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Platform under growth region stabilizes melt for more uniform crystal growth. In new crucible, platform just below growth interface so melt is too shallow to support convection. Critical depth for onset of pertinent instability calculated from heat flux through surface of melt, volume coefficient of thermal expansion, thermal conductivity, thermal diffusivity, and kinematic viscosity.
The purpose of this study is to investigate the question: Would eliminating the crucible eliminate the wall-induced nucleation of one of the liquid phases in an immiscible alloy and result in undercooling of the liquid into the metastable region thereby producing significant differences in the separation process and the microstructure upon solidification. Another primary objective of this research is to study systems with a metastable miscibility gap and to directly determine the metastable liquid miscibility gap by undercooling experiments. Nucleation and growth of droplets in these undercooled metallic liquid-liquid mixtures is also being studied. Results of this investigation indicate that containerless processing of immiscibles may not promote the undercooling of the single-phase liquid into the metastable region. Although no recalescence event was observed for this liquid-liquid transition, undercooling did occur across the miscibility gap for the solidification of the Ti phase that eventually separated.
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The modified CG2000 crystal grower construction, installation, and machine check-out was completed. The process development check-out proceeded with several dry runs and one growth run. Several machine calibrations and functional problems were discovered and corrected. Several exhaust gas analysis system alternatives were evaluated and an integrated system approved and ordered. A contract presentation was made at the Project Integration Meeting at JPL, including cost-projections using contract projected throughput and machine parameters. Several growth runs on a development CG200 RC grower show that complete neck, crown, and body automated growth can be achieved with only one operator input. Work continued for melt level, melt temperature, and diameter sensor development.
The process development continued, with a total of nine crystal growth runs. One of these was a 150 kg run of 5 crystals of approximately 30 kg each. Several machine and process problems were corrected and the 150 kg run was as successful as previous long runs on CG2000 RC's. The accelerated recharge and growth will be attempted when the development program resumes at full capacity in FY '82. The automation controls (Automatic Grower Light Computer System) were integrated to the seed dip temperature, shoulder, and diameter sensors on the CG2000 RC development grower. Test growths included four crystals, which were grown by the computer/sensor system from seed dip through tail off. This system will be integrated on the Mod CG2000 grower during the next quarter. The analytical task included the completion and preliminary testing of the gas chromatograph portion of the Furnace Atmosphere Analysis System. The system can detect CO concentrations and will be expanded to oxygen and water analysis in FY '82.
The modified CG2000 crystal grower construction, installation, and machine check out was completed. The process development check out proceeded with several dry runs and one growth run. Several machine calibrations and functional problems were discovered and corrected. Exhaust gas analysis system alternatives were evaluated and an integrated system approved and ordered. Several growth runs on a development CG2000 RC grower show that complete neck, crown, and body automated growth can be achieved with only one operator input.
The design and development of an advanced Czochralski crystal grower are described. Several exhaust gas analysis system equipment specifications studied are discussed. Process control requirements were defined and design work began on the melt temperature, melt level, and continuous diameter control. Sensor development included assembly and testing of a bench prototype of a diameter scanner system.
Six growth runs used the Kayex-Hameo Automatic Games Logic (AGILE) computer based system for growth from larger melts in the Mod CG2000. The implementation of the melt pyrometer sensor allowed for dip temperature monitoring and usage by the operator/AGILE system. Use of AGILE during recharge operations was successfully evaluated. The tendency of crystals to lose cylindrical shape (spiraling) continued to be a problem. The hygrometer was added to the Furnace Gas Analysis System and used on several growth runs. The gas chromatograph, including the integrator, was also used for more accurate carbon monoxide concentration measurements. Efforts continued for completing the automation of the total Gas Analysis System. An economic analysis, based on revised achievable straight growth rate, is presented.
Technique yields better mixing of impurities and superior qualiity crystals. Accellerated motion stirs melt which reduces temperature gradients and decreases boundary layer for diffusion of impurities near growing surface. Results better mixing of impurities into melt, decrease in tendency for dendritic growth or cellular growth and crystals with low dislocation density. Applied with success to solution growth and Czochralski growth, resulting in large crystals of superior quality.
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The number of pixels per unit area sampling an image determines Nyquist resolution. Therefore, the highest pixel density is the goal. Unfortunately, as reduction in pixel size approaches the wavelength of light, sensitivity is lost and noise increases. Animals face the same problems and have achieved novel solutions. Emulating these solutions offers potentially unlimited sensitivity with detector size approaching the diffraction limit. Once an image is 'captured', cellular preprocessing of information allows extraction of high resolution information from the scene. Computer simulation of this system promises hyperacuity for machine vision.
The wetting angles of several semiconductor-substrate combinations that are of practical importance for crystal growth have been measured: Ga-GaSb-Sb on fused quartz; Ge on fused quartz and carbon-based substrates, each with different roughness; Si on fused quartz plates and on plates coated with fused quartz, Si3N4, and BN powders. The Ga-GaSb-Sb system showed no significant dependence of the wetting angle on the composition despite a large composition dependence of the surface tension. For Ge, the effect of the roughness on the angle could initially be seen on both types of substrates, but for the fused quartz substrates an equilibrium value independent of the surface treatment was reached after several hours of contact time. For Si, total wetting was found for Si3N4 powders. A reduction of the angle over time was found for both fused quartz and BN powders, with the BN powder showing the highest angle at 150-120 deg.
