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Gradients are controllable from zero to 500 degrees C/cm. Typical temperature profile superimposed on partial cross section of furnace. Steepness of gradient varied by adjusting flow of energy to and from different zones of furnace. Specimen placed in ampoule moved inside ceramic tube according to needs of experiment. Furnace provides axial temperature profiles for material processing experiments.
The nickel-base superalloy MAR-246(Hf) was studied to determine the factors affecting basic morphology and fatigue properties. Of particular interest was the degradation of fatigue properties with deviation from the 001 growth orientation. Examination of directionally solidified samples showed a dependence of carbide shape and interdentritic segregation on growth rate. Heat treatment studies focused on the gamma prime structure, determining that it reaches maximum growth after twenty-four hours but its size and stability depends on the temperature of the treatment. Fatigue test specimens were oriented crystallographically in the failed and unfailed regions and found to have rotated their orientation during the testing if they were located a significant distance from 001. This would place increased strain on the crystal and precipitate early failure.
A model of dendritic growth in both supercooled pure and alloy melts is presented. In a pure melt, dendrite morphology is determined by the value of the dimensionless parameter sigma = 2 alpha (L)d(o)/sq Rr(t) whereas, in an alloy melt it is determined by the parameter sigma = 2 lambda (c)D(L)/sq Rr(t). The application of the above analysis to cylindrical and spherical growth morphologies obtained in highly supercooled melts has been discussed. An upper and lower bound for the particle or tip radius in this case has been obtained in terms of the growth rate and the initial bath supercooling.
Radial growth anisotropies and equilibrium forms of point nucleated, dislocation free silicon sheets spreading horizontally on the free surface of a silicon melt were measured for (100), (110), (111), and (112) sheet planes. The growth process was recorded. Qualitative Wulff surface free energy polar plots were deduced from the equilibrium shapes for each sheet plane. Predicted geometries for the tip shape of unidirectional, dislocation free, horizontally grown sheets growing in various directions within the planes were analyzed. Polycrystalline sheets and dendrite propagation were analyzed. For dendrites, growth rates on the order of 2.5 m/min and growth rate anisotropies of 25 are measured.
One lamellar eutectic sample and one fiber-like eutectic sample were solidified directionally during the TEXUS-6 rocket flight. The microstructures and the results of the thermal analysis, obtained from the temperatures recorded on the cartridge skin, are compared. No appreciable modifications of the regularity of the eutectic structures were observed by passing from 1 g to 0.0001 g in these experiments. No steady state growth conditions were achieved in these experiments.
Experimental work is described on undercooling and structure of tin-lead droplets emulsified in oil. The droplets, predominantly in the size range of 10-20 microns, were cooled at rates ranging from about 0.04 K/sec to 1,000,000 K/sec. The higher cooling rates were obtained by a newly developed technique of quenching the emulsified droplets in a cold liquid. Measured undercoolings (at the lower cooling rates) ranged up to about 100 C. Structures obtained depended strongly on undercooling, cooling rate before nucleation, droplet size, alloy composition and the rate of heat extraction after nucleation.
The microstructures of directionally grown monotectic alloys in metallic and organic systems fall into two categories those which can form aligned fibrous composite structures with even phase spacings and fiber sections, and those in which the phase distribution is coarser and less regular. This division appears to relate to the form of the phase diagram and has been rationalized by Cahn (1977, 1979) in terms of the relative surface energies between solid and two liquids to give steady state or nonsteady state profiles. The transition in growth behavior occurs when the ratio of the monotectic temperature to that of the upper consolute temperature is approximately 0.9. Differences in phase spacings between a range of monotectic and eutectic systems are discussed in terms of the expected growth interface shapes and the factors which will influence them.
Experimental work on undercooling and structure of tin-lead droplets emulsified in oil is described. The droplets, predominantly in the size range of 10 to 20 microns, were cooled at rates (just before nucleation) ranging from about 0.1 to 1 million K/s. The higher cooling rates were obtained by a newly developed technique of quenching the emulsified droplets in a cold liquid. Measured undercoolings (at the lower cooling rates) ranged up to about 100 K. Structures obtained depend strongly on undercooling, cooling rate before and after nucleation, and alloy composition. Droplets containing up to 5 wt pct Pb were apparently single phase when undercooled and rapidly quenched. Droplets in the composition range of about 25-90 wt pct Pb solidified dendritically, even at the most rapid quench rates employed, apparently because these alloys undercooled only slightly before nucleation of the primary phase.
A quantitative calculation of growth rates and tip radii is presented for dendrites growing in undercooled dilute solutions. Included in the calculations are the capillary corrections to the steady-state Ivantsov needle-crystal solutions. The results show good agreement with available experimental data and support the validity of the marginal-stability theory of dendritic growth.
Samples of rod eutectics Bi/MnBi were directionally solidified in a growth-up Bridgman-Stockbarger configuration in the presence of a transverse magnetic field up to 3 kg to determine whether gravity-driven convective effects could be reduced or eliminated. The experiments were carried out over a range of furnace velocities, V, of 0.2 to 50 cm per hour with a thermal gradient at the liquid-solid interface of 100 C/cm and 150 C/cm. Morphological, thermal and magnetic analyses were carried out on samples grown with and without an applied magnetic field. For samples grown at V greater than 3 cm per hour in a transverse magnetic field, reduced mean rod diameter and interrod spacing occurred as well as undercooling and increased coercive strength. The data agreed with that obtained for low-g growth at 50 cm per hour and 30 cm per hour.
