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At least 1,153 records · Page 64

Steady state growth and segregation under zero gravity: InSb

It was established that ideal diffusion controlled steady state conditions, never accomplished on earth, were achieved during the growth of Te-doped InSb crystals in Skylab. Surface tension effects were found to establish non-wetting conditions under which free surface solidification took place in confined geometry. It was further found that, under forced contact conditions, surface tension effects led to the formation of surface ridges (not previously observed on earth) which isolated the growth system from its container. In addition, it was possible for the first time to identify unambiguously: the origin of segregation discontinuities associated with facet growth, the mode of nucleation and propagation or rotational twin boundaries, and the specific effect of mechanical-shock perturbations on segregation. The results obtained prove the advantageous conditions provided by outer space. Thus, fundamental data on solidification thought to be unattainable because of gravity induced interference on earth are now within reach.

Witt, A. F.↗

Processing eutectics in space

Studies which have been done in an earth-based laboratory environment have generally not yielded specimens with the degree of perfection required of the eutectic microstructure to provide test data to evaluate their nonstructural applications. It has been recognized that the low-g environment of an orbiting space laboratory provides a unique environment to re-examine the process of solidification with the goal of producing better microstructures. The objective of this program is to evaluate the feasibility of using the space environment for producing eutectics with microstructures which can be of value on earth. In carrying out this objective, evaluative investigations were carried out on the technology of solidification in a 1-g environment to provide sound baseline data for planning space laboratory experiments.

Douglas, F. C.↗

Characterization of nickel-copper alloy specimens processed as a part of the M553 sphere forming experiment during the Skylab 1 and 2 flight

Both processed nickel-copper alloy specimens apparently completely melted by the electron beam in the Skylab M512 materials processing facility and either floated free in space, but collided with some smooth flat surface before solidifying, or remained attached to its support post during solidification. Both specimens had a smooth flat area on the surface due to this adherence during solidification. The nominal composition of the alloy before processing in space was 70 percent Ni and 30 percent Cu. Tests show that a considerable amount of copper was lost during processing by evaporation. It was further found that less copper was present in the cap areas, particularly at the surface, than was in the remainder of the specimens. The microchemistry of the dendrites and interdendritic regions, however, is in agreement with the phase diagram for this alloy. The measured densities of these specimens were less than the theoretical density of the alloy due to the amount of porosity present, however, no large voids were found by radiographic techniques.

Hubbard, J. L.↗

Fluid flow effects on crystalline perfection

Optimum solidification parameters for the production of highly perfect copper crystals by Czochralski growth are sought along with the documentation of crystal imperfections under various growth conditions. X-ray techniques which do not in their application produce defects and which allow the characterization of imperfections in single crystals are chosen to assess crystal perfection. The X-ray techniques employed ranged from ordinary Laue photography through Borrmann topography to double-crystal scanning diffractometry, thus allowing crystals with a wide variation in perfection to be studied. As a set of controllable solidification parameters, the rotation of the seed and of the melt and the diameter of the bottleneck are chosen. X-ray diffraction topographs are analyzed along with the data obtained from rocking curve measurements. Tables of growth conditions and quantitative data of rocking curve widths are presented.

Kuriyama, M.↗

Indium antimonide crystal growth experiment M562

It was established that ideal diffusion controlled steady state conditions, never accomplished on earth, were achieved during the growth of Te-doped InSb crystals in Skylab. Surface tension effects led to nonwetting conditions under which free surface solidification took place in confined geometry. It was further found that, under forced contact conditions, surface tension effects led to the formation of surface ridges (not previously observed on earth) which isolated the growth system from its container. In addition, it was possible, for the first time, to identify unambiguously: the origin of segregation discontinuities associated with facet growth, the mode of nucleation and propagation of rotational twin boundaries, and the specific effect of mechanical-shock perturbations on segregation. The results obtained prove the advantageous conditions provided by outer space. Thus, fundamental data on solidification thought to be unattainable because of gravity-induced interference on earth are now within reach.

Gatos, H. C.↗

Metallurgical processing in space

Research in metallurgical processing to study the effects of reduced gravity started with Apollo 14 and advanced with Skylab. Experiments provided specimens for analysis which solidified while constrained and while freely floating, which contained a mixture of normally immiscible materials, demonstrated enhanced capillary flow, solubility and ordered growth of a directionally solidified eutectic. The smaller, equiaxed grain structure obtained in reduced gravity compared to the larger, elongated grains obtained in one gravity indicate a difference in convection due to gravity in constrained solidification. Freely floating nickel alloy specimens showing metallic gas evolution at low pressure and reduced gravity suggest reduced pressure reactions which cannot occur on earth even in high vacuum chambers due to the hydrostatic head in the molten metal. Directionally solidified eutectics showed fewer termination defects when grown in reduced gravity. These are a few of the differences observed due to reduced gravity which could have important consequences on the future of metallurgy. In this paper we attempt to correlate the results of several Skylab solidification experiments.