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Report prepared for NDEP
A replenishment crucible is mounted adjacent the usual drawing crucible, from which a monocrystalline boule is drawn according to the Czochralski method. A siphon tube for molten semiconductor transfer extends from the replenishment crucible to the drawing crucible. Each crucible is enclosed within its own hermetic shell and is provided with its own heater. The siphon tube is initially filled with molten semiconductor by raising the inert atmospheric pressure in the shell surrounding the replenishment crucible above that surrounding the drawing crucible. Thereafter, adjustment of the level of molten semiconductor in the drawing crucible may be achieved by adjusting the level in either crucible, since the siphon tube will establish the same level in both crucibles. For continuous processing, solid semiconductor may be added to and melted in the replenishment crucible during the process of drawing crystals from the drawing crucible. A constant liquid level of melted semiconductor is maintained in the system by an optical monitoring device and any of several electromechanical controls of the rate of replenishment or crucible height.
The compatibilities of various monotectic alloy systems with several different crucible materials were evaluated. The study was carried out using small candidate alloy samples of compositions that produced fifty volume percent of each liquid phase at the monotectic temperature. Compatibility was based on the evaluation of the wetting tendency of the two immiscible phases with the crucible material in a one-g solidified sample. Three types of wetting phenomena were observed during the evaluation. Type 1 indicates an alloy-crucible combination where the L2 phase preferentially wets the crucible material. Since L2 is usually the minority phase in desirable alloys, this material combination would be difficult to process and is therefore considered incompatible. Type 2 behavior indicates an alloy-crucible combination where the L1 phase preferentially wets the crucible material. This type of combination is considered compatible since surface tension effects should aid in processing the alloy to a useful form. Type 3 indicates any combination that leads to major reactions between the alloy and crucible material, gas entrapment, or separation of the metal from the crucible wall. Additional compatibility evaluations would have to be carried out on combinations of this category. The five alloy systems studied included aluminum-bismuth, copper-lead, aluminum-indium, aluminum-lead and cadmium-gallium. The systems were combined with crucibles of alumina, boron nitride, mullite, quartz, silicon carbide and zirconia.
It is known that the predictive life of the refractory ceramic liner of nuclear waste glass melters is conservative, as demonstrated by performance of these materials such as in the Defense Waste Processing Facility (DWPF). The motivation for this task is to maximize the useful life of the melters that will be operated at the Waste Treatment and Immobilization Plant (WTP), which will in turn minimize procurement and disposal costs and melter outage times, as well as to identify maximum loadings in the waste glass of those species that corrode melter components. This task was initiated jointly with Pacific Northwest National Laboratory (PNNL) with the objective to develop a methodology and model to enable more accurate prediction of refractory service life under prototypic conditions from laboratory-scale material corrosion tests. Refractory corrosion is generally reported as physical material loss, measured in units of distance (e.g., inch) or as physical material loss rate, measured in units of distance per time (e.g., inch/day). In post-operational melters, the refractory corrosion is measured directly, sometimes reported as corrosion depth. Crucible tests are used in the laboratory to accelerate the refractory corrosion to facilitate a meaningful measurement in a commensurate amount of time. Crucible tests are particularly useful in understanding refractory corrosion across a large glass composition space, where operational testing would be prohibitive. Some of the critical parameters that are known to influence refractory corrosion by molten glass in a crucible test are temperature, system redox, molten salt phases, glass chemistry, and test duration. The majority of data collected for Monofrax® K-3 (hereafter referred to as K-3) corrosion is from crucible tests, but a small amount comes directly from scaled and production melters. Crucible test data has been collected under varying conditions, whereas data collected from operational melters is relatively fewer and represents conditions specific to the melter campaign. The result is that the published data can be grouped and analyzed in multiple ways, not all of which are readily comparable. The Standard Test Method for Isothermal Corrosion Resistance of Refractories to Molten Glass (ASTM C621) outlines the general guidelines used across industry. That method describes a sealed, static test in which the surface area of the refractory coupon and the volume of glass are fixed. A significant portion of the crucible data pertaining to nuclear waste glasses has been collected in a modified configuration; the most notable differences being the surface area of the refractory coupon to volume of the glass and use of a method for bubbling the melt. To our knowledge, the influence of those parameters on the refractory corrosion has not been quantified. In this work, it was determined that static tests and bubbled tests would be performed. Savannah River National Laboratory (SRNL) was tasked with setting up and performing static testing while PNNL was tasked with setting up and performing bubbled testing. Initial activities were performed to establish laboratory methods that reproduce data comparable to existing data sets of K-3 refractory corrosion by low activity waste (LAW) and high-level waste (HLW) glass compositions. Later activities were focused on refining the test parameters to establish a standard test practice to be used between Laboratories and collecting additional data to be used in the enhanced waste glass model development. This document serves primarily to convey the refractory loss measurement results from corrosion testing of K-3 refractory with waste glass compositions developed for use in the WTP melters. The data will be used in the enhanced property/composition models being developed for waste glass vitrification and melter operations.