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At least 19 records

Directional solidification of silicon in carbon crucibles by an oscillating crucible technique

The quality of silicon cast by present techniques is limited by the presence of dislocations and grain boundaries in unseeded growth and by cellular structures with dislocation networks in the case of the seeded growth. To address these concerns, a new method of directional solidification called the oscillating crucible technique (OCT) is developed. During growth, a carbon crucible is oscillated to provide for effective stirring of the melt. This growth technique (seeded growth only), along with material characterization and solar-cell fabrication and testing, is described. Solar-cell efficiencies of up to 13 percent at 100 mW/sq cm area obtained in the single crystalline areas. Minority-carrier diffusion lengths exceeding 100 microns are measured even in the polycrystalline areas of the wafers. Limitations of the present setup and possible future improvements are discussed.

Daud, T.

Covering a Crucible with Metal Containing Channels

In a procedure that partly resembles the lost-wax casting process, a crucible made of a brittle material (ceramic, quartz, or glass) is covered with a layer of metal containing channels. The metal cover and the channels can serve any or all of several purposes, depending upon the application: Typically, the metal would serve at least partly to reinforce the crucible. The channels could be used as passages for narrow objects that could include thermocouples and heat-transfer strips. Alternatively or in addition, channels could be used as flow paths for liquid or gaseous coolants and could be positioned and oriented for position- or direction-selective cooling. In some cases, the channels could be filled with known gases and sealed so that failure of the crucibles could be indicated by instruments that detect the gases. The process consists of three main steps. In the first step, a pattern defining the channels is formed by wrapping or depositing a material in the desired channel pattern on the outer surface of the crucible. The pattern material can be a plastic, wax, low-ash fibrous material, a soluble material, or other suitable material that can subsequently be removed easily. In a proof-of-concept demonstration (see figure), the crucible was an alumina cylinder and the mold material was plastic tie-down tape. In the second step, the patterned crucible is coated with metal. In one variation of the second step, a very thin layer containing or consisting of an electrically conductive material (e.g., gold, silver, or carbon) is painted or otherwise deposited on the mold-covered crucible, then the covering metal required for the specific application is electrodeposited on the very thin conducting layer. In another variation of the second step, the metal coat is formed by chemical vapor deposition. In the proof-of-concept demonstration, a layer of nickel 0.003 in. ( 0.08 mm) thick was electrodeposited. In the third step, the patterned material is removed. This is generally done by heating the crucible assembly until the patterned material melts and runs out, vaporizes, and/or decomposes to an ash, leaving the channels. Alternatively, if the patterned material is soluble, it can be removed by use of a suitable solvent. In the proof-of-concept demonstration, the tape was burned away by heating the assembly to a temperature of 600 C.

Grugel, Richard N.

Mutiple Czochralski growth of silicon crystals from a single crucible

An apparatus for the Czochralski growth of silicon crystals is presented which is capable of producing multiple ingots from a single crucible. The growth chamber features a refillable crucible with a water-cooled, vacuum-tight isolation valve located between the pull chamber and the growth furnace tank which allows the melt crucible to always be at vacuum or low argon pressure when retrieving crystal or introducing recharge polysilicon feed stock. The grower can thus be recharged to obtain 100 kg of silicon crystal ingots from one crucible, and may accommodate crucibles up to 35 cm in diameter. Evaluation of the impurity contents and I-V characteristics of solar cells fabricated from seven ingots grown from two crucibles reveals a small but consistent decrease in cell efficiency from 10.4% to 9.6% from the first to the fourth ingot made in a single run, which is explained by impurity build-up in the residual melt. The crystal grower thus may offer economic benefits through the extension of crucible lifetime and the reduction of furnace downtime.

Lane, R. L.