Mckannan, E. C.↗

Containerless processing of single crystals in low-G environment

Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.

Walter, H. U.↗

Electromagnetic levitation facility incorporating electron beam

An electromagnetic levitation apparatus incorporating an electron beam for auxiliary heating and melting has been developed for experiments on containerless vacuum purification and undercooled solidification of high melting materials. Stable levitation of 10-g specimens of molten tungsten has been achieved and a variety of containerless solidification experiments is being performed, including pure polycrystalline castings and single tungsten crystals grown from the undercooled levitated melts.

Wouch, G.↗

Skylab M551 metals melting experiment

The objectives of the M551 Metals Melting Experiment were to: (1) study behavior of molten metal, (2) characterize metals melted and solidified in the low gravity space environment compared to one-gravity of earth, and (3) determine feasibility of joining metals in space. The experiment used the electron beam (EB) and chamber of the M512 apparatus to make a dwell puddle and a melt in a rotating disc of varying thickness. Hence, the EB performed cut-through, full and partial penetration melts, in addition to a resolidified button. The three disc materials were aluminum 2219-T87, 304 stainless steel, and pure tantalum to provide a wide range of density and melting conditions. Observations to date include the proof that EB welding, cutting, and melting can be done successfully in low gravity. Earlier, some welding authorities had postulated that without gravity the EB would force the molten puddle out of contact. However, the experiment proved that surface tension forces predominate. From the viewpoint of cast-solidification, small, equiaxed grains in Skylab specimens compared to large, elongated grains in ground based specimens were observed. The former are thought to be associated with constitutional supercooling and nucleation where the latter are associated with dendritic solidification. In further support of the more equiaxed grain growth in Skylab, symmetric subgrain patterns were frequently observed where there was much less symmetry in ground based specimens.

Poorman, R. M.↗

Halide eutectic growth experiment MA-131

Fiberlike sodium chloride/lithium fluoride eutectic mixtures have been produced on earth and in space by the directional solidification technique. Macroscopic and microscopic examinations were made on longitudinal and transverse sections of Apollo Soyuz Test Project space grown and earth grown ingots. It was found that samples grown in space have a higher percentage of fibers alined with the growth axis. The enhanced alinement of fibers is attributed to the absence of convection currents in the liquid during solidification. Optical transmittance measurements of transverse sections of the space grown and earth grown ingots were performed with an infrared spectrometer. For a given sample thickness, the highest transmittance was obtained from ingots grown in space. For samples of different thicknesses, grown either in space or on earth, it was found that the thinner the sample, the higher the transmittance. This is in agreement with the general optical property of transparent materials.

Yue, A. S.↗

Space processing float zone thermal analysis

Thermal analysis (BETA) computer program adaptations were prepared to analyze phase change histories in crystal specimens. The first program (BETA-CYL) treats right circular cylinder configurations and the second, more general, program (BETA-BOR) treats a generalized body-of-revolution configuration. A series of computer runs were made for silicon material to determine boundary conditions which produce flat solidification interfaces while, at the same time, minimizing peak temperatures in the molten zone. Flat solidification interfaces are a goal believed by some investigators to be required to produce high quality semiconductor materials. The thermal effects of convection in a molten zone were examined and found to be negligible in comparison to the conduction heat transfer of the melt.

Pogson, J. T.↗

Transverse tensile and stress rupture properties of gamma/gamma prime-delta directionally solidified eutectic

Tensile and stress rupture properties were determined primarily at 760 C for specimens oriented at various angles (0 deg, 10 deg, 45 deg, and 90 deg) from the solidification direction of bars and/or slabs of the Ni-20Cb-6Cr-2.5A (gamma/gamma prime-delta) eutectic. Threaded-head specimens yielded longer rupture lives with significantly less scatter than did tapered-head specimens. Miniature specimens are suitable for determining traverse tensile and rupture properties of 1.2 centimeter diameter bar stock. The 300 hour rupture stress at 760 C for specimens oriented at 10 deg from the solidification direction was reduced from 740 to 460 MPa, and to 230 MPa for material oriented at either 45 deg or 90 deg.

