Engineering topics
Publications and source records attributed to Gillies, Donald C..
Following a brief overview of NASA s Microgravity Materials Science programs, specific examples will be given showing electron beam and optical microscopic applications to two-phase glass structures, dendrite tip radii, solid solution semiconductors, undercooled two-phase stainless steels and meteorites.
With judicious selection of parameters, computed tomography can provide high precision density data. Such data can lead to a non-destructive determination of the phases and phase distribution within large solid objects. Of particular interest is the structure of the Mundrabilla meteorite, which has 25 volumes, percent of a sulfide within a metallic meteorite. 3D digital imaging has enabled a quantitative evaluation of the distribution and contiguity of the phases to be determined.
Computed Tomography (CT) has advanced considerably since being responsible for such dramatic advances in diagnostics within the medical field. It has become a major tool in non destructive evaluation (NDE), and is used in many fields as diverse as coal-mining to metal solidification to examination of rock cores. A review of industrial applications has been written by Dennis. It is only recently that the technique has been seriously used to determine composition through precise measurement of density. While such applications are restricted to cases when there is no ambiguity in the relationship of composition to density. Thus alloy solid solutions lend themselves to compositional analysis provided there is a large change in density with composition. The technique is most useful when rapid non-destructive evaluation is needed. Such cases will occur with samples returning from the International Space Station (ISS) when knowledge of the results could affect future strategies for processing of on-board samples. Experiments from those Principal Investigators (PI) that are most likely to benefit from early CT scanning are discussed. With a dearth of samples, the major emphasis in the first part of this project has been on preparing suitable standards, optimizing the CT technique for these applications, and using the CT system to determine density variations with temperature. An interesting application of CT has been in the examination of meteorites, which can be classified as space-grown materials and will certainly have solidified in a low gravity environment.
The differentiated meteorite, Mundrabilla, exhibits a rare structure of primary kamacite/taenite, and at least 25 volume % of sulfide (troilite and daubreelite). The structure has been investigated in three dimensions using the technique of gamma-ray computed tomography (CT) with a radioactive (60)Co isotope as the source of the flux. Using CT, a 50 kg slab with dimensions 12.6 x 8.2 x approx. 70 cm has been sectioned at 1 mm intervals over 50 cm length, and the three dimensional structure is at present being evaluated. These data revealed, in addition to the metallic and troilite-rich phases, the presence and distribution of graphite-rich cones (up to 5 cm long), and small (1-2 mm), low density particles. The graphite cones are readily visible on the surfaces of many of the sections of Mundrabilla, while the smaller phases have a density (determined from CT) of approximately 2.9 g/cc, and are assumed to be silicate inclusions. CT spatial resolution is not adequate to elucidate the shapes of these particles. One can only state that they show no directionality and are equiaxed.
Ground-based research in Materials Science for NASA's Microgravity program serves several purposes, and includes approximately four Principal Investigators for every one in the flight program. While exact classification is difficult. the ground program falls roughly into the following categories: (1) Intellectual Underpinning of the Flight Program - Theoretical Studies; (2) Intellectual Underpinning of the Flight Program - Bringing to Maturity New Research; (3) Intellectual Underpinning of the Flight Program - Enabling Characterization; (4) Intellectual Underpinning of the Flight Program - Thermophysical Property Determination; (5) Radiation Shielding; (6) Preliminary In Situ Resource Utilization; (7) Biomaterials; (8) Nanostructured Materials; (9) Materials Science for Advanced Space Propulsion. It must be noted that while the first four categories are aimed at using long duration low gravity conditions, the other categories pertain more to more recent NASA initiatives in materials science. These new initiatives address NASA's future materials science needs in the realms of crew health and safety, and exploration, and have been included in the most recent NASA Research Announcements (NRA). A description of each of these nine categories will be given together with examples of the kinds of research being undertaken.