Compatibility of molten plutonium with wrought and additively manufactured metal crucibles

Understanding plutonium’s interaction with metals is crucial for optimizing pyrochemical operations, nuclear fuel containment, and various actinide processing techniques. Traditionally, tantalum crucibles are employed for plutonium processing due to their high durability, excellent temperature stability, and low solubility in plutonium. However, tantalum faces challenges such as plutonium wetting and diffusion, making surface coatings particularly important for crucibles in pyrochemical applications to enhance corrosion resistance against plutonium. Tantalum is also expensive and difficult to machine, prompting the need for advanced manufacturing techniques to address these challenges. Here, in this work, we investigate the interaction of Pu with tantalum and titanium crucibles fabricated using both traditional machining methods and laser powder bed fusion (LPBF) additive manufacturing (AM). LPBF-AM is an advanced technique that allows for the creation of complex geometries from traditionally difficult-to-machine metals by using a high-powered laser to build parts. Previous studies of conventional manufactured tantalum have utilized oxidation and carburization of the surface to mitigate plutonium wetting; however, no studies of surface modified LPBF-AM material have been undertaken. These studies are crucial, given the typical differences in the grain structure between conventional and LPBF-AM materials. All crucibles underwent differential scanning calorimetry to confirm the melting of plutonium. Subsequently, the crucibles were sectioned and mounted in epoxy for microstructural analysis using optical microscopy and scanning electron microscopy. This investigation, comparing the performance of wrought vs AM metal crucibles, provides a basis for future tooling applications in actinide processing techniques and can address the challenges associated with traditional machining, particularly in pyrochemical applications.

Actinides

Method of Fabricating Protective Coating for a Crucible with the Coating Having Channels Formed Therein

A method is provided for the fabrication of a protective coating for a crucible with channels being formed in the coating. A material is adhered to the outer wall of the crucible to form a pattern thereon. The outer wall of the crucible along with the pattern of material adhered thereto is next coated with another material. The material used to form the pattern should extend through the outer material coating to define at least one port therein. Next, the crucible with its pattern of material and outer coating material is heated to a temperature of transformation at which the pattern of material is transformed to a fluidic state while the crucible and outer coating material maintain their solid integrity. Such transformation could also be accomplished by using a solvent that causes the pattern of material to dissolve. Finally, the material in its fluidic state is removed via the at least one port formed in the outer material coating thereby leaving channels defined in the coating adjacent the outer wall of the crucible.

Richard N Grugel

Rotatable crucible for rapid solidification process

This invention relates to an apparatus for producing filament, fiber, ribbon or film from a molten material, comprising a preferably heat extracting crucible which contains a pool of molten material at a selected horizontal level in the pool. The crucible has an opening extending from above the free surface level to a bottom edge of the opening, the bottom edge being sufficiently below the free surface level so that the molten material cannot form and hold a meniscus by surface tension between the edge and the level of the free surface and further comprises a heat extracting substrate laterally disposed with respect to the crucible and which rotates about an axis of rotation. The substrate is positioned adjacent the edge of the opening which confines the molten material and prevents it from overflowing downwardly out of the crucible. The invention features rotating means which includes a first drive means for tiltably rotating the crucible about an axis of rotation which is coaxial with the axis of rotation of the substrate, so the crucible edge can be maintained a predetermined constant distance from the substrate. The distance chosen is suitable for depositing molten material on the substrate and the apparatus also has a second drive means which is drivingly connected to the substrate for continuously moving the surface of the substrate upwardly past the edge and a melt front formed at the interface of the molten material and the substrate surface.

Gaspar, Thomas

Quench Crucibles Reinforced with Metal

Improved crucibles consisting mainly of metal-reinforced ceramic ampules have been developed for use in experiments in which material specimens are heated in the crucibles to various high temperatures, then quenched by, for example, plunging the crucibles into water at room temperature. In a traditional quench crucible, the gap between the ampule and the metal cartridge impedes the transfer of heat to such a degree that the quench rate (the rate of cooling of the specimen) can be too low to produce the desired effect in the specimen. One can increase the quench rate by eliminating the metal cartridge to enable direct quenching of the ampule, but then the thermal shock of direct quenching causes cracking of the ampule. In a quench crucible of the present improved type, there is no gap and no metal cartridge in the traditional sense. Instead, there is an overlay of metal in direct contact with the ampule, as shown on the right side of the figure. Because there is no gap between the metal overlay and the ampule, the heat-transfer rate can be much greater than it is in a traditional quench crucible. The metal overlay also reinforces the ampule against cracking.

