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The present industrial requirements for float zone silicon are summarized. Developments desired by the industry in the future are reported. The five most significant problems faced today by the float zone crystal growth method in industry are discussed. They are economic, large diameter, resistivity uniformity, control of carbon, and swirl defects.
Presentations made on space based float zone crystal growth and melt behavior are summarized and handouts illustrating the presentations are presented.
Scientific experiments conducted in a low-gravity environment make it possible to study effects, such as surface tension-driven flows, which are often masked by buoyancy-driven flows. A summary is provided of several early experiments which demonstrate that unwanted convective flows can be effectively suppressed in experiments conducted in orbiting spacecraft. Possible applications of low-G processing are discussed, taking into account Bridgman growth of solid solution alloy-type semiconductors, Bridgman growth of eutectic systems, and float-zone crystal growth. The control of macrosegregation and phase separation in castings is considered, giving attention also to containerless melting and solidification. A description of experiment facilities and opportunities is provided.
Suitably chosen liquid encapsulant placed around melt zone in float-zone crystal-growth system performs four important functions enhancing purity and reducing strains and dislocations in final crystal. In new technique, grow dislocation-free crystals with precisely controlled composition even from materials not amenable to conventional float-zone crystal-growth method. Support provided by encapsulant make it practical to process materials of low surface tension.
Recent advances in CO2 laser technology and its applications are examined. Topics discussed include the excitation of CO2 lasers by microwave discharge, a compact RF-excited 12-kW CO2 laser, a robotic laser for three-dimensional cutting and welding, three-dimensional CO2-laser material processing with gantry machine systems, and a comparison of hollow metallic waveguides and optical fibers for transmitting CO2-laser radiation. Consideration is given to an aerodynamic window with a pump cavity and a supersonic jet, cutting and welding Al using a high-repetition-rate pulsed CO2 laser, speckle reduction in CO2 heterodyne laser radar systems, high-power-laser float-zone crystal growth, melt dynamics in surface processing with laser radiation, laser hardfacing, surface melting of AlSi10Mg with CO2 laser radiation, material processing with Cu-vapor lasers, light-induced flow at a metal surface, and absorption measurements in high-power CW CO2-laser processing of materials.
A vertical melt column set up between an upper heating rod and a lower sample rod, i.e., the so-called half-zone system, is a convenient experimental tool for studying convection in the melt in floating-zone crystal growth. In order to help understand the convection observed in the melt column, a computer model has been developed to describe steady state, axisymmetrical thermocapillary flow and natural convection in the melt. The governing equations and boundary conditions are expressed in general non-orthogonal curvilinear coordinates in order to accurately treat the unknown melt/solid interface as well as all other physical boundaries in the system. The effects of key dimensionless variables on the following items are discussed: (1) convection and temperature distribution in the melt; (2) the shape of the melt/solid interface; (3) the height of the melt column. These dimensionless variables are the Grashof, Marangoni and Prandtl numbers.
In this paper we consider an isothermal finite liquid bridge under zero-gravity. A sinusoidal interfacial shear stress drives a nonparallel flow in the bridge. The linear stability of this flow to three-dimensional disturbances (which may deform the cylindrical gas-liquid interface) is determined numerically by solving an elliptic eigenvalue problem. Previous results on shear stabilization of capillary break-up of axially unbounded cylindrical interfaces containing a parallel flow are hereby extended to a nonparallel flow. The turning flow regions influence the stability significantly. However, for the particular cases considered, a small area in parameter space remains where the capillary instability is suppressed through interfacial shear. Second, non-axisymmetric oscillatory instabilities are found which originate from an interaction of the interface deformation and the basic flow. These instabilities may be the isothermal limit of the oscillatory instabilities observed in float-zone crystal growth.
The objectives are to: (1) Understand the influence in low gravity of flow on interface shape. For example, document and control the influence of axial flow on the Plateau-Rayleigh instability of a liquid bridge; and (2) Extend the ground-based density-matching technique of low gravity simulation to situations with flow; that is, develop Plateau chamber experiments for which flow can be controlled. Containerless containment of liquid by surface tension has broad importance in low gravity. For space vehicles, the behavior of liquid/gas interfaces is crucial to successful liquid management systems. In microgravity science, free interfaces are exploited in various applications. Examples include float-zone crystal growth, phase separation near the critical point of liquid mixtures (spinoidal decomposition) and quenching of miscibility gap molten metal alloys. In some cases, it is desired to stabilize the capillary instability while in others it is desired to induce capillary breakup. In all cases, understanding the stability of interface shape in the presence of liquid motion is central.
