heat Treating Network, and Akron Steel Treating Company. Equipment installed at the Akron Steel Treating Company showed the feasibility of the method. Clear and well-defined spectra of carbon monoxide, nitrogen and hydrogen were obtained by means of an optical probe mounted on the endothermic gas line of a gas generator inside the plant, with the data reduction hardware located in the basement laboratory. Signals to and from the probe were transmitted via optical fibers.

deGroot, W. A.↗

NASA NTRS1997

Gravitational Effects in Smoldering and SHS

Bernard J Matkowsky↗

NASA NTRS1993

Bulk Growth of 2-6 Crystals in the Microgravity Environment of USML-1

The first United States Microgravity Laboratory Mission (USML- 1) flew in June 1992 on the Space Shuttle Columbia. An important part of this SpaceLab mission was the debut of the Crystal Growth Furnace (CGF). Of the seven samples grown in the furnace, three were bulk grown 2-6 compounds, two of a cadmium zinc telluride alloy, and one of a mercury zinc telluride alloy. Ground based results are presented, together with the results of computer simulated growths of these experimental conditions. Preliminary characterization results for the three USML-1 growth runs are also presented and the flight sample characteristics are compared to the equivalent ground truth samples. Of particular interest are the effect of the containment vessel on surface features, and especially on the nucleation, and the effect of the gravity vector on radial and axial compositional variations and stress and defect levels.

Gillies, Donald C.↗

NASA NTRS1997

Effects of Experiment Location and Orbiter Attitude on the Residual Acceleration On-Board STS-73 (USML-2)

A knowledge of the quasi-steady acceleration environment on the NASA Space Shuttle Orbiter is of particular importance for materials processing experiments which are limited by slow diffusive processes. The quasi-steady (less than 1 HZ) acceleration environment on STS-73 (USML-2) was measured using the Orbital Acceleration Research Experiment (OARE) accelerometer. One of the facilities flown on USML-2 was the Crystal Growth Furnace (CGF), which was used by several Principal Investigators (PIS) to grow crystals. In this paper the OARE data mapped to the sample melt location within this furnace is presented. The ratio of the axial to radial components of the quasi-steady acceleration at the melt site is presented. Effects of Orbiter attitude on the acceleration data is discussed.

Hakimzadeh, Roshanak↗

NASA NTRS1997

Regolith Evolved Gas Analyzer (REGA)

The instrument consists of five subsystems: (1) a programmable furnace which can be loaded with samples of regolith, (2) a mass spectrometer which detects and measures atmospheric gases or gases evolved during heating, (3) a tank of pressurized gas which can be introduced to the regolith material while detecting and measuring volatile reaction products, (4) a mechanism for dumping the regolith sample and repeating the experiment on a fresh sample, and (5) a data system which controls and monitors the furnace, gas system, and mass spectrometer.

Allen, Carlton C.↗

NASA NTRS1995

STS-94 Day 09 Highlights

On this ninth day of the STS-94 mission, the flight crew, Cmdr. James D. Halsell, Jr., Pilot Susan L. Still, Payload Cmdr. Janice E. Voss, Mission Specialists Michael L. Gernhardt and Donald A. Thomas, and Payload Specialists Gregory T. Linteris and Roger K. Crouch spend their morning in the Spacelab module working on several experiments. Thomas has been working with the Large Isothermal Furnace (LIF), a vacuum-heating furnace designed to heat large samples uniformly; the Middeck Glovebox (MGBX) unit; and the Internal Flows in a Free Drop Experiment (IFFD). The IFFD experiment involves containerless processing of materials using acoustic positioning techniques.

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NASA NTRS1997

Evaluation of Optimum HgZnTe Crystal Growth Parameters and USML-2 Flight Support

Work associated with contract provided support for the approved flight experiment 'Crystal Growth of Selected 2-6 Semiconducting Alloys by Directional Solidification.' General activities included ground-based melt studies, compositional and microstructure characterization of the grown crystals, and participation in the continuing assessment of the program. Specifically, work was performed to determine the optimum furnace translation rate at which a HgZnTe sample could be removed from the crystal growth furnace to avoid shrinkage cavities. Additionally, nine HgZnTe ampoules were prepared and delivered to Marshall Space Flight Center for Ground Control Experiment Laboratory Testing.

