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Dendrite free eutectic mixture of Pb-Sb is expected to be superelastic material that can be used in formation of shaped charge liners for industrial explosive metal-forming processes and other applications.
The formation of segregation channels during the unidirectional solidification of base chilled ingots has been studied as a function of composition in binary Pb-Sn and Pb-Sb and ternary Pb-Sn-Sb alloys. The patterns of channel distribution were characterized in the binary and ternary systems and are described as functions of temperature gradients, growth rates, dendrite spacings, and interdendritic permeabilities. Channels appear to nucleate at random across a dendritic front and subsequently to interact as they propagate, decreasing in density across the front. Assuming that the interdendritic spacing is the characteristic distance for a liquid perturbation, yields critical effective Rayleigh numbers which lie within a factor of x 40 for both metallic and aqueous systems. This correlation is close, considering the sensitivity to any assumed dimension and the range of material properties involved, and is taken to support a model for channel nucleation occurring close to the dendritic growth front.
The experiment objectives, design/operational concepts, and final results of each of nine scientific experiments conducted during the first Space Processing Applications Rocket (SPAR) flight are summarized. The nine individual SPAR experiments, covering a wide and varied range of scientific materials processing objectives, were entitled: solidification of Pb-Sb eutectic, feasibility of producing closed-cell metal foams, characterization of rocket vibration environment by measurement of mixing of two liquids, uniform dispersions of crystallization processing, direct observation of solidification as a function of gravity levels, casting thoria dispersion-strengthened interfaces, contained polycrystalline solidification, and preparation of a special alloy for manufacturing of magnetic hard superconductor under zero-g environment.
Experiment objectives, design/operational concepts, and final results are summarized for six materials science experiments conducted during the second space processing applications rocket mission flown by NASA. The individual experiments discussed are: (1) solidification of Pb-Sb eutectic; (2) feasibility of producing closed-cell metal foams; (3) direct observation of dendrite remelting and macrosegregation in castings; (4) agglomeration in immiscible liquids; (5) casting dispersion - strengthened composites at zero gravity; and (6) solidification behavior of Al-In alloys under zero gravity conditions.
This newly funded project seeks to extend our NASA-sponsored project on modeling of dendritic microstructures to facilitate collaboration between our research group and those of other NASA investigators. In our ongoing program, we have applied advanced computational techniques to study microstructural evolution in dendritic solidification, for both pure isolated dendrites and directionally solidified alloys. This work has enabled us to compute dendritic microstructures using both realistic material parameters and experimentally relevant processing conditions, thus allowing for the first time direct comparison of phase field computations with laboratory observations. This work has been well received by the materials science and physics communities, and has led to several opportunities for collaboration with scientists working on experimental investigations of pattern selection and segregation in solidification. While we have been able to pursue these collaborations to a limited extent, with some important findings, this project focuses specifically on those collaborations. We have two target collaborations: with Prof. Glicksman's group working on the Isothermal Dendritic Growth Experiment (IDGE), and with Prof. Poirier's group studying directional solidification in Pb-Sb alloys. These two space experiments match well with our two thrusts in modeling, one for pure materials, as in the IDGE, and the other directional solidification. Such collaboration will benefit all of the research groups involved, and will provide for rapid dissemination of the results of our work where it will have significant impact.
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.