Computed Tomography (CT) has proved to be of inestimable use in providing a rapid evaluation of a variety of samples from Mechanics of Granular Materials (MGM) to electronic materials (Ge-Si alloys) to space grown materials such as meteorites. The system at Kennedy Space Center (KSC), because of its convenient geographical location, is ideal for examining samples immediately after returning to Earth. It also has the advantage of the choice of fluxes, and in particular the use of a radioactive cobalt source, which is basically monochromatic. This permits a reasonable measurement of density to be made from which chemical composition can be determined. Due to the current dearth of long duration space grown materials, the CT instrument has been used to characterize materials in preparation for flight, to determine thermal expansion values, and to examine long duration space grown materials, i.e. meteorites. The work will first describe the establishment of the protocol for obtaining the optimum density readings for any material. This will include both the effects of the hardware or instrumental parameters that can be controlled, and the techniques used to process the CT data. Examples will be given of the compositional variation along single crystals of germanium-silicon alloys. Density variation with temperature has been measured in preparation for future materials science experiments; this involved the fabrication and installation of a single zone furnace incorporating a heat pipe to ensure of high temperature uniformity. At the time of writing the thermal expansion of lead has been measured from room temperature to 900 C. Three methods are available. Digital radiography enable length changes to be determined. Prior to melting the sample is small than the container and the diameter change can be measured. Most critical, however, is the density change in solid, through the melting region, and in the liquid state. These data are needed for engineering purposes to aid in the design of containment cartridges, and for enabling fluid flow calculations. A second sample, with the lead alloyed with antimony is ready for scanning. This corresponds to the planned composition of Dr. Poirier's flight experiment. Finally, three-dimensional results will be shown of the structure of a two-phase metallic meteorite of metal and sulfide, in which the iron-nickel phase has coarsened during slow cooling over hundreds of millions of years.
The purpose behind this work is to provide NASA Principal Investigators (PIs) rapid information, nondestructively, about their samples. This information will be in the form of density values throughout the samples, especially within slices 1 mm high. With correct interpretation and good calibration, these values will enable the PI to obtain macro chemical compositional analysis for his/her samples. Alternatively, the technique will provide information about the porosity level and its distribution within the sample. Experience gained with a NASA Microgravity Research Division-sponsored Advanced Technology Development (ATD) project on this topic has brought the technique to a level of maturity at which it has become a viable characterization tool for many of the Materials Science Pls, but with equipment that could never be supported within their own facilities. The existing computed tomography (CT) facility at NASA's Kennedy Space Center (KSC) is ideally situated to furnish information rapidly and conveniently to PIs, particularly immediately before and after flight missions.
The solidification of a solid solution semiconductor, having a wide separation between liquidus and solidus has been extensively studied in ground based, high magnetic field and Spacelab experiments. Two alloys of mercury cadmium telluride have been studied; with 80.0 mole percent of HgTe and 84.8 mole percent of HgTe respectively, the remainder being cadmium telluride. Such alloys are extremely difficult to grow by directional solidification on earth due to high solutal and thermal density differences that give rise to fluid flow and consequent loss of interface shape and composition. Diffusion controlled growth is therefore impossible to achieve in conventional directional solidification. The ground based experiments consisted of growing crystals in several different configurations of heat pipe furnaces, NASA's Advanced Automated Directional Solidification Furnace (AADSF), and a similar furnace incorporated in a superconducting magnet capable of operating at up to 5T. The first microgravity experiment took place during the flight of STS-62 in March 1994, with the AADSF installed on the second United States Microgravity Payload (USMP-2). The alloy was solidified at 3/4 inch per day over a 9 day period, and for the first time a detailed evaluation was performed correlating composition variations to measured residual acceleration. The second flight experiment took place in the fourth United States Microgravity Payload Mission (USMP-4) in November 1997. Due to contamination of the furnace system, analysis shows that the conditions prevailing during the experiment were quite different from the requirements requested prior to the mission. The results indicate that the sample did accomplish the desired objectives.
Recently, NASA's Microgravity Research Division was re-aligned to match the Agency's increasing awareness of the importance of biological and nano-structural sciences. The Division has become the Physical Sciences Research section within the newly created Office of Biological and Physical Research. Within materials science and in the last few years, new programs aimed at biomaterials have been initiated. Results from these programs and also new research pertaining to materials for radiation protection will be discussed.