Scripa, Rosalia N.↗

NASA NTRS1998

Development of Advanced Multizone Facilities for Microgravity Processing

NASA has been interested in experimental ground based study to investigate the fundamental processes involved in phase transformation processes during growth of metallic, nonmetallic and electronic materials. Solidification, vapor growth and solution growth techniques of growing crystals are of special interest because of the inherent importance of convection in the nutrient solution. Convection enhances the mass transport through the nutrient and results in faster growth rates. Availability of low gravity environment of space has provided scientists a new variable to control the extent of convection and thus isolate the diffusive phenomena for their better understanding. The thermal gradient at the liquid-solid interface is determined by the alloy characteristics, the hot zone temperature, cold zone temperature and the width of the insulating zone. The thermal profiles get established by the existing material and geometrical constraints of the experimental set up. The major effort under this research was devoted to designing a programmable furnace which can be used to obtain thermal profiles along the length of the sample as per the demands of the scientists. The furnace did not have active cooling of the zones. Only active heating and passive cooling were utilized.

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NASA NTRS1998

High Temperature Mechanical Characterization of Ceramic Matrix Composites

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Gyekenyesi, John Z.↗

NASA NTRS1998

The Effect of Microgravity Direction on the Growth of PbSnTe

The Space Shuttle Columbia was launched as STS-75 at 2018 GMT (Greenwich Mean Time) on February 22, 1996. One of the two major experiment packages was the Third United States Microgravity Payload (USMP-3), and one of the principal instruments on the USMP was the Advanced Automated Directional Solidification Furnace (AADSF). The AADSF is a multizone directional solidification furnace, and at the time of the USMP-3 flight was capable of processing only one sample per Shuttle mission which, for that flight, was a lead tin telluride (PbSnTe) crystal growth experiment. In the one year since the flight experiment the sample has been retrieved from the spacecraft and analysis has begun. After presenting introductory material on why PbSnTe was chosen as a test material, why microgravity processing was expected to produce desired results, and what we expected to find in conducting these tests, this report discusses the results to date which are far from complete.

Fripp, A. L.↗

NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the projects in the present grant is to test hypotheses for the reported influence of microgravity on the microstructure of eutectics. The prior experimental results on the influence of microgravity on the microstructure of eutectics have been contradictory. With lamellar eutectics, microgravity had a negligible effect on the microstructure. Microgravity experiments with fibrous eutectics sometimes showed a finer microstructure and sometimes a coarser microstructure. Most research has been done on the MnBi/Bi rod-like eutectic. Larson and Pirich obtained a two-fold finer microstructure both from microgravity and by use of a magnetic field to quench buoyancy-driven convection. Smith, on the other hand, observed no change in microgravity. Prior theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in front of a growing eutectic sufficiently to cause a measurable change in microstructure. We assumed that the bulk melt was at the eutectic composition and that freezing occurred at the extremum, i.e. with minimum total undercooling at the freezing interface. There have been four hypotheses attempting to explain the observed changes in microstructure of fibrous eutectics caused by convection: I .A fluctuating freezing rate, combined with unequal kinetics for fiber termination and branching. 2. Off-eutectic composition, either in the bulk melt due to an off-eutectic feed or at the freezing interface because of departure from the extremum condition. 3. Presence of a strong habit modifying impurity whose concentration at the freezing interface would be altered by convection. At the beginning of the present grant, we favored the first of these hypotheses and set out to test it both experimentally and theoretically. We planned the following approaches: I .Pass electric current pulses through the MnBi/Bi eutectic during directional solidification in order to produce an oscillatory freezing rate. 2. Directionally solidify the MnBi/Bi eutectic on Mir using the QUELD II gradient freeze furnace developed by Professor Smith at Queen's University. 3. Select another fibrous eutectic system for investigation using the Accelerated Crucible Rotation Technique to introduce convection. 4. Develop theoretical models for eutectic solidification with an oscillatory freezing rate. Because of the problems with Mir, we substituted ground-based experiments at Queen's University with QUELD II vertical and horizontal, with and without vibration of the furnace. The Al-Si system was chosen for the ACRT experiments. Three related approaches were used to model eutectic solidification with an oscillatory freezing rate. A sharp interface model was used to calculate composition oscillations at the freezing interface in response to imposed freezing rate oscillations.