We have found that it is possible to have steady thermocapillary flows in any of these three systems provided the liquid layer is not too thin or the surface tension is not too small. If these conditions are not met, then no steady solutions are possible and the film thins and approaches a condition of rupture near the hot end. Future work on these problems will include the effect of liquid inertia in the calculations for the cylindrical cavity. The stabilization effect of inertia may offset the destabilization effect inherent in the cylindrical geometry and result in a stable film flow on the cylinder. This type of behavior could be very significant in terms of understanding the stability of thermocapillary flow in liquid bridges and in the float-zone crystal growth process.
Tests are planned in the low gravity environment of the International Space Station (ISS) of new methods for the suppression of the capillary instability of liquid bridges. Our suppression methods are unusual in that they are not limited to liquid bridges having very special properties and may impact a variety of low-gravity and earth-based technologies. There are two main approaches to be investigated: (1) Passive Acoustic Stabilization (PAS); and (2) Active Electrostatic Stabilization (AES). In PAS, the suppression of the mode growth is accomplished by placing the bridge in an acoustic field having the appropriate properties such that the acoustic radiation pressure automatically pulls outward on the thinnest portion of the bridge. In AES, the bridge deformation is sensed optically and counteracted by actively adjusting the electrostatic Maxwell stresses via two ring electrodes concentric with the slightly conducting bridge to offset the growth of the unstable mode. While the present work emphasizes cylindrical bridges, the methods need not be restricted to that case. The methods to be explored are relevant to the suppression of capillary instabilities in floating zone crystal growth, breakup of liquid jets and columns, bubbles, and annular films as well as the management of coolants or propellants in low-gravity.
Immiscible fluid layers are found in a host of applications ranging from materials processing, for example the use of encapsulants in float zone crystal growth technique and a buffer layer in industrial Czochralski growth of crystals to prevent Marangoni convection, to heat transfer phenomena in day-to-day processes like the presence of air pockets in heat exchangers. In the microgravity and space processing realm, the exploration of other planets requires the development of enabling technologies in several fronts. The reduction in the gravity level poses unique challenges for fluid handling and heat transfer applications. The present work investigates the efficacy of controlling thermal convective flow using magnetic fluids and magnetic fields. The setup is a two-layer immiscible liquids system with one of the fluids being a diluted ferrofluid (super paramagnetic nano particles dispersed in carrier fluid). Using an external magnetic field one can essentially dial in a volumetric force - gravity level, on the magnetic fluid and thereby affect the system thermo-fluid behavior. The paper will describe the experimental and numerical modeling approach to the problem and discuss results obtained to date.
Understanding the mechanism of detached Bridgman growth and establishing the growth of large scale germanium-silicon crystals by the float-zone technique are the key points of the project "RDGS - Reduction of Defects in Germanium-Silicon". The contact angle of the melt and the growth angle of the crystal are essential parameters which allow a controlled use of detached growth. The contact angle was determined for a variety of different substrates and melt compositions; pBN showed the highest value for pure germanium as well as for germanium-rich GeSi melts. The growth angle of Ge(sub 0.95) Si(sub 0.05) was measured to be 8.5-10.5 degrees which concurs with the values of pure germanium and silicon, respectively. The temperature dependence and the concentration dependence of the surface tension were determined for concentrations up to 10at% silicon (partial derivative (gamma)/partial derivative T=-0.08 (raised dot) 10(exp -3)N/m (raised dot) K, partial derivative (gamma)/partial derivative (C)=2.2 (raised dot) 10(exp -3)N/m (raised dot) at%). Using these values, the critical Marangoni number indicating the transition to time-dependent thermocapillary flow will be exceeded for the growth of large scale float-zone crystals onboard the ISS. Therefore, suitable tools for flow control are required.
