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A structured device placed in an aerated crucible to pack ceramics molding substance that is to be processed was designed. The structure is wrapped by sealing material made of pyrex glass and graphite foil or sheet with a weight attached on top of it. The crucible is made of carbon; the ceramics material to be treated through heat intervenient press process is molding substance consisting mainly of silicon nitride.
Metals, ceramics, and glasses just some of possible raw materials. Key components of equipment for new microballoon fabrication process nozzle, crucible assembly, and drop tube. Recessed, conical inner orifice aids in producing uniform, symmetrical microballoons. All-graphite crucible assembly resistant to misalinement and cracks. Drop tube ensures timely solidification of microballoons used in fluidized-bed heat exchangers; as containers for hazardous materials; catalysts in chemical and pharmaceutical processes; solid fuel for rockets; fuel containers for fusion power experiments; shock-wave dampers; and starting materials for high-strength, low-density sintered alloys and ceramics.
The optimum conditions for crystal growth are usually achieved either by suppressing convective fluid flows (e.g., by the use of a low-gravity environment) or by over-riding thermal and solutal convection by the use of a strong stirring action. A novel stirring technique has been developed which involves subjecting a vertical crucible to a circle in a horizontal plane (without rotation). Use of an amplitude of 3 mm at a frequency of approx 6 Hz produced complete mixing of a non-uniform aqueous liquid in a few seconds. The mixing action involved the downward flow of liquid in the outer annulus of the liquid, driven by surface waves. When the downward flowing liquid reaches the bottom of the crucible, it is reflected in a central, upward flowing spiral. This flow pattern should be beneficial for crystal growth by the Bridgman method since it will sweep impurities away from the walls and produce a more convex solid-liquid interface. Initial attempts to apply the new stirring technique to CdTe crystal growth did not show significant improvement in the number of crystals nucleated, but the interface shape appeared to be close to that predicted.
A mixture containing glass 70 to 95 and BN or B4C powder (0.1-10 microns) 5 to 30 vol. % is used as a secondary pressure medium in hot isostatic pressing of ceramics. Thus, Pyrex beads were mixed with 15% vol. BN powder (average diameter 2 microns), fused at 1400 deg for 2 h, cooled, crushed, and put into a graphite crucible. A Si3N4 sintered body was embedded in the powder, heated in vacuum at 1200 deg for 2 h, treated in a hot isostatic press furnace at 1700 deg and 1000 atm. for 1 h, and cooled to give a Si3N4 ceramic. It was easily separated from the crucible.
In the hot isostatic pressing of ceramic materials in molten glass using an inert gas as a pressing medium, glass adhered to the sintered ceramics is heated to convert it to a porous glass and removed. Thus, Si3N4 powder was compacted at 5000 kg/sq cm, coated with a 0.5 mm thick BN, embedded in Pyrex glass in a graphite crucible, put inside a hot isostatic press containing Argon, hot pressed at 1750 C and 100 kg/sq cm; cooled, taken out from the crucible, heated at 1100 C for 30 minutes, cooled, and then glass adhered to the sintered body was removed.
The present invention is directed to an apparatus for stirring materials using planar orthogonal axes oscillations. The apparatus has a movable slide plate sandwiched between two fixed parallel support plates. Pressurized air is supplied to the movable slide plate which employs a tri-arm air bearing vent structure which allows the slide plate to float and to translate between the parallel support plates. The container having a material to be stirred is secured to the upper surface of the slide plate through an aperture in the upper support plate. A motor driven eccentric shaft loosely extends into a center hole bearing of the slide plate to cause the horizontal oscillations. Novelty lies in the combination of elements which exploits the discovery that low frequency, orthogonal oscillations applied horizontally to a Bridgman crucible provides a very rigorous stirring action, comparable with and more effective by an order of magnitude than the accelerated crucible rotation technique.
The Crucible Melt Extraction Process was demonstrated to convert scraps of aluminum alloy 2219, used in the Space Shuttle External Tank, into fibers. The cast fibers were then consolidated by cold welding. The X-ray diffraction test of the cast fibers was done to examine the crystallinity and oxide content of the fibers. The compressive stress-strain behavior of the consolidated materials was also examined. Two conceptual schemes which would adapt the as-developed Crucible Melt Extraction Process to the microgravity condition in space were finally proposed.
