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Proposed improvement for silicon crystal growing enables rapid heating of melt in vicinity of liquid-solid interface to compensate for decreases in melt temperature, to ensure uniform diameter and composition in ingot. Intended for growing large silicon ingots by Czochralski process, cylindrical single-crystal ingot pulled from molten silicon. Heating confined to small mass near growing crystal.
Understanding how liquid phase particles are engulfed or pushed during freezing of a monotectic is addressed. The additional complication is that the solid-liquid interface is nonplanar due to constitutional undercooling. Some evidence of particle pushing where the particles are the liquid phase of the montectic was already observed. Cellular freezing of the succinonitrile-glycerol system also occurred. Only a few compositions were tested at that time. The starting materials were not especially pure so that cellular interface observed was likely due to the presence of unkown impurities, the major portion of which was water. Topics addressed include: the effort of modeling the particle pushing process using the computer, establishing an apparatus for the determination of phase diagrams, and the measurement of the temperature gradients with a specimen which will solidify on the temperature gradient microscope stage.
The shape of a stationary solid-liquid interface in a temperature gradient near a grain boundary in a pure material is calculated for anisotropic crystal-melt surface tension and equal thermal conductivities of crystal and melt. Results are compared with those for the well-known problem of the two-dimensional equilibrium shape of a crystal. For small anisotropy, the resulting interface shapes have continuously turning tangents but differ in detail from the grain boundary groove shapes that have been calculated for isotropic surface tension. For larger anisotropy, the interface shapes have discontinuities in slope as a result of missing orientations.
Numerical experiments are used to study thermally driven flows which occur during vertical Bridgman crystal growth of a single component fluid. The solid-liquid interface was specified as parabolic and flow patterns were calculated for various insulation thicknesses, Grashof, Prandtl, and Biot numbers. When the melt is on top and the gravity vector is axially downward it is shown that flow persists as long as a radial temperature gradient is present. If the interface is convex, as viewed from the liquid, a single cell is observed. A concave interface exhibits multiple counterrotating cells. The insulation thickness and Grashof, Prandtl, and Biot numbers influence the flow in a quantitative manner.
Wyle Laboratories is currently designing and fabricating two KC-135 materials processing furnaces for Marshall Space Flight Center. The first of these, called the Rapid Melt/Rapid Quench (RM/RQ) Furnace, will be used to melt and resolidify Cu-, Al-, and Ni-based alloys and composites, all during the 20 to 30 seconds of low gravity (0.1 to 0.001 g) available in a single parabola of the KC-135. In addition, it will be capable of directional solidification of these alloys. The furnace can be configured for either liquid or gas quenching of the samples. The second furnace, called the Polymer Solidification Transparent (PST) Furnace, will use a wide range of sample translation rates to directionally solidify polymers and low-melting-point metals as the KC-135 flies a series of parabolic maneuvers. The use of transparent crucibles and an optics system between the hot and cold zones of the furnace will allow for high-resolution video monitoring of the solid-liquid interface during processing. It is hoped that the development of these two furnaces will lead to significant increases in understanding of interface kinetics, fluid flow, and heat transfer in materials during solidification in a low-gravity environment.
Numerical methods are used to study thermally/gravitationally induced convection during solidification. The primary object is aimed at understanding the flow field in the liquid metal pool due to convection. An Al-0.5Fe weight percent alloy is assumed to fill a small scale vertical rectangular enclosure model for this study. The Alternating Direction Implicit method and Successive Overrelaxation method are employed to solve these equations, which include the energy balance equation coupled with the mass and momentum equations. Both transient and steady state conditions under 1 g and low gravity (0.001 g) are investigated. The solutions for the two-dimensional isotherms and streamlines under 1 g conditions are graphically presented. The quantitative results show that the convection which occurs in the liquid metal pool is very small and is likely to have a negligible effect on the solute redistribution ahead of the solid-liquid interface.
A numerical method for solving phase change problems involving a moving heat source is presented and illustrated by a two-dimensional example. The method uses a fixed grid and does not require the implementation of the Stefan condition at the solid-liquid interface; the procedure can thus be easily implemented using existing fixed grid codes. The problem considered as an example involves natural convection flow in the molten metal during tungsten inert gas welding.
A directionally solidified PbCl2 material was prepared and analyzed and subsequently used to grow single crystals. It was found that silicon, halogens, sulfur, magnesium, and phosphorus were the hardest impurities to remove by the single-pass directional freezing. Single crystals grown from the purified material displayed good scattering beam quality and showed no absorption peaks between 0.30 to 20 microns. Direct photographic observations of the solid-liquid interface at several G/V (denoting the temperature gradient and the translation velocity, respectively) ratio values showed that, as the G/V ratio decreased, the interface varied from a smooth convex surface to dendritic.
Chill-block melt-spun ribbons of Ni-Mo alloys with Mo contents of 8 to 41.8 wt pct have been examined for microstructure and texture dependence on processing conditions. Linear features observed in grains solidified with a planar liquid-solid interface at the quench side of the ribbons have been identified to be due to the twins on the (111)gamma plane formed during solidification. Grain size variation with the wheel surface speed and the alloy composition has been studied. The crystallographic texture on the quench side and the free surface side of the ribbons has been investigated.
The purpose is to examine solidification in the LiCl-KCl system to determine if phenomena such as solute rejection can be obseved by laser schlieren imaging. Molten salts have attributes that make them attractive as physical models in solidification studies. With optical techniques of investigation such as schlieren imaging, it is possible to study fluid flow phenomena in molten salts and to watch the trajectory of the solid-liquid interface.