The accurate measurement of density in both liquid and solid samples is of considerable interest to Principal Investigators with materials science experiments slated for the ISS. The work to be described is an innovative application of a conventional industrial nondestructive evaluation instrument. Traditional applications of industrial computed tomography (CT) rely on reconstructing cross sections of large structures to provide two-dimensional planar views which can identify defects such as porosity, or other material anomalies. This has been done on microgravity materials science experiments to check the integrity of ampoule-cartridge assemblies for safety purposes. With a substantially monoenergetic flux, as can be obtained with a radioactive cobalt source, there will be a direct correlation between absorption and density. Under such conditions it then becomes possible to make accurate measurements of density throughout a sample, and even when the sample itself is enclosed within a furnace and a safety required cartridge. Such a system has been installed at Kennedy Space Center (KSC) and is available to PIs to examine samples before and after flight. The CT system is being used to provide density information for two purposes. Firstly, the determination of density changes from liquid to solid is vital information to the PI for purposes of modeling the solidification behavior of his sample, and to engineers who have to design containment ampoules and must allow for shrinkage and other volume changes that may occur during processing. While such information can be obtained by pycnometric measurements, the possibility of using a furnace installed on the CT system enables one to examine potentially dangerous materials having high vapor pressures, while not needing visible access to the material. In addition, uniform temperature can readily be obtained, and the system can be controlled to ramp up, hold, and ramp down while collecting data over a wide range of parameters automatically. Results of initial tests on low melting point elements such as gallium, indium and tin will be presented, and the intent is to proceed to compounds such as InSb, HgCdTe and CdTe. Alloys such as Pb-Sb (PI - Poirier, U AZ) and Cu-Al (PI - Trivedi, Ames Lab.), which are the subjects of flight experiments, will also be examined. The second application is the conversion of measured density values directly to composition. This was successfully done with the mercury cadmium telluride alloys grown on the second and fourth United States Microgravity Payload (USMP-2 and USMP-4) missions by Lehoczky. CdTe values along the length of the boules were obtained at KSC prior to cutting the sample, and could have been obtained prior to its removal from the cartridge and ampoule. Examples of the data obtained will be shown. It is anticipated that several of the materials science PIs will avail themselves of the technique described, initially for determining densities prior to flight, and then to acquire early quantitative data on the compositional variation within their samples.
A general finite element model of non-dilute alloy solidification was used to simulate growth of HgCdTe from the melt. 2-D and 3-D models with and without Oberbeck-Boussinesq (O-B) approximation were used. Verification of the 3-D model was based on experimental data. The location and the shape of the interface were determined using melting temperatures obtained from the HgCdTe liquidus curve. Double-diffusive convection in the melt is caused by radial temperature gradients and by rejection at the solid-melt interface of the heavier HgTe-rich solute. Because of these complicating factors, dimensional rather than non-dimensional modeling was performed. Models based on complete set of Navier-Stokes equations for compressible media are superior to the O-B approximation in microgravity, because they provide more accurate estimation of convection.
The purpose behind this work is to provide NASA Principal Investigators (PI) rapid information, non-destructively, about their samples. This information will be in the form of density values throughout the samples, especially within slices 1 mm high. With correct interpretation and good calibration, these values will enable the PI to obtain macro chemical compositional analysis for his/her samples. Alternatively, the technique will provide information about the porosity level and its distribution within the sample. Experience gained with a NASA MRD-sponsored Advanced Technology Development (ATD) project on this topic has brought the technique to a level of maturity at which it has become a viable characterization tool for many of the Materials Science PIs, but with equipment that could never be supported within their own facilities. The existing computed tomography (CT) facility at NASA's Kennedy Space Center (KSC) is ideally situated to furnish information rapidly and conveniently to PIs, particularly immediately before and after flight missions.
A description will be made of the current materials science program within the microgravity research division. This presentation will be made at a plenary session of the biennial materials Science Conference.
The part to be played by materials scientists to further NASA's exploration missions cannot be underestimated. To quote Jerome Groopman (New Yorker, February 14, 2000), "The rocket science will be the easy part". The four main risks on the Critical Path Road Map during a three-year sojourn to Mars are osteoporosis, psychological problems, radiation induced cancer and acute medical trauma. NASA's microgravity materials science program has investigations in membrane fabrication, bone growth and materials for radiation protection. These programs will be reviewed in the context of the four main risks, as will other potential uses of biomaterials and applications of biomimetic processing.
