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The power needed to zone silicon crystals by radio frequency heating was analyzed. The heat loss mechanisms are examined. Curves are presented for power as a function of crystal diameter for commercial silicon zoning.
Floating-zone crystal growth under microgravity, though free from natural convection, can still be susceptible to Marangoni convection. The use of a ring heater in contact with most of the surface of the melt zone, has recently been considered as one way of reducing Marangoni convection in the melt zone. In order to study Marangoni convection in the melt zone in this modified floating-zone crystal growth process, a half-zone system was adopted. Computer simulation and direct observation of Marangoni convection in the half-zone system were carried out for two different cases. In the first case, the surface of the melt zone was completely free, while in the second it was mostly in contact with a quartz ring. The results of computer simulation and direct observation both indicated that in the second case Marangoni convection was significantly reduced near the melt/solid interface as well as in the bulk melt.
The objective was to study thermocapillary convection in a transparent floating zone. The floating zone process is a unique process for crystal growth in that the melt is free from contamination by a crucible. Microgravity is ideal for the floating zone process because there is no significant gravity to cause the molten zone to collapse as under normal gravity. Since gravity-induced buoyancy convection is suppressed, surface- tension-induced thermocapillary convection dominates in the molten zone. In floating zone crystal growth, thermocapillary convection can be strong enough to cause formation of dopant striations and a convex growth front - both are undesirable in crystal growth.
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.
Floating zone refining or crystal growth is carried out by providing rapid relative rotation of a feed rod and finish rod while providing heat to the junction between the two rods so that significant forced convection occurs in the melt zone between the two rods. The forced convection distributes heat in the melt zone to allow the rods to be melted through with a much shorter melt zone length than possible utilizing conventional floating zone processes. One of the rods can be rotated with respect to the other, or both rods can be counter-rotated, with typical relative rotational speeds of the rods ranging from 200 revolutions per minute (RPM) to 400 RPM or greater. Zone refining or crystal growth is carried out by traversing the melt zone through the feed rod.
During a floating zone experiment involving the growth of indium on a recent orbiter mission, (STS 32) oscillation of the zone shapes were observed to occur in response to the background acceleration. An understanding of the nature of the response of the zone shape to forced (g-jitter) oscillations and predictions of its impact on future experiments is of great interest not only to the PI's but to other commercial and academic investigators who plan to fly similar experiments in the orbiter and on space station. Motivated by this, a 15 month study was undertaken to analyze the nature of the g-sensitivity of the STS 32 floating zone crystal growth experiment. Numerical models were used to describe the time-dependent free surface motion of the zone as it responds to the spacecraft residual acceleration. Relevant experimental data concerning the acceleration environment was obtained from the Honeywell in Space Accelerometer (HISA) investigators through MSFC's ACAP program and processed and analyzed. For the indium floating zone experiment, a series of calculations were made using time-dependent axial accelerations g(t). The form of g(t) included simple sinusoidal disturbances as well as actual data (subject to appropriate filtering) measured on the STS 32 mission. Focus was on the calculation of the response of the free surface of the zone as well as the internal flows and internal heat transfer. The influence of solidification on the response of the zone shape was also examined but found to be negligible.
The solvent-laser heated floating zone (solvent-LHFZ) growth method is being developed to grow long single crystal SiC fibers. The technique combines the single crystal fiber growth ability of laser heated floating zone with solvent based growth techniques (e.g. traveling solvent method) ability to grow SiC from the liquid phase. Initial investigations reported in this paper show that the solvent-LHFZ method readily grows single crystal SiC (retains polytype and orientation), but has a significant amount of inhomogeneous strain and solvent rich inclusions.
The solvent-laser heated floating zone (solvent-LHFZ) growth method is being developed to grow long single crystal SiC fibers. The technique combines the single crystal fiber growth ability of laser heated floating zone with solvent based growth techniques (e.g. traveling solvent method) ability to grow SiC from the liquid phase. Initial investigations reported in this paper show that the solvent-LHFZ method readily grows single crystal SiC (retains polytype and orientation), but has a significant amount of inhomogeneous strain and solvent rich inclusions.
The float zone (FZ) growth method for silicon crystallization has advantages and disadvantages when compared to the other principal growth method, the Czochralski (CZ) technique. CZ growth is attractive for the following reasons: large diameters, high single crystal yields, low thermal gradients, low operator skill requirements, efficient power utilization, and low feed material costs. Some areas where FZ growth is advantageous include high purity, axial resistivity uniformity (on a macroscale), visibility of the growth region, low consumable material costs, and high growth rates.
Floating zone methods have potential applications in growing single high-quality semi-conductor crystals. In this method, melts can be sustained without containers and, therefore, are free from contamination from the containers. The main objective of this project is to use the Image Furnace to study a large diameter, (20 mm) single crystal of InSb under microgravity conditions. The behavior of the liquid column is recorded on the VTR tapes and is compared with what is expected theoretically. The single crystal grown in space is characterized by comparing it with single crystals grown on the ground with respect to crystallographic and electronic properties. The goal of this project is to confirm the effects of the microgravity on the single crystals.
The process and apparatus for growing crystals using float zone techniques are described. A rod of crystalline materials is disposed in a cylindrical container, leaving a space between the rod and container walls. This space is filled with an encapsulant, selected to have a slightly lower melting point than the crystalline material. The rod is secured to a container end cap at one end and to a shaft at its other end. A piston slides over the rod and provides pressure to prevent loss of volatile components upon melting of the rod. Prior to melting the rod the container is first heated to melt the encapsulant, with any off-gas from this step being vented to a cavity behind the piston. The piston moves slightly forward owing to volume change upon melting of the encapsulant, and the vent passageway is closed. The container is then moved longitudinally through a heated zone to progressively melt sections of the rod as in conventional float zone processes. The float zone technique may be used in the microgravity environment of space.