The formation of chiral solidlike domains observed by Weiss and McConnell (1984) in monolayers of depalmitoylphosphatidylcholine (DPPC) floating on an air-water interface is investigated theoretically. It is proposed that the diffusion tensor for the two-dimensional fluidlike phase of the DPPC molecules has a chiral component acting perpendicular to the concentration gradient and coupled to the rotational motion of a pinwheellike molecule by the viscous forces. Diagrams are provided, and numerical estimates of the forces involved are shown to be in agreement with the observed behavior of the structures.
A Ni-base superalloy containing 13Al-9Mo-2Ta (in at. percent) has been characterized in both the rapidly solidified condition and after dynamic compaction. Dynamically compacted specimens were examined in the as-compacted condition and observations related to current theories of interparticle bonding. In addition, the recrystallization behavior of the compacted material at relatively low temperature (about 0.5-0.75 Tm) was investigated.
The Ni-base superalloy MAR-M246 (Hf) was directionally solidified during low gravity maneuvers aboard a NASA KC-135 aircraft. Gravity force variations during this process yielded a concomitant variation in microstructure and microsegregation. Secondary dendrite arm spacings are noted to be larger in the low-g portion; this, in turn, decreases the extent of interdendritic segregation. The amount of Hf in both the carbides and interdendritic eutectic increases as the gravity force diminishes. Fewer carbides are present in the low-g regions.
This research is composed of three major components: (1) development of interface morphology control for automated Bridgman growth of semiconductor systems; (2) comparative analysis of segregation during crystal growth in a reduced gravity environment and in the presence of magnetic fields; and (3) consequences of seeding by meltback in Bridgman growth under reduced gravity conditions. In attempts to optimize furnace design for crystal growth in a reduced gravity environment, an analytical approach to heat transfer was developed. It was thus found that charge confining crucibles diminish the ability to control the growth interface morphology through its position within the gradient zone. A heat pipe hot zone system for Bridgman growth, in reduced gravity environment, of crystal with diameters up to 16 mm was developed. For growth of Ga-doped germanium in the multipurpose (ASTP) furnace, it was found that the application of transverse magnetic fields (up to 36 kg) does not substantially increase the effective distribution coefficient; i.e., diffusion-controlled segregation observed in reduced gravity environment cannot be reached nor approached by magnetic field induced melt stabilization.
The objective of this program is to analyze the mechanisms involved in the composite solid structure formation obtained from a miscibility gap alloy under microgravity. The metallic system aluminum-indium was chosen for its low critical temperature, broad miscibility gap, and rather well-known thermodynamic properties. The experiment was performed aboard the Salyut-7 spacecraft. The theories of capture of particulates by an advancing front were not able to explain the observations made on SPAR and Salyut-7 experiments. A new model was developed based on the filtration theory considering the globules population: the solid/liquid interface is like a filter of negligible thickness for the globules and its efficiency is limited by a pressure barrier measured for Al-In alloys by ground based experiments. The Materials Experiment Assembly (MEA)-3 experiment was consequently adjusted to take into account the new model. The behavior of the globules in an interacting population on the solid front is, of course, an essential factor in the theory. The theory is at present being completed by results obtained by the Laboratoire d'Aerothermique of Meudon. The hydrodynamic and thermal interactions between pairs of globules placed in a temperature gradient have been calculated showing a large reduction of the Marangoni effect compared to the isolated globule. Physico-chemical properties of metallic liquid interface are currently being investigated.
A model for dendritic growth in a binary alloy melt, in the presence of a positive temperature gradient in the liquid, is presented. The model describes satisfactorily the transition from a dendritic interface to a planar interface at very low and very large growth rates. A dendrite tip stability parameter is derived, strictly from steady state considerations, without resorting to a perturbation analysis. The estimates of the parameter agree with those obtained by models based on perturbation analyses.
A process of metallurgical grade (MG) silicon production is presented which appears particularly suitable for photovoltaic (PV) applications. The MG silicon is prepared in a 240 KVA, three electrode submerged arc furnace, starting from high grade quartz and high purity silicon carbide. The silicon smelted from the arc furnace was shown to be sufficiently pure to be directionally solidified to 10 to 15 kg. After grinding and acid leaching, had a material yield larger than 90%. With a MG silicon feedstock containing 3 ppmw B, 290 ppmw Fe, 190 ppmw Ti, and 170 ppmw Al, blended with 50% of off grade electronic grade (EG) silicon to reconduct the boron content to a concentration acceptable for solar cell fabrication, the 99% of deep level impurities were concentrated in the last 5% of the ingot. Quite remarkably this material has OCV values higher tham 540 mV and no appreciable shorts due to SiC particles.
Microstructural changes enhance properties of alloys. Major feature of process is rapid quenching of alloys or intermetallic compounds from liquid to solid state at cooling rates of 10 to the 6th power C/s.