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At least 55 records · Page 3

Dendritic growth of undercooled nickel-tin. I, II

A comparison is made between high speed cinematography and optical temperature measurements of the solidification of an undercooled Ni-25 wt pct Sn alloy. The first part of this study notes that solidification during the recalescence period at all undercoolings studied occurred in the form of a dendritelike front moving across the sample surface, and that the growth velocities observed agree with calculation results for the dendrite growth model of Lipton et al. (1986); it is concluded that the coarse structure observed comprises an array of much finer, solute-controlled dendrites. In the second part, attention is given to the solidification of levitated metal samples within a transparent glass medium for the cases of two undercooled Ni-Sn alloys, one of which is eutectic and another hypoeutectic. The data obtained suggest a solidification model involving dendrites of very fine structure growing into the melt at temperatures near the bulk undercooling temperature.

Wu, Y.↗

Undercooling of bulk high temperature metals in the 100 meter drop tube

The 100-meter drop tube at NASA Marshall Space Flight Center provides an excellent opportunity to study the effects of containerless, microgravity processing in metals and alloys. In a series of experiments high melting temperature pure metals were melted in an electron beam furnace and dropped in vacuum. Sample sizes ranged from 0.175 to 1.2 grams. Large undercoolings on the order of 18 percent of the melting temperature were observed in Ti, Zr, Nb, Mo, Rh, Ta, and Pt. Undercoolings of 5 to 18 percent T(m) were observed in Ru and Ir. These undercooling results are consistent, repeatable, and occur in a high percentage of experiments. The experimental technique will be presented as well as the resultant microstructures of undercooled drops. The data will be discussed with respect to nucleation theory.

Hofmeister, William↗

Undercooling studies on Nb-Pt and Nb-Si alloys using the 105 meter drop tube

Niobium-platinum samples of compositions ranging from 16 to 32 at. pct have been undercooled to as much as 540 K in the low gravity, containerless environment of a 105 meter drop tube. Undercooling was terminated in the Nb-Pt samples by the nucleation and growth of the Nb3Pt phase. In the 16-18 at. pct Pt samples, this resulted in samples which are completely Nb3Pt, in contrast to both the equilibrium phase diagram and the nonundercooled samples which formed with Nb dendrites and interdendritic Nb3Pt. Undercoolings for the Nb-Si samples were up to 670 K, which corresponds to 27 percent of the liquidus temperature or 80 percent of the estimated hypercooling limit. In the Nb-Si system, a coupled zone was identified as well as a metastable extension of the solubility limit of Si in Nb due to deep undercooling.

Robinson, M. B.↗

Thermodynamic properties and crystallization kinetics at high liquid undercooling

The heat capacities of liquid and crystalline Au-Pb-Sb alloys in the glass-forming composition range were measured with droplet emulsion and bulk samples. Based on the measured C(sub p) data, the entropy, enthalpy, and Gibbs free energy functions of the eutectic, solid mixture, and undercooled liquid were determined as a function of undercooling and compared with theoretical predictions. The results indicate an isentropic temperature at 313 + or - 5 K, which agrees well with experimental data for the glass transition. A kinetics analysis of the nucleation undercooling response suggests that the proper choice for the Gibbs free energy change during crystallization is most important in analyzing the nucleation kinetics. By classical nucleation theory, the prefactors obtained, based on a variety of theoretical predictions for the driving force, can differ by six orders of magnitude. If the nucleation rates are extrapolated to high undercooling, the extrapolations based on measured heat capacity data show agreement, whereas the predicted nucleation rates are inconsistent with results from drop tower experiments. The implications for microg experiments are discussed.

Fecht, Hans J.↗

Phase selection during crystallization of undercooled liquid eutectic lead-tin alloys

During rapid solidification substantial amounts of undercooling are in general required for formation of metastable phases. Crystallization at varying levels of undercooling and melting of metastable phases were studied during slow cooling and heating of emulsified PB-Sn alloys. Besides the experimental demonstration of the reversibility of metastable phase equilibra, two different principal solidification paths have been identified and compared with the established metastable phase diagram and predictions from classical nucleation theory. The results suggest that the most probable solidification path is described by the 'step rule' resulting in the formation of metastable phases at low undercooling, whereas the stable eutectic phase mixture crystallizes without metastable phase formation at high undercooling.

Fecht, H. J.↗

Microstructural transitions during containerless processing of undercooled Fe-Ni alloys

In order to identify the possible hierarchy of microstructural pathways and transitions, a systematic evaluation of the microstructural evolution in undercooled Fe-Ni alloys was performed on uniformly processed samples covering seven orders of magnitude in volume. At appropriate undercooling levels, alternate solidification pathways become thermodynamically possible and metastable product structures can result from the operation of competitive solidification kinetics. For thermal history evaluation, a heat flow analysis was applied and tested with large Fe-Ni alloy particles (1 to 3 mm) to assess undercooling potential. Alloy powders (10 to 150 microns), with large liquid undercoolings, were studied under the same composition and processing conditions to evaluate the solidification kinetics and microstructural evolution, including fcc/bcc phase selection and the thermal stability of a retained metastable bcc phase. The identification of microstructural transitions with controlled variations in sample size and composition during containerless solidification processing was used to develop a microstructure map which delineates regimes of structural evolutions and provides a unified analysis of experimental observations in the Fe-Ni system.