If a binary homogeneous melt is cooled into an immiscible region, the newly formed second phase will generally have a density different from the parent phase, and will separate readily by sedimentation. Observation of solidification processes in microgravity indicates that outside of sedimentation, at least two other important effets can separate the phases: (1) preferential wetting, and (2) thermal migration of second-phase droplets due to interfacial tension gradients. The latter effect would drive the minority phase along the thermal gradient toward the hottest part (assuming the interfacial tension decreases with increasing temperature), which is usually away from the crucible wall. On the other hand, if the minority phase preferentially wets the crucible, a minority phase layer which thickens as initial solution compositions approach critical, will form adjacent to the solid surface and remain in the coldest region of the ingot. This study presents compelling preliminary evidence that these two effects do exist and that they compete with one another. However, the temperature dependence of preferential wetting below T(c) for the current system of study is, as yet, undetermined. These effects are sensitive to the initial concentration of a hypermonotectic solution cooling through a miscibility gap.
A simple model for the crystal growth by the Czochralski (CZ) process has been proposed based on semiquantitative arguments. The model provides empirical relationships for the dependence of the pulling rate and the interface shape on the important process variables such as crystal radius, crucible temperature, height of the melt level, and the height of the exposed portion of the crucible wall. The parameters of the model can be evaluated by matching the results obtained from a detailed mathematical model of the CZ process or from extensive experimental data. The model has, therefore, the potential application for determining the best process conditions and for on-line control and optimization of the crystal puller to grow crystals with constant diameter and nearly planar interface.
Semiempirical mathematical model proposed for control of growth of single crystals of silicon by Czochralski process. Expresses dependence of pulling rate and shape of liquid/solid interface upon important process variables; radius of growing crystal, temperature of crucible, level of melt, and height of exposed portion of crucible wall. Necessary to control shape of interface in manner consistent with other variables, to maintain radially uniform concentration of dopant, and reduce thermally induced stresses in vicinity of interface. Used to simulate complete growth cycles without requiring excessive computer time consumed by rigorous finite-element modeling.
The production of H(-) ions by heating LiH powder in a high-temperature crucible was investigated experimentally and theoretically. It is found that the efficiency of H(-) ion production by this method is high. However, the theory for the negative surface ionization indicates that such high efficiency is not possible at crucible temperatures of about 750 C. The need for a further study of LiH ionization is emphasized.
Electrolytic extraction of O2 from molten lunar soil is conceptually simple and thus a candidate process for producing O2 on the Moon. Possible container and electrode materials are being tested for durability in corrosive high-temperature silicate melts and looking for complications that might increase energy requirements. Gaseous oxygen is being produced by electrolysis of 1-2 gram quantities of silicate melts in spinel (MgAl2O4) crucibles; in these melts, spinel is a stable phase. The concentration of FeO was kept low because FeO decrease O2 production efficiency. Platinum electrodes were placed about 0.5 cm apart in the melt. The spinel crucible was still intact after 40 minutes of electrolysis, when the experiment was halted for examination. The Pt anode was also intact; its Pt was maintained in a dynamci state in which the anode was continuously oxidized but quickly reduced again by the silicate melt, inhibiting migration of Pt away from the anode. In melts with low concentrations of Al2O3 + SiO2 (2 wt percent), the energy of resistance heating was only approximately equal to 10 to 20 percent of the theoretical amount required to produce O2. In melts substantially more concentrated in Al2O3 + SiO2, higher melt viscosity resulted in frothing that, in the worst case, caused high enough melt resistivities to raise the energy requirements to nearly 10 times theoretical. Both Fe and Si are produced at the cathode; in iron-rich melts, a- and c-iron and molten ferrosilicon were observed. Production was also observed at the cathode of a previously unrecognized gas; which is not yet identified. The solubility of metallic species was measured in silicate melts. They are too low to reduce significantly the efficiency of O2 production.
DTA and both isothermal and nonisothermal DSC techniques are presently used to investigate the crystallization kinetics of a 40 (mol) percent Li2O-60 percent SiO2 glass as a function of glass powder particle size, the use of either alumina or Pt as the crucible material, the use of N, O, or Ar atmospheres, and surface pretreatments of the glass powder with deionized water, HCl, or HF. Neither the furnace atmosphere nor the crucible material had a significant effect on activation energy, frequency factor, or Avrami exponent. Washings of the glass with the three different fluids decreased the crystallization temperature by 25 to 30 C.
Research at the Army Materials Technology Laboratory (AMTL) and elsewhere has shown that many glass properties including elastic modulus, hardness, and corrosion resistance are improved markedly by the substitution of nitrogen for oxygen in the glass structure. Oxynitride glasses, therefore, offer exciting opportunities for making high modulus, high strength fibers. Processes for making oxynitride glasses and fibers of glass compositions similar to commercial oxide glasses, but with considerable enhanced properties, are discussed. We have made glasses with elastic moduli as high as 140 GPa and fibers with moduli of 120 GPa and tensile strengths up to 2900 MPa. AMTL holds a U.S. patent on oxynitride glass fibers, and this presentation discusses a unique process for drawing small diameter oxynitride glass fibers at high drawing rates. Fibers are drawn through a nozzle from molten glass in a molybdenum crucible at 1550 C. The crucible is situated in a furnace chamber in flowing nitrogen, and the fiber is wound in air outside of the chamber, making the process straightforward and commercially feasible. Strengths were considerably improved by improving glass quality to minimize internal defects. Though the fiber strengths were comparable with oxide fibers, work is currently in progress to further improve the elastic modulus and strength of fibers. The high elastic modulus of oxynitride glasses indicate their potential for making fibers with tensile strengths surpassing any oxide glass fibers, and we hope to realize that potential in the near future.