The dependence of microsegregation behavior on growth rate and thermal gradient has been examined in a Pb-8.4 at. pct Au alloy material partially directionally solidified and quenched. The composition of the quenched 'liquid' at the dendrite tip (Ct), that of the eutectic-like solid phase freezing from the interdendritic liquid at the base of dendrite (Cse), the volume fraction of this eutectic-like region (fe), and solute profiles in the interdendritic quenched liquid and ahead of the dendrite have been measured. Two dendritic growth models for solidification of a binary alloy melt in a positive thermal gradient at the liquid-solid interface, one for dendrites with 'minimum undercooled dendrite tip' and the other for an Ivantsov type of dendrite with 'marginally stable tip', have been examined for a quantitative comparison with measured values of Ct, Cse, and fe. Convection in the melt, possibly due to horizontal density gradients, is found to be a serious limitation for theoretical understanding of the observed experimental behavior and meaningful comparison of theories.
A mathematical model, which incorporates heat of mixing in the energy balance, has been developed to analyze the morphological stability of a planar solid-liquid interface during the directional solidification of a binary alloy. It is observed that the stability behavior is almost that predicted by the analysis of Mullins and Sekerka (1963) at low growth velocities, while deviations in the critical concentration of about 20-25 percent are observed under rapid solidification conditions for certain systems. The calculations indicate that a positive heat of mixing makes the planar interface more unstable, whereas a negative heat of mixing makes it more stable, in terms of the critical concentration.
The validity of the notion of absolute stability (AS) of a planar solid-liquid interface, proposed by Mullins and Sekerka (M-S, 1964), was tested using experimental data obtained for a number of dilute Ag-Cu and Sn-In alloys and for ultrahigh-purity succinonitrile. It is shown that the restriction applied by the M-S theory is satisfied during the steady-state planar solidification in an undercooled melt, provided the undercooling is quite small. The findings obtained on the Ag-Cu and Sn-In alloys are compared with early measurements by Davis and Fryzuk (1971) in dilute Sn-In alloys with 25 to 400 ppm additions of In.
The dependence of primary arm spacings on growth speed was investigated for cellular and dendritic arrays in Pb-10 wt percent Sn samples directionally solidified under a constant positive thermal gradient in the melt. The gradient of constitutional supercooling was varied from almost zero (near the break-down of the planar liquid-solid interface at small growth speeds, cellular morphology) to near unity (large growth speeds, dendritic morphology). The spatial arrangements of cells and dendrites, as given by their coordination number, are not very different from each other. It appears that primary arm spacing maxima and the cell to dendrite transition are strongly influenced by the magnitude of the solute partition coefficient. The planar to cellular bifurcation is supercritical in Pb-Sn which has a high partition coefficient, as compared to the subcritical behavior reported in Al-Cu and succinonitrile-acetone, both of which have low partition coefficients. The primary arm spacing model due to Hunt agrees with the experimentally observed trend for the whole growth regime. There is a good quantitative agreement at higher gradients of supercooling. However, the model overpredicts the primary arm spacings at low gradients of constitutional supercooling.
The dependence of primary arm spacings on growth speed was investigated for cellular and dendritic arrays in Pb-10 wt percent Sn samples directionally solidified under a constant positive thermal gradient in the melt. The gradient of constitutional supercooling was varied from almost zero (near the break-down of the planar liquid-solid interface at small growth speeds, cellular morphology) to near unity (large growth speeds, dendritic morphology). The spatial arrangements of cells and dendrites, as given by their coordination number, are not very different from each other. It appears that primary arm spacing maxima and the cell to dendrite transition are strongly influenced by the magnitude of the solute partition coefficient. The planar to cellular bifurction is supercritical in Pb-Sn which has a high partition coefficient, as compared to the subcritical behavior reported in Al-Cu and succinonitrile-acetone, both of which have low partition coefficients. The primary arm spacing model due to Hunt agrees with the experimentally observed trend for the whole growth regime. There is a good quantitative agreement at higher grdients of supercooling. However, the model overpredicts the primary arm spacings at low gradients of constitutional supercooling.
New developments in x-ray radiography that may be applicable to containerless experimentation are presented. The two features discussed are the use of radiography to determine the position and shape of the solid-liquid interface and, with the aid of appropriate markers, the flow patterns in either the surface or bulk of the liquid state. Both surface energy and fluid viscosity measurements can be made with the aid of the described radiographic system.
Hg(0.80)Cd(0.20)Te crystals were grown vertically in a transverse magnetic field by directional solidification. The effect of a magnetic field on the nature of fluid flow in the melts was investigated by measuring compositional variations along the axial and radial directions of the grown ingots. Magnetic field effects were shown to be significant over the entire field range employed (i.e., 2 to 5 kG). The axial compositional profiles (determined by precision density measurements) showed an abrupt decrease in the mole fraction of CdTe when the field was applied. Radial compositional mapping by IR transmission and X-ray energy dispersion spectrometry indicated that the solid-liquid interface evolved through three stages when the field was applied (i.e., from a radially symmetric concave interface to an off-center concave shape when the field was initially applied, then to a tilted plane, and, finally, to an off-center concave interface). The axial compositional profile of an Hg(0.84)Zn(0.16)Te ingot showed similar field effects.
A gauging system is proposed to enable monitoring of slush density, solid-liquid interface, and slush level as well as its flow rate. It is based on the principle that the electromagnetic radiation mass attenuation coefficient of a multiphase chemical compound is constant for all relative phase concentrations. Results showing the essential constancy of mass attenuation coefficients for single-phase water vapor, liquid water, ice, and multiphase mixtures of water/ice are described.