Thoma, D. J.↗

Containerless, Low-Gravity Undercooling of Ti-Ce Alloys in the MSFC Drop Tube

Previous tests of the classical nucleation theory as applied to liquid-liquid gap miscibility systems found a discrepancy between experiment and theory in the ability to undercool one of the liquids before the L1-L2 separation occurs. To model the initial separation process in a two-phase liquid mixture, different theoretical approaches, such as free-energy gradient and density gradient theories, have been put forth. If there is a large enough interaction between the critical liquid and the crucible, both models predict a wetting temperature (T(sub w)) above which the minority liquid perfectly wets and layers the crucible interface, but only on one side of the immiscibility dome. Materials with compositions on the other side of the dome will have simple surface adsorption by the minority liquid before bulk separation occurs when the coexistence (i.e., binoidal) line in reached. If the interaction between the critical liquid and the crucible were to decrease, T(sub w) would increase, eventually approaching the critical consolute temperature (T(sub cc)). If this situation occurs, then there could be large regions of the miscibility gap where non-perfect wetting conditions prevail resulting in droplets of L1 liquid at the surface having a non-zero contact angle. The resulting bulk structure will then depend on what happens on the surface and the subsequent processing conditions. In the past several decades, many experiments in space have been performed on liquid metal binary immiscible systems for the purpose of determining the effects that different crucibles may have on the wetting and separation process of the liquids. Potard performed experiments that showed different crucible materials could cause the majority phase to preferentially wet the container and thus produce a dispersed microstructure of the minority phase. Several other studies have been performed on immiscibles in a semi-container environment using an emulsion technique. Only one previous study was performed using completely containerless processing of immiscible metals and the results of that investigation are similar to some of the emulsion studies. In all the studies, surface wetting was attributed as the cause for the similar microstructures or the asymmetry in the ability to undercool the liquid below the binoidal on one side of the immiscibility dome. By removing the container completely from the separation process, it was proposed that the loss of the crucible/liquid interaction would produce a large shift in T(sub w) and thus change the wetting characteristics at the surface. By investigating various compositions across the miscibility gap, a change in the type and amount of liquid wetting at the surface of a containerless droplet should change the surface nucleating behavior of the droplet - whether it be the liquid-liquid wetting or the liquid-to-solid transition. Undercooling of the liquid into the metastable region should produce significant differences in the separation process and the microstructure upon solidification. In this study, we attempt to measure these transitions by monitoring the temperature of the sample by optical pyrometry. Microstructural analysis will be made to correlate with the degree of undercooling and the separation mechanisms involved.

Robinson, M. B.↗

High Undercooling of Ni59Nb41 Alloy in a Containerless Electrostatic Levitation Facility

Utilizing the containerless electrostatic levitation facility at NASA/MSFC, we were able to undercool the Ni59Nb41 (atomic) alloy by 210 K which was 160 degrees farther than the results of previous flight experiments. Undercoolings were clustered around 200 K during the repeated melting-freezing cycles on a single sample. Prior to this work, a metastable liquid separation had been presumed to limit the undercooling of this alloy. However, microstructural observations have revealed that undercooling was limited by crystal nucleation.

Robinson, M. B.↗

High Undercooling of Ni59Nb41 Alloy in a Containerless Electrostatic Levitation Facility

Utilizing the containerless electrostatic levitation facility at NASA/MSFC, we were able to undercool the Ni-59Nb-41 (atomic) alloy by 210 K which was 160 deg. farther than the results of previous flight experiments. Undercoolings were clustered around 200 K during the repeated melting-freezing cycles on a single sample. Prior to this work, a metastable liquid separation had been presumed to limit the undercooling of this alloy. However, microstructural observations have revealed that undercooling was limited by crystal nucleation.

Robinson, M. B.↗

Effect of Viscosity on the Crystallization of Undercooled Liquids

There have been numerous studies of glasses indicating that low-gravity processing enhances glass formation. NASA PI s are investigating the effect of low-g processing on the nucleation and crystal growth rates. Dr. Ethridge is investigating a potential mechanism for glass crystallization involving shear thinning of liquids in 1-g. For shear thinning liquids, low-g (low convection) processing will enhance glass formation. The study of the viscosity of glass forming substances at low shear rates is important to understand these new crystallization mechanisms. The temperature dependence of the viscosity of undercooled liquids is also very important for NASA s containerless processing studies. In general, the viscosity of undercooled liquids is not known, yet knowledge of viscosity is required for crystallization calculations. Many researchers have used the Turnbull equation in error. Subsequent nucleation and crystallization calculations can be in error by many orders of magnitude. This demonstrates the requirement for better methods for interpolating and extrapolating the viscosity of undercooled liquids. This is also true for undercooled water. Since amorphous water ice is the predominant form of water in the universe, astrophysicists have modeled the crystallization of amorphous water ice with viscosity relations that may be in error by five orders-of-magnitude.