Holmes, Richard R.

Effects of crucible wetting during solidification of immiscible Pb-Zn

Many industrial uses for liquid phase miscibility gap alloys are proposed. However, the commercial production of these alloys into useful ingots with a reasonable amount of homogeneity is arduous because of their immiscibility in the liquid state. In the low-g environment of space gravitational settling forces are abated, thus solidification of an immiscible alloys with a uniform distribution of phases becomes feasible. Elimination of gravitational settling and coalescence processes in low-g also makes possible the study of other separation and coarsening mechanisms. Even with gravitational separation forces reduced, many low-g experiments have resulted in severely segregated structures. The segregation in many cases was due to preferential wetting of the crucible by one of the immiscible liquids. The objective was to analyze the wetting behavior of Pb-Zn alloys on various crucible materials in an effort to identify a crucible in which the fluid flow induced by preferential wetting is minimized. It is proposed that by choosing the crucible for a particular alloy so that the difference in surface energy between the solid and two liqud phases is minimized, the effects of preferential wetting can be diminished and possibly avoided. Qualitative experiments were conducted and have shown the competitive wetting behavior of the immiscible Pb-Zn system and 13 different crucible materials.

Degroh, Henry C., III

Effects of crucible wetting during solidification of immiscible Pb-Zn alloys

Many industrial uses for liquid phase miscibility gap alloys are proposed. However, the commercial production of these alloys into useful ingots with a reasonable amount of homogeneity is arduous because of their immiscibility in the liquid state. In the low-g environment of space gravitational settling forces are abated, thus solidification of an immiscible alloy with a uniform distribution of phases becomes feasible. Elimination of gravitational settling and coalescence processes in low-g also makes possible the study of other separation and coarsening mechanisms. Even with gravitational separation forces reduced, many low-g experiments have resulted in severely segregated structures. The segregation in many cases was due to preferential wetting of the crucible by one of the immiscible liquids. The objective was to analyze the wetting behavior of Pb-Zn alloys on various crucible materials in an effort to identify a crucible in which the fluid flow induced by preferential wetting is minimized. It is proposed that by choosing the crucible for a particular alloy so that the difference in surface energy between the solid and two liquid phases is minimized, the effects of preferential wetting can be diminished and possibly avoided. Qualitative experiments were conducted and have shown the competitive wetting behavior of the immiscible Pb-Zn system and 13 different crucible materials.

De Groh, H. C., III

Influence of Crucible Materials on High-temperature Properties of Vacuum-melted Nickel-chromium-cobalt Alloy

A study of the effect of induction-vacuum-melting procedure on the high-temperature properties of a titanium-and-aluminum-hardened nickel-base alloy revealed that a major variable was the type of ceramic used as a crucible. Reactions between the melt and magnesia or zirconia crucibles apparently increased high-temperature properties by introducing small amounts of boron or zirconium into the melts. Heats melted in alumina crucibles had relatively low rupture life and ductility at 1,600 F and cracked during hot-working as a result of deriving no boron or zirconium from the crucible.

MATERIALS, PROPERTIES - STRESS-RUPTURE

Recharging the Silicon Crucible in a Hot Furnace

"Melt recharger" adds raw silicon to crucible in crystal-growing furnace without disturbing inert-gas atmosphere or significantly lowering temperature of melt. Crucible-refill hopper is lowered into hot zone of crystal-pulling chamber through an isolation valve. Cable that supports hopper is fastened to cone-shaped stopper in bottom of hopper. Stopper moves out of opening in hopper, allowing part of polysilicon charge to drop into crucible.

Lane, R. L.

Barrier for Continuous-Crystal-Growth Crucible

Properly designed openings permit free flow of melt while restraining pellets. Redesigned partition between growth region and melt-replenishment region of crystal-growth crucible makes it less likely crucible will run out of feed material in middle of cycle. Supply of molten silicon is maintained by addition of silicon pellets to compartment at one end of heated crucible, and partition or barrier is required to hold pellets while allowing melted silicon to flow from compartment.

Skutch, M. E.