Wilcox. William R.↗

NASA NTRS1999

Melt Stabilization of PbSnTe in a Magnetic Field

Both the experimental observation and numerical simulation indicate that the Bridgman growth of PbSnTe under the microgravity environment in space is still greatly influenced by buoyancy-induced convection. The application of a magnetic field during the semiconductor growth can dampen the convective flow in the metal-like melt. However, for Bridgman growth of PbSnTe on earth (with either vertical or horizontal configuration), both experimental observation and numerical modeling suggest that even with a strong magnetic furnace (5-Tesla constant axial magnetic field), the convective flow in the melt still cannot be sufficiently suppressed to reach the diffusion-controlled level. In order to completely dampen the buoyancy-induced convection on earth, estimates based on scaling analysis indicate that for common experimental conditions, an extremely high magnetic field is required, far beyond the capacity of the experimental apparatus currently available. Therefore, it is proposed that only the combination of microgravity environment and magnetic damping will produce the desired diffusion-controlled growth state for this particular material. The primary objectives of this study are to provide a quantitative understanding of the complex transport phenomena during solidification of non-dilute binarys, to furnish a numerical tool for furnace design and growth condition optimization, to provide estimates of the required magnetic field strength for low gravity growth, and to assess the role of magnetic damping for space and earth control of the double-diffusive convection. As an integral part of a NASA research program, our numerical simulation supports both the flight and ground-based experiments in an effort to bring together a complete picture of the complex physical phenomena involved in the crystal growth process. For Bridgman growth of PbSnTe under microgravity (with both vertical and horizontal configurations), the simulations suggest that a moderate axial magnetic field of only a few kilo-Gauss in strength could effectively eliminate buoyancy-induced convection in the melt and control solute segregation. Therefore, this work confirms the idea that the combination of microgravity environment and the magnetic damping will indeed be sufficient to produce the desired diffusion-controlled growth state for PbSnTe.

Fripp, Archibald L.↗

NASA NTRS1999

Filtration Combustion in Smoldering and SHS

Smolder waves and SHS (self-propagating high-temperature synthesis) waves are both examples of filtration combustion waves propagating in porous media. Smoldering combustion is important for the study of fire safety. Smoldering itself can cause damage, its products are toxic and it can also lead to the more dangerous gas phase combustion which corresponds to faster propagation at higher temperatures. In SHS, a porous solid sample, consisting of a finely ground powder mixture of reactants, is ignited at one end. A high temperature thermal wave, having a frontal structure, then propagates through the sample converting reactants to products. The SHS technology appears to enjoy a number of advantages over the conventional technology, in which the sample is placed in a furnace and "baked" until it is "well done". The advantages include shorter synthesis times, greater economy, in that the internal energy of the reactions is employed rather than the costly external energy of the furnace, purer products, simpler equipment and no intrinsic limitation on the size of the sample to be synthesized, as exists in the conventional technology. When delivery of reactants through the pores to the reaction site is an important aspect of the combustion process, it is referred to as filtration combustion. The two types of filtration combustion have a similar mathematical formulation, describing the ignition, propagation and extinction of combustion waves in porous media. The goal in each case, however, is different. In smoldering the desired goal is to prevent propagation, whereas in SHS the goal is to insure propagation of the combustion wave, leading to the synthesis of desired products. In addition, the scales in the two areas of application differ. Smoldering generally occurs at lower temperatures and propagation velocities than in SHS. Nevertheless, the two applications have much in common, so that what is learned in one application can be used to advantage in the other. We have considered a number of problems involving filtration combustion. Here we describe two such studies: (A) fingering instabilities in filtration combustion, (B) rapid filtration combustion waves driven by convection.

Matkowsky, Bernard↗