The Materials Science program within NASA's Microgravity Research Division will be outlined. Particular emphasis will be placed on those experiments slated for the International Space Station which pertain to high temperature materials. These include experiments designed to examine theories pertaining to solidification and pattern selection, coarsening and phase transformation.
The solidification of a solid solution semiconductor, having a wide separation between liquidus and serious has been extensively studied in ground based, high magnetic field and Spacelab experiments. Two alloys of mercury cadmium telluride have been studied; mercury cadmium telluride with 80.0 mole percent of HgTe and 84.8 mole percent respectively. These alloys are extremely difficult to grow by directional solidification on earth due to high solutal and thermal density differences that give rise to fluid flow and consequent loss of interface shape and composition. Diffusion controlled growth is therefore impossible to achieve in conventional directional solidification. The ground based experiments consisted of growing crystals in several different configurations of heat pipe furnaces, NASA's Advanced Automated Directional Solidification Furnace (AADSF), and a similar furnace incorporated in a superconducting magnet capable of operating at up to 5T. The first microgravity experiment took place during the flight of STS-62 in March 1994, with the AADSF installed on the second United States Microgravity Payload (USMP-2). The alloy was solidified at 3/4 inch per day over a 9 day period, and for the first time a detailed evaluation was performed of residual acceleration effects. The second flight experiment took place in the fourth United States Microgravity Payload Mission (USMP-4) in November 1997. Due to contamination of the furnace system by a previously processed sample, the sample was not received until May 1998, and the preliminary analysis shows that the conditions prevailing during the experiment were quite different from the requirements requested prior to the mission. Early results are indicating that the sample may not accomplish the desired objectives. As with the USMP-2 mission, the results of the ground based experiments were compared with the crystal grown in orbit under microgravity conditions. On the earth, it has been demonstrated that the application of the magnetic field leads to a significant reduction in fluid flow, with improved homogeneity of composition. The field strength required to suppress flow increases with diameter of the material. The 8 mm diameter sample used here was less than the upper diameter limit for a ST magnet. The configuration for USMP-4 was changed so that the material was seeded and other processing techniques were also modified. It was decided to examine the effects of a strong magnetic field under the modified configuration and parameters. A further change from USMP-2 was that a different composition of material was grown, namely with 0.152 mole fraction of cadmium telluride rather than the 0.200 of the USMP-2 experiment. The objective was to grow highly homogeneous, low defect density material of a composition at which the conduction band and the valence band of the material impinge against each other. As indicated, the furnace was contaminated during the mission. As a result of solid debris remaining in the furnace bore, the cartridge in this experiment, denoted as SL1-417, was significantly bent during the insertion phase. During translation the cartridge scraped against the plate which isolates the hot and cold zones of the furnace. Thermocouples indicated that a thermal assymetry resulted. The scraping in the slow translation or crystal growth part of the processing was not smooth and it is probable that the jitter was sufficient to give rise to convection in the melt. Early measurements of composition from the surface of the sample have shown that the composition varies in an oscillatory manner.
The objective of the study is to establish the effects of processing semiconducting, solid solution, single crystals in a microgravity environment on the metallurgical, compositional, electrical, and optical characteristics of the crystals. The alloy system being investigated is the solid solution semiconductor Hg(1-x)Cd(x)Te, with x-values appropriate for infrared detector applications in the 8 to 14 mm wavelength region. Both melt and Te-solvent growth are being performed. The study consists of an extensive ground-based experimental and theoretical research effort followed by flight experimentation where appropriate. The ground-based portion of the investigation also includes the evaluation of the relative effectiveness of stabilizing techniques, such as applied magnetic fields, for suppressing convective flow during the melt growth of the crystals.
The Microgravity Research Division of NASA funds research programs in all branches of materials science including ceramics and glasses. A NASA Research Announcement (NRA)is currently planned with proposals due in March 1999. Proposals are accepted for both flight- definition and ground- based research projects with a main criterion being a strong justification for microgravity. A review of the program in its entirety will be given, with special emphasis on microgravity related ceramics research. The topics of current interest in the NRA will be discussed in terms of International Space Station research and NASA's Human Exploration and Development of Space (HEDS) initiative.