Source record↗

Undercooling of materials during solidification in space

A theoretical research program was undertaken on the under cooling and solidification of materials under variable external field conditions. A catalog of theories and models of nucleation of solid phases in the melt is provided, as is a discussion of the relation of undercooling to intermolecular potentials, the dependence of growth rate on undercooling, the influence of undercooling on liquid-solid interface stability and solid structure, the direct effects of external fields on melts, the relation of solid physical properties to structure and the role of nucleants in solidification. Results of the theoretical analysis of several experiments related to the space processing applications program are given, and recommendations for future experiments and further theoretical developments along with procedures for correlation of theory and experiment are specified.

Miller, R. I.↗

Solidification mechanism of highly undercooled metal alloys

Experiments were conducted on metal droplet undercooling, using Sn-25wt%Pb and Ni-34wt%Sn alloys. To achieve the high degree of undercooling, emulsification treatments were employed. Results show the fraction of supersaturated primary phase is a function of the amount of undercooling, as is the fineness of the structures. The solidification behavior of the tin-lead droplets during recalescence was analyzed using three different hypotheses; (1) solid forming throughout recalescence is of the maximum thermodynamically stable composition; (2) partitionless solidification below the T sub o temperature, and solid forming thereafter is of the maximum thermodynamically stable composition; and (3) partitionless solidification below the T sub o temperature with solid forming thereafter that is of the maximum thermodynamically metastable composition that is possible. The T sub o temperature is calculated from the equal molar free energies of the liquid solid using the regular solution approximation.

Shiohara, Y.↗

Containerless undercooling and solidification of bulk metastable Nb3Ge alloys

Experiments using containerless undercooling and low-gravity solidification of Nb(1-x)Ge(x) alloys for x=0.13-0.27 have been carried out in a 32-m drop-tube apparatus to study the feasibility of forming metastable Nb3Ge in bulk form. It is found that bulk samples (2-3 mm diam) of Nb-Ge alloys with 18-22% Ge can be undercooled by large amounts (300-500 K) and solidified in a containerless environment. Subsequent quenching of the solidified samples in oil helps preserve the metastable A-15 phase by removing the latent heat of fusion and quickly cooling the samples to a stable temperature below 1000 C. Even at an undercooling of less than 100 K, the superconducting transition temperature of the material is enhanced over the cast material by about 1 K.

Lacy, L. L.↗

Rapid solidification of highly undercooled alloy droplets

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.

Chu, M. G.↗

The Influence of Containerless Undercooling and Rapid Solid-State Quenching on the Superconductive and Magnetic Properties of Some Clustering Alloy Systems

The potential of the 100-meter drop-tube for producing materials with new and important properties by their rapid solidification containerless undercooling was investigated. Materials produced exhibit evidence of very rapid quenching. The importance of rapid quenching in producing materials of considerable scientific and technological interest is emphasized. It is indicated that containerless undercooling, using at first a drop tube and eventually a space-shuttle-serviced orbiting laboratory, will provide another powerful approach for rapid quenching. A special advantage of the drop tube is that the microgravity condition is imposed ballistically; it is therefore possible to obtain either spherical samples by allowing solidification to take place in flight, or splats by allowing the sample material while still in undercooled liquid form to impact a stationary quench plate.

Collings, E. W.↗

Dendritic Growth in Undercooled Melts

The kinetic and morphological behavior of systems solidifying at small undercooling were investigated with emphasis on the role of convective and diffusive transport and the influence of gravity. A data base was established for pure succinonitrile which permits a comprehensive check on diffusional dendrite growth theory and the development of scaling laws to extend the theory to other material systems. A departure from diffusional-controlled growth was observed which becomes more significant at smaller undercoolings. A shuttle experiment is prepared to test the theory at the low undercoolings where convective effects begin to dominate.

Glicksman, M. E.↗

Containerless Processing of Undercooled Melts

The physical mechanisms controlling liquid undercooling were studied for application to solidification processing methods. The undercooling potential of containerless processing was assessed on droplet samples of high melting temperature metals drop tube and drop tower facilities and in a laboratory-scale apparatus. New insight into nucleation and crystal growth will be obtained in undercooled liquids of high melting temperature iron and nickel-base systems. The processing parameters include melt superheat, droplet size and particle statistics and droplet surface coating. The solidification behavior is determined by thermal analysis and by structural and metallographic characterization.

Perepezko, J. H.↗

Undercooling of pure metals in a containerless, microgravity environment

The 105-m drop tube at NASA/Marshall Space Flight Center has been used in a series of undercooling experiments on pure metals. Ti, Zr, Nb, Mo, Rh, Hf, Ta, and Pt were undercooled 17-20 percent of the melting temperature in a containerless, microgravity environment. Ir and Ru were undercooled to 13 percent Tm. Sample sizes ranged from 175 to 880 mg.

Robinson, M. B.↗