Cold crucible Czochralski for solar cells

The efficiency and radiation resistance of present silicon solar cells are a function of the oxygen and carbon impurities and the boron doping used to provide the proper resistivity material. The standard Czochralski process used grow single crystal silicon contaminates the silicon stock material due to the use of a quartz crucible and graphite components. The use of a process which replaces these elements with a water cooled copper to crucible has provided a major step in providing gallium doped (100) crystal orientation, low oxygen, low carbon, silicon. A discussion of the Cold Crucible Czochralski process and recent float Zone developments is provided.

Trumble, T. M.

Two-Crucible Czochralski Process

Scheme for continuous melt replenishment increases capacity of Czochralski crystal-growing furnace. Replenishing and drawing crucibles of improved Czochralski apparatus connected by heated quartz siphon. When doped silicon added to replenishing crucible, liquid silicon flows into drawing crucible, equalizing two melt levels. Addition of new material automatically controlled in response to optically sensed melt level. Results of this semicontinuous operation higher production speed, lower cost, and good control of crystal quality.

Fiegl, G.

PbO reduction and crucible reactions of 70 wt pct PbO-30 wt pct B2O3 glass

NASA has conducted an investigation of PbO-B2O3 glass with a view to PbO reduction and subsequent crucible reactions as a function of temperature and oxygen partial pressure, in order to establish the optimum processing conditions for subcentimetric glass hollow spheres applicable to inertial confinement fusion targets. The results obtained support the selection of appropriate crucible materials and oxygen partial pressure-temperature combinations that avoid phase separation from PbO reduction and/or crucible reactions.

Schilling, Christopher H.

Crystal growth of YBa2Cu3O(7-x) and reaction of gold crucible with Ba-Cu-rich flux

YBa2Cu3O(7-x) crystals are grown in a gold crucible by a self-flux method. The flux moves along the gold surface due to surface wetting and leaves Y123 crystals behind. The obtained crystals are clean and have a size up to two millimeters and a Tc is greater than 90 K. In an effort to recycle the used crucibles, it is found that the used gold is contaminated by copper. A CuO thin film is easily formed on the surface of the crucible that is made of the used gold. This film provides good surface wetting and a buffer layer, which reduces the reaction between gold and the Y-Ba-Cu-oxide melt.

Tao, Y. K.

Directional Solidification and Convection in Small Diameter Crucibles

Pb-2.2 wt% Sb alloy was directionally solidified in 1, 2, 3 and 7 mm diameter crucibles. Pb-Sb alloy presents a solutally unstable case. Under plane-front conditions, the resulting macrosegregation along the solidified length indicates that convection persists even in the 1 mm diameter crucible. Al-2 wt% Cu alloy was directionally solidified because this alloy was expected to be stable with respect to convection. Nevertheless, the resulting macrosegregation pattern and the microstructure in solidified examples indicated the presence of convection. Simulations performed for both alloys show that convection persists for crucibles as small as 0.6 mm of diameter. For the solutally stable alloy, Al-2 wt% Cu, the simulations indicate that the convection arises from a lateral temperature gradient.

Chen, J.

Effect of Crucible Diameter Reduction on the Convection, Macrosegregation, and Dendritic Morphology during Directional Solidification of Pb-2.2 Wt Pct Sb Alloy

The Pb-2.2 wt pct Sb alloy has been directionally solidified in 1-, 2-, 3-, and 7-mm-diameter crucibles with planar and dendritic liquid-solid interface orphology. For plane front solidification, the experimentally observed macrosegregation along the solidified length follows the relationship proposed by Favier. Application of a 0.4 T transverse magnetic field has no effect on the extent of convection. Reducing the ampoule diameter appears to decrease the extent of convection. However, extensive convection is still present even in the 1-mm-diameter crucible. An extrapolation of the observed behavior indicated that nearly diffusive transport conditions require ampoules that are about 40 microns in diameter. Reduction of the crucible diameter does not appear to have any significant effect on the primary dendrite spacing. However, it results in considerable distortion of the dendrite morphology and ordering. This is especially true for the 1-mm diameter samples.

Chen, Jun