Gray, H. H.↗

The grape cluster, metal particle 63344,1

The grape cluster metal particle 63344,1 found in lunar coarse fines is examined using the scanning electron microscope (SEM), electron microprobe, and an optical microscope. This metal particle is approximately 0.5 cm in its largest dimension and consists of hundreds of metallic globules welded together to form a structure somewhat like a bunch of grapes. Electron microprobe analysis for Fe, Ni, Co, P, and S in the metal was carried out using wavelength dispersive detectors. No primary solidification structure is observed in the globules, and the particle is slow cooled from the solidification temperature (nearly 1300 C) taking days to probably months to reach 600 C. Two mechanisms for the formation of globules are proposed. One mechanism involves the primary impact of an iron meteorite which produces a metallic liquid and vapor phase. The second mechanism involves the formation of a liquid pool of metal after impact of an iron meteorite projectile followed by a secondary impact in the liquid metal pool.

Goldstein, J. I.↗

Evolution of major mineral compositions and trace element abundances during fractional crystallization of a model lunar composition

The evolution of major mineral compositions and trace element abundances during perfect fractional crystallization of a model lunar magma ocean was calculated. The minerals in the model lunar composition were olivine, orthopyroxene, clinopyroxene, and plagioclase. Lunar bulk composition data, major mineral/melt equilibria data, and trace element partition data were taken from published sources. The results show olivine beginning to crystallize at 1380 C. Approximately 50% of the system crystallizes as olivine. From 50 to 60% solidification, orthopyroxene crystallizes alone. During the final 40% solidification, Ca-rich clinopyroxene and plagioclase crystallize together. Various changes in composition of all these minerals are also noted during the process. Concomitant evolution of major element abundances in the melt is followed along with that of trace element abundances. Consequences of the results for constraints on some aspects of the composition of the lunar magma ocean and of the primitive moon are discussed.

Drake, M. J.↗

Summary of the pre-ASTP results

A general overview of materials experiments done on several Apollo missions and Skylab as well as the ground research that led to these experiments is given. Demonstrations of composite solidification, electrophoresis, and fluid flow were developed for Apollo. Fourteen different experiments in metal processing and single crystal growth were done in the space processing facility on Skylab. Metals were melted and solidified in a variety of configurations using different methods of heating to produce improved alloys and composite materials. Single crystals were grown by directional solidification and vapor transport to achieve uniform crystalline perfection, decreased structural defects, and homogeneity of the dopant material.

Snyder, R. S.↗

Microstructure and composition of InSb-GaSb ingots directionally solidified aboard Skylab

InSb-GaSb solid solution ingots prepared by directional solidification aboard Skylab and on earth consist of twins with (111) twin planes parallel to the direction of solidification and growth directions that lie along 211, 110, or 321 crystallographic directions. Significant fractions of several ingots prepared aboard Skylab were solidified from melts that were not in contact with container walls, resulting in convection driven by surface tension gradients in the melt and corresponding radially-symmetric composition variations in the ingot. In these regions, adjacent twins exhibit marked differences in indium content, indicating a substantial dependence of composition on crystallographic orientation.

Lefever, R. A.↗

Structure-property relationships in eutectic composites

The preparation of a composite material of eutectic composition directly from the molten state is investigated. The manufacture of eutectic composites by unidirectional solidification is reviewed, and it is shown how two-phase composite structures of given relative volume fraction can be produced with a range of particle sizes. Crystallographic relationships and the thermal stability of interfaces in controlled eutectic structures are examined, the mechanical behavior of aligned eutectic microstructures is discussed, and characteristics of eutectic composites having mechanical properties of engineering significance are evaluated. Specific properties of the Ni-Nb eutectic alloy are reviewed to demonstrate the effect of structure control (through directional solidification) on the mechanical response of a eutectic composite. It is noted that unidirectionally solidified eutectic composites possess highly aligned and thermally stable microstructures and also exhibit excellent combinations of strength and ductility to very high temperature levels.

Hertzberg, R. W.↗

Distribution of molecular weight in glyceride polymerizates or aggregates of them after contact with lunar grains

An attempt is made to report on experiments in which a molecular-weight increase was determined in thin layers of triglyceride-containing glycerides after thin-layer contact for two years with lunar topsoil grains at 25 C without any thermal activation. It is noted that solidification was observed on both dielectric grains and metal-rich areas and that changes in viscosity and molecular weights were first detected by solidification of surface layers. Gel permeation chromatography is described which detected a general shift of the Gaussian distribution of the molecular-weight data toward generally higher molecular weights as well as an increase in mean molecular weight. Reaction mechanisms are considered, and results of spectrographic analysis are cited which support the interpretations of the molecular-weight data.

Asunmaa, S. K.↗