Simulations that assess the effect of space vehicle acceleration environments on the solidification of Pb-Sb alloys are reported. Space microgravity missions are designed to provide a near zero-g acceleration environment for various types of scientific experiments. Realistically. these space missions cannot provide a perfect environment. Vibrations caused by crew activity, on-board experiments, support systems stems (pumps, fans, etc.), periodic orbital maneuvers, and water dumps can all cause perturbations to the microgravity environment. In addition, the drag on the space vehicle is a source of acceleration. Therefore, it is necessary to predict the impact of these vibration-perturbations and the steady-state drag acceleration on the experiments. These predictions can be used to design mission timelines. so that the experiment is run during times that the impact of the acceleration environment is acceptable for the experiment of interest. The simulations reported herein were conducted using a finite element model that includes mass, species, momentum, and energy conservation. This model predicts the existence of "channels" within the processing mushy zone and subsequently "freckles" within the fully processed solid, which are the effects of thermosolutal convection. It is necessary to mitigate thermosolutal convection during space experiments of metal alloys, in order to study and characterize diffusion-controlled transport phenomena (microsegregation) that are normally coupled with macrosegregation. The model allows simulation of steady-state and transient acceleration values ranging from no acceleration (0 g). to microgravity conditions (10(exp -6) to 10(exp -3) g), to terrestrial gravity conditions (1 g). The transient acceleration environments simulated were from the STS-89 SpaceHAB mission and from the STS-94 SpaceLAB mission. with on-orbit accelerometer data during different mission periods used as inputs for the simulation model. Periods of crew exercise, quiet (no crew activity), and nominal conditions from STS-89 were used as simulation inputs as were periods of nominal. overboard water-dump, and free-drift (no orbit maneuvering operations) from STS-94. Steady-state acceleration environments of 0.0 and 10(exp -6) to 10(exp -1) g were also simulated, to serve as a comparison to the transient data and to assess an acceptable magnitude for the steady-state vehicle drag
Pb-2.2 wt% Sb alloy was directionally solidified in 1, 2, 3 and 7 mm diameter crucibles. Pb-Sb alloy presents a solutally unstable case. Under plane-front conditions, the resulting macrosegregation along the solidified length indicates that convection persists even in the 1 mm diameter crucible. Al-2 wt% Cu alloy was directionally solidified because this alloy was expected to be stable with respect to convection. Nevertheless, the resulting macrosegregation pattern and the microstructure in solidified examples indicated the presence of convection. Simulations performed for both alloys show that convection persists for crucibles as small as 0.6 mm of diameter. For the solutally stable alloy, Al-2 wt% Cu, the simulations indicate that the convection arises from a lateral temperature gradient.
Numerical models of solidification including a mushy zone are notoriously inefficient; most of them are based on formulations that require the coupled solution of the velocity components in the momentum equation greatly restricting the range of applicability of the models. There are only two models known to the authors that have used a projection or fractional step formulation, but none of these were used to model problems of any significant size. A third model was only applied to a partial mushy zone with no all-fluid region. Our initial attempts at modeling directional solidification in the presence of a developing mushy zone using a projection formulation encountered very serious difficulties once solidification starts. These difficulties were traced to the inability of the method to deal with large local density differences in the vicinity of the fluid-mush interface. As a result, a modified formulation of the projection method has been developed, that maintains the coupling between the body force and the pressure gradient and is presented in this work. The new formulation is shown to be robust and efficient, and can be applied to problems involving very large meshes. This is illustrated in this work through its application to simulations involving Pb-Sb and Pb-Sn alloys.
PbSb3 crystallizes in the hexagonal P6_3/mmc space group. The structure is three-dimensional. Pb2+ is bonded to twelve equivalent Sb+0.67- atoms to form a mixture of face and corner-sharing PbSb12 cuboctahedra. There are six shorter (3.39 Å) and six longer (3.55 Å) Pb–Sb bond lengths. Sb+0.67- is bonded in a 12-coordinate geometry to four equivalent Pb2+ and eight equivalent Sb+0.67- atoms. There are a spread of Sb–Sb bond distances ranging from 3.28–3.49 Å.
Pb3Sb crystallizes in the hexagonal P6_3/mmc space group. The structure is one-dimensional and consists of two Pb3Sb ribbons oriented in the (0, 0, 1) direction. Pb is bonded in a 2-coordinate geometry to two equivalent Sb atoms. Both Pb–Sb bond lengths are 3.38 Å. Sb is bonded in a 12-coordinate geometry to six equivalent Pb atoms.
PbSb crystallizes in the orthorhombic Cmmm space group. The structure is three-dimensional. Pb2+ is bonded in a 8-coordinate geometry to four equivalent Sb2- atoms. All Pb–Sb bond lengths are 3.43 Å. Sb2- is bonded in a distorted body-centered cubic geometry to four equivalent Pb2+ and four equivalent Sb2- atoms. All Sb–Sb bond lengths are 3.39 Å.
PbSb is Halite, Rock Salt structured and crystallizes in the cubic Fm-3m space group. The structure is three-dimensional. Pb2+ is bonded to six equivalent Sb2- atoms to form a mixture of edge and corner-sharing PbSb6 octahedra. The corner-sharing octahedral tilt angles are 0°. All Pb–Sb bond lengths are 3.18 Å. Sb2- is bonded to six equivalent Pb2+ atoms to form a mixture of edge and corner-sharing SbPb6 octahedra. The corner-sharing octahedral tilt angles are 0°.