The purposes of the float zone working group are summarized. Present and proposed U.S. and European research programs are listed, and power needs for float zoning surveyed. A 1981 to 1991 schedule for development efforts is presented.
To produce superior crystals of cadmium telluride, floating zone melting in space has been proposed. Techniques required for floating zone melting of cadmium telluride are being developed. We have successfully float-zoned cadmium telluride on earth using square rods. A resistance heater was constructed for forming the molten zone. Evaporation of the molten zone was controlled by adding excess cadmium to the growth ampoule combined with heating of the entire ampoule. An effective method to hold the feed rod was developed. Slow rotation of the growth ampoule was proven experimentally to be necessary to achieve a complete symmetric molten zone. Most of the resultant cylindrical rods were single crystals with twins. Still needed is a suitable automatic method to control the zone length. We tried a fiber optical technique to control the zone length, but experiments showed that application of this technique to automate zone length control is unlikely to be successful.
A summary of the Analytical Float Zone Experiment System (AFZES) concept is presented. The types of experiments considered for such a facility are discussed. Reports from various industrial producers and users of float zone material are presented. Special emphasis is placed on state-of-the-art developments in low gravity manufacturing and their applications to space processing.
Hear and mass transfer in float-zone processing are strongly influenced by convective flows in the zone. They are caused by buoyancy convection, thermocapillary (Marangoni) convection, or artificial sources such as rotation and radio frequency heating. Flows in conducting melts can be controlled by the use of magnetic fields, either by damping fluid motion with static fields or by generating a def@ned flow with rotating fields. The possibilities of using static and rotating magnetic fields in silicon floating-zone growth have been investigated by experiments in axial static fields up to ST and in transverse rotating magnetic fields up to 7.S mT. Static fields of a few 100 MT already suppress most striations but are detrimental to the radial segregation by introducing a coring effect. A complete suppression of dopant striations caused by time-dependent thermocapillary convection and a reduction of the coring to insignificant values, combined with a shift of the axial segregation profile towards a more diffusion-limited case, is possible with static fields ? 1T. However, under certain conditions the use of high axial magnetic fields can lead to the appearance of a new type of pronounced dopant striations, caused by thermoelec:romagnetic convection. The use of a transverse rotating magnetic field influences the microscopic segregation at quite low inductions, of the order of a few mT. The field shifts time-dependent flows and the resulting striation patterns from a broad range of low frequencies at high amplitudes to a few high frequencies at low amplitudes
Heat and mass transfer in float-zone processing are strongly influenced by convective flows in the zone. They are caused by buoyancy convection, thermocapillary (Marangoni) convection, or artificial sources such as rotation and radio-frequency heating. Flows in conducting melts can be controlled by the use of magnetic fields, either by damping fluid motion with static fields or by generating a defined flow with rotating fields. The possibilities of using static and rotating magnetic fields in silicon floating-zone growth have been investigated by experiments in axial static fields up to 5 T and in transverse rotating magnetic fields up to 7.5 mT. Static fields of a few 100 mT already suppress most striations but are detrimental to the radial segregation by introducing a coring effect. A complete suppression of dopant striations caused by time-dependent thermocapillary convection and a reduction of the coring to insignificant values, combined with a shift of the axial segregation profile toward a more diffusion-limited case, is possible with static fields greater than or equal to 1 T. However, under certain conditions the use of high axial magnetic fields can lead to the appearance of a new type of pronounced dopant striations, caused by thermoelectromagnetic convection. The use of a transverse rotating magnetic field influences the microscopic segregation at quite low inductions, of the order of a few millitesla. The field shifts time- dependent flows and the resulting striation patterns from a broad range of low frequencies at high amplitudes to a few high frequencies at low amplitudes.
This presentation will examine in detail the role of vibration-induced streaming flow in the context of float-zone crystal growth. It is very well known that during float-zone materials processing, the naturally occurring temperature gradients along the zone surface impose a thermocapillary flow in the zone. Under certain processing conditions, the thermocapillary flow can also become nonsteady (oscillatory). The presence of thermocapillary flow is detrimental to crystal quality, for it can promote non-uniform dopant distribution and crystal striations. To null this effect we have imposed a counter streaming flow in the zone, via end-wall vibration. This technique has been adapted to float-zone processing of Sodium Nitrate-Barium Nitrate eutectic alloys, under both steady and nonsteady thermocapillary flow conditions. The beneficial effects of counter streaming flow have been clearly brought out through the before and after comparisons of the crystal microstructure. In addition, we are also examining the theoretical underpinnings of the balancing of thermocapillary flows with vibration-driven counter flows in float-zones.
This presentation will examine in detail the role of vibration-induced streaming flow in the context of float-zone crystal growth. It is very well known that during float-zone materials processing, the naturally occurring temperature gradients along the zone surface impose a thermocapillary flow in the zone. Under certain processing conditions, the thermocapillary flow can also become nonsteady (oscillatory). The presence of thermocapillary flow is detrimental to crystal quality, for it can promote non-uniform dopant distribution and crystal striations. To null this effect we have imposed a counter streaming flow in the zone, via end-wall vibration. This technique has been adapted to float-zone processing of Sodium Nitrate-Barium Nitrate eutectic alloys, under both steady and nonsteady thermocapillary flow conditions. The beneficial effects of counter streaming flow have been clearly brought out through the before and after comparisons of the crystal microstructure. In addition, we are also examining the theoretical underpinnings of the balancing of thermocapillary flows with vibration-driven counter flows in float-zones.