Aec-Nasa Tech Brief
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March 1969 Brief 69-10079 sty C AEC-NASA TECH BRIEF YES AEC-NASA Tech Briefs describe innovations resulting from the research and development program of the U.S. AEC or from AEC-NASA interagency efforts. They are issued to encourage commercial application. Tech Briefs are published by NASA and may be purchased, at 15 cents each, from the Clearinghouse for Federal Scientific and Technical Information, Springfield, Virginia 22151. Preparation of Thorium by Magnesium—Zinc Reduction Stirring Motor Ball Valve Stuffing Box Assembly Sampling Port - Water Annulus Graphitar Bearing 1___._Hea t Shields SST Shaft Ta Thermowell Graphite Secondary Crucible Heated Ta Shaft Graphite Pouring Mold Baffled Crucible^v I SST Shell Ta Paddle THORIUM DIOXIDE REDUCTION APPARATUS A technique for the preparation of thorium metal success of the process. by magnesium—zinc reduction of thorium dioxide has The present method for commercial production of been investigated on a laboratory scale. The extent thorium metal involves metallothermic reduction of of reduction was determined as a function of time, thorium tetrafluoride with calcium in the presence of amount and composition of flux, temperature, agita- zinc chloride. However, calcium is expensive as a re- tion, particle size of the oxide, and magnesium con- ductant and the process requires a prior hydro-fluo- centration in the alloy. It was found that the use of rination step. Using magnesium—zinc alloy for the a flux of the proper composition is essential to the reduction of thorium dioxide has potential economic (continued overleaf) This document was prepared under the sponsorship of the Atomic liability resulting from the use of the information contained in this Energy Commission and/or the National Aeronautics and Space document, or warrants that the use of any information, apparatus, Administration. Neither the United States Government nor any per- method, or process disclosed in this document may not infringe pri- son acting on behalf of the United States Government assumes any vately owned rights. advantages; relatively inexpensive reagents are used Notes: for the metal and flux phases, and metal of acceptable I. Procedures and results have been published in quality can be produced in good yield. "Preparation of Metals by Magnesium-Zinc Reduc- For the experiments, the molten salt fluxes were pre- tion--Part II. Reduction of Thorium Dioxide," ANI.- pared from anhydrous, reagent-grade salts, except 7058, June 1965, by A. V. Hariharan, J. B. Knigh- for magnesium chloride, which was obtained as a by- ton, and R. K. Steunenberg of Argonne National product from a process used for the production of zir- Laboratory. This report is available from the Clear- conium. The thorium dioxide was a high-fired mate- inghouse for Federal Scientific and Technical In- rial that had been screened to —325 mesh. The zinc formation, Springfield, Va. 22151; price: $3.00 and magnesium were 99.99 and 99.95 % pure, re- (microfiche copies, $0.65), Reference: 69-10079. spectively. Preliminary reductions were performed in Additional information is also contained in Patent the open air. No. 3,164,462 (January 5, 1965) "Preparation of Although complete reductions were achieved in air Thorium Metal from the Oxide," which is avail- atmosphere, the rate and extent of reduction were able from the U. S. Patent Office at $0.50 each. improved by the use of an argon atmosphere. The ap- 2. Thorium metal is used in electronics industries paratus shown in the figure was used for the argon for its thermionic emission, low work function, and atmosphere experiments. It consisted primarily of a action as a "getter." Since this information may help resistance-heated, tilt-pour, stainless-steel furnace. to improve production processes of thorium, it The reductions were conducted in a tantalum crucible, should be of interest to persons in the electronic equipped with four baffles to enhance mixing, and lo- industries. cated inside a graphite secondary container. By tilting 3. Inquiries concerning this innovation may be dir- the entire furnace, the molten contents of the crucible ected to: could be poured into the mold. The furnace was also Office of Industrial Cooperation equipped with a thermocouple wall, a sampling port, Argonne National Laboratory and provisions for applying vacuum or an argon atmos- 9700 South Cass Avenue phere. Argonne, Illinois 60439 Under optimum conditions, over 99% reduction of Reference: B69-10079 thorium dioxide was obtained in less than 4 hours, Source: A. V. Hariharan, J. B. Knighton with product purities up to 99.7 %. These optimum and R. K. Steunenberg conditions were: 800°C, argon atmosphere, a mag- (ARG- 10245) nesium conc. of 5 to 10 w/o in the zinc phase, a flux Patent status: containing a large proportion of magnesium chloride Inquiries about obtaining rights for commercial use and 10 m/o calcium or magnesium fluoride, and a of this innovation may be made to: thorium dioxide; flux weight ratio of about 0.22 %. Mr. George H .Lee, Chief In addition, four small-scale demonstration experi- Chicago Patent Group ments were performed, in which thorium dioxide was U. S. Atomic Energy Commission reduced by zinc—magnesium alloy. The resulting liquid- Chicago Operations Office metal solution was distilled to produce a thorium metal 9800 South Cass Avenue sponge, which was consolidated by arc-melting. Argonne, Illinois 60439 Brief 69-10079 Category 03.