Macrosegregation produced during vertical Bridgeman directional solidification of Csl-1 wt. pct. Tll in crucibles of varying diameter, from 0.5 to 2.0 cm, was examined. Gravity driven convection is present in the melt even in the smallest crucible diameter of 0.5 cm. Observed solutal profiles are in agreement with the analytical boundary layer model of Favier which describes macrosegregation in the presence of convection. The scintillation efficiency of Csl decreases along the specimen length as the thallium iodide content of the alloy increases.
The Fiber Pulling Apparatus (FPA) is a device designed to produce continuous glass fibers from simulated lunar soil, and to determine the effects of reduced gravity, specifically 1/6 g on fiber formation and resultant properties. Briefly, pre-melt simulated lunar soil will be placed in a pint crucible and heated to 1200 C or higher, up to a maximum temperature of 1400 C. At a given temperature, a quartz fiber will be immersed into the melt and then pulled through a chill block and wound onto a cylindrical bobbin using a servo motor control. A high resolution video camera will record the fiber as it is being pulled. This assembly wil be enclosed in Plexiglas. Before fiber pulling commences, the apparatus will be backfilled with dry nitrogen. A separate data acquisition system will support this apparatus. This system will contain a personal computer, video recorder, and monitor. Temperature, acceleration, winding speed, and video images will be controlled and recorded using the data acquisition system. Thus, the FPA will consist of two hardware packages, the fiber production assembly and the data acquisition rack. The primary objective of this test is to determine the effects of 1/6 g on the formation of continuous glass fiber made from simulated lunar soil. Baseline studies using the FPA on the ground will provide a reference for the 1/6 g studies. Of particular interest will be the effect of 1/6 g on the free fluid zone where the fiber exits the crucible. In the fiber spinning parlance this zone is known as the upper jet region, where the boundary slope is greater than one tenth. The properties of the resulting glass fiber will depend on the jet shape as well as distributions of velocity, temperature and tension within the jet. It is unknown at this time how 1/6 g will effect these parameters.
Research carried out over the past two decades in which attempts have been made to produce desirable microstructures in immiscible alloys is reviewed. Factors affecting the formation of desirable microstructures in immiscible alloys are addressed and some of the techniques that have been successful in controlling these factors in order to produce useful structures are discussed. Some of the intended applications of these alloys require a dispersion of one phase in the other, while other applications favor the use of aligned, fibrous microstructures with continuity of both phases. The microstructures obtained in immiscible alloys are often strongly influenced by processing conditions. Perhaps the most well known effect is gravity induced sedimentation of the denser immiscible phase during solidification. This difficulty with sedimentation led to low gravity processing in attempts to produce dispersed microstructures. However, experimentation under low gravity conditions soon revealed that many other factors, including wetting of the crucible walls and surface tension driven flows, often resulted in complete separation and coalescence of the two immiscible phases. The production of aligned fibrous microstructures in hypermonotectic alloys appears to be even more difficult than the formation of a dispersion. Here, in addition to sedimentation and crucible wetting, convective and interfacial instabilities must be considered as well. Calculation of the limits of stability during directional solidification were carried out but require experimental verification.
The results of the diffusion experiment for solar He and Ne in IDP's in a magnetic separate from Pacific Ocean sediment suggest that solar He and Ne would be easily released from IDP grains and hence lost from subducting slabs at shallow depths. However, since the diffusion experiments was conducted under high vacuum, there may be a possibility that magnetite grains, which are supposedly the main constituent of the magnetic fraction, might be partly reduced to form a metal phase due to low oxygen fugacity in the experimental condition. If this is the case, such a phase change might affect the gas release and hence the results of the diffusion coefficients. In order to examine whether or not such a phase change really occurred in the condition of the diffusion experiment, I conducted a heating experiment for a magnetic separate from Pacific Ocean sediment. In the same condition as in the diffusion experiment, and the run products were examined with an x ray diffraction method. Three samples were prepared: they were wrapped with platinum foil, put in a vacuum line, and heated in a molybdenum crucible for two hours at 500 C, 800 C,and 950 C, respectively. After cooling the furnace, the samples were taken out from the crucible and analyzed with an x ray diffraction method.