Room-temperature slip in zone-melted tungsten single crystals - plastic deformation
Colorless transparent apoferritin (Mr = 450KDa) crystals have been grown from gel with Cd(2+) as precipitant in the presence of reddish brown-colored ferritin dimers (Mr = 900KDa). In agreement with our previous measurements, showing preferential trapping of dimers (distribution coefficient K = 4), the apoferritin crystals become strongly colored while the gel solution around them became nearly colorless. The depth of the depletion with respect to the colored dimer impurity allowed us to visualize the impurity depletion zone. Depletion with respect to impurity as compared to the crystallizing protein is discussed.
Single crystals of the metallic Ruddlesden-Popper trilayer nickelates R 4 Ni 3 O 10 ( R = La , Pr ) were successfully grown using an optical-image floating zone furnace under oxygen pressure ( p O 2 ) of 20 bar for La 4 Ni 3 O 10 and 140 bar for Pr 4 Ni 3 O 10 . Furthermore, a combination of synchrotron and laboratory x-ray single-crystal diffraction, high-resolution synchrotron x-ray powder diffraction and measurements of physical properties revealed that R 4 Ni 3 O 10 ( R = La , Pr ) crystallizes in the monoclinic P 2 1 / a ( Z = 2 ) space group at room temperature, and that a metastable orthorhombic phase ( Bmab ) can be trapped by postgrowth rapid cooling. Both La 4 Ni 3 O 10 and Pr 4 Ni 3 O 10 crystals undergo a metal-to-metal transition (MMT) below room temperature. In the case of Pr 4 Ni 3 O 10 , the MMT is found at 157.6 K. For La 4 Ni 3 O 10 , the MMT depends on the lattice symmetry: 147.5 K for Bmab vs 138.6 K for P 2 1 / a . Lattice anomalies were found at the MMT that, when considered together with the pronounced dependence of the transition temperature on subtle structural differences between Bmab and P 2 1 / a phases, demonstrate a not insignificant coupling between electronic and lattice degrees of freedom in these trilayer nickelates.
Two rare spinel-bearing Al-rich chondrules are identified in chondrite finds from Roosevelt County, New Mexico-RC 071 (L4) and RC 072 (L5). These chondrules have unusual mineralogies dominated by highly and asymmetrically zoned Al-Cr-rich spinels. Two alternatives exist to explain the origin of this zoning-fractional crystallization or metamorphism. Fractional crystallization formed the zoning of the trivalent cations and caused a localized depletion in chromites around the large Al-Cr-rich spinels. Diffusive exchange and partitioning of Fe and Mg between olivine and spinel during parent-body metamorphism can explain the asymmetric zoning of these elements. The bulk compositions of the chondrules suggest affinities with the Na-Al-Cr-rich chondrules, as would be expected from the abundance of Al-Cr-rich spinels. The most important factors are the temperature to which the molten chondrule was heated and the cooling rate during crystallization. These two chondrules cooled rapidly from near the liquidus, as indicated by the zoning, occurrence and sizes of spinels, radiating chondrule textures and localized chromite depletions.
The single-crystal lead tin telluride (PbSnTe) semiconductor is most promising as a laser radiation element and infrared detecting element in the far infrared region. However, it is very difficult to grow a large single crystal with a homogeneous composition on Earth because the elements have a very strong tendency to separate from each other in the molten phase due to differences in their specific gravities and melting points. The purpose of the experiment is to grow a single crystal of PbSnTe by a traveling zone method in microgravity, and to study the spatial fluctuation of the composition and the electrical properties of the crystal.
CuFeO 2 single crystals up to 50 mm in length and up to 10 mm in diameter were grown by the optical floating-zone method. Stoichiometric polycrystalline rods with a diameter of 6–12 mm were used as feed materials to produce crystals of sufficient size to be used as substrates for the growth of thin films of delafossites. For stable growth along the c-axis, low growth rates of 0.4 mm/h are necessary. Due to the incongruent melting behavior of CuFeO 2 , a stable melt zone requires adjustment of the lamp power during growth. The melting of CuFeO 2 is not simply incongruent because the thermodynamic equilibrium includes more than two solid phases and the melt; the gas phase is also involved. Finaly, the crystals were characterized by X-ray diffraction and X-ray fluorescence measurements.