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Liquid Oxygen of Argon

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Liquid Oxygen of Argon USOO6780390B2 (12) United States Patent (10) Patent No.: US 6,780,390 B2 Bhagat et al. (45) Date of Patent: Aug. 24, 2004 (54) METHOD OF PRODUCING HIGH PURITY OTHER PUBLICATIONS GERMANIUM TETRAFLUORIDE Dennis et al., “Germanium. XXI Germanium Tetrafluoride', (75) Inventors: Sudhir Solomon Bhagat, Tulsa, OK Z. Phys. Chem. 130 (1927), pp. 520–531.* (US); Dayal T. Meshri, Tulsa, OK Adams, et al. “The Preparation and Some Properties of New (US); Sanjay D. Meshri, Tulsa, OK Germanium Flouride”. J. Inorg. Nucl. Chem., 1971, vol. 33, (US); Michale Shane Petty, Claremore, pp. 1301-1306, no month. OK (US) Burg, Anton B. “Germanium Tetrafluoride”, Fluorine Chem istry, Edited by Dr. J.H. Simons. Academic Press Inc., (73) Assignee: Advance Research Chemicals, Inc., Publishers, New York, NY. 1950. vol. 1, pp. 110-111, Catoosa, OK (US) 118-119, no month. Hiroyuki et al. “Production of Germanium Tetrafluoride (*) Notice: Subject to any disclaimer, the term of this Having High Purity”. PAJ 00–23–76, 01051329 JP, NDN patent is extended or adjusted under 35 190-0003-9421-0, no month. U.S.C. 154(b) by 173 days. Isao et al. "Production of Germanium Tetrafluoride'. PAJ 08-01-94, 06234523 JP, NDN- 190-0171-8558-1. (21) Appl. No.: 10/218,894 * cited by examiner (22) Filed: Aug. 14, 2002 Primary Examiner Ngoc-Yen Nguyen Prior Publication Data (74) Attorney, Agent, or Firm-Fellers, Snider, (65) Blankenship, Bailey & Tippens, P.C. US 2004/0076577 A1 Apr. 22, 2004 (57) ABSTRACT (51) Int. Cl." ............................ C01G 17/04; CO1B 9/08 (52) U.S. Cl. .................. ... 423/489; 423/494; 423/659 A method of producing high purity germanium tetrafluoride (58) Field of Search ................................. 423/489, 494, comprising the Step of flowing a mixture of inert gas and 423/659 fluorine gas through a reactor chamber preferably containing germanium powder. The reactor effluent Stream is conducted (56) References Cited through at least one product trap effective for condensing and retaining at least a portion of the germanium tetrafluo U.S. PATENT DOCUMENTS ride product. The product is preferably then purified by 4,960,581 A : 10/1990 Harada et al. .............. 423/489 repeatedly Subliming the product as necessary to remove 5,899,733 A : 5/1999 Gisdakis et al. ............ 438/528 Volatile impurities. 5,918,106 A : 6/1999 Bulko et al. ................ 423/260 2001/00494.57 A1 : 12/2001 Stephens .................... 570/123 23 Claims, 1 Drawing Sheet /ed N Heater Coil 4. Heater Coil Liquid Oxygen of Argon 2 (a vrrestressuassets U.S. Patent Aug. 24, 2004 US 6,780,390 B2 2/-~~~~ # 9 |No. U|||||||||||U US 6,780,390 B2 1 2 METHOD OF PRODUCING HIGH PURITY remove Volatile impurities. The Volatile impurities are pref GERMANIUM TETRAFLUORIDE erably removed by Subliming the germanium tetrafluoride in a product container through one or more “freeze/thaw' BACKGROUND OF THE INVENTION cycles and then evacuating the head gas from the product 5 container to remove vaporized impurities therefrom. The The present invention relates to methods of producing Steps of Subliming and evacuating are preferably repeated germanium tetrafluoride. More particularly, but not by way until essentially all of the Volatile impurities are removed. limitation, the present invention relates to methods for In yet another aspect, the inventive method preferably producing ultra high purity germanium tetrafluoride Suitable further includes the Step of removing nonvolatile impurities for use in, for example, Semiconductor applications. from the germanium tetrafluoride product by (a) Sublimating Several processes are known in the art for producing the germanium tetrafluoride, in a container, to a vapor State technical grade germanium tetrafluoride. One method and (b) transferring the Sublimated germanium tetrafluoride involves the fluorination of germanium with undiluted fluo out of the container Such that the nonvolatile impurities are rine or nitrogen trifluoride gas wherein the germanium is Separated from the germanium tetrafluoride vapor. placed in a batch reaction chamber and the chamber is filled 15 with the undiluted gas. The batch reactor is then allowed to Further objects, features, and advantages of the present Set at a pressure of about 3 atmospheres and a temperature invention will be apparent to those skilled in the art upon of from 250-500 C. Another production method involves examining the accompanying drawing and upon reading the the decomposition of barium fluorogermanate in a quartz following detailed description of the preferred embodi tube at 750-1000 C. Another method involves the decom mentS. position of hexafluorogermanic acid at 400-600 C. Another BRIEF DESCRIPTION OF THE DRAWING method utilizes halogen exchange between GeCl and SbF to yield a mixture comprising germanium tetrafluoride, The drawing Schematically illustrates a reactor and recov GeFCI, GeFC1 and GeFCls. Still another method involves ery System 2 preferred for use in the inventive method. the reaction of Sulfuric acid with a mixture of germanium 25 DETAILED DESCRIPTION OF THE oxide and one or more metal fluorides. Yet another method involves the reaction of germanium with uranium tetrafluo PREFERRED EMBODIMENTS ride. An embodiment 2 of a reactor and recovery System Unfortunately, each of these prior techniqueS produces a particularly well Suited for use in connection with the Substantial amount of Volatile and/or nonvolatile impurities present invention is depicted in the drawing. The reactor and that are difficult and costly to Separate from the desired recovery System 2 preferably comprises: a tubular reactor 4, reaction product. Examples of Such impurities include: a tray 6 which is removably positionable in reactor 4 for Silicon tetrafluoride, Sulfur hexafluoride, carbon holding a quantity of finely divided elemental germanium 8; tetrafluoride, NO, potassium fluorochlorides, hydrogen an electrical heating coil, a Steam jacket, or other heating fluoride, germanium difluoride, transition metal fluorides, 35 System 10 for warming reactor 4, a gas feed conduit 12 and elemental fluorine. which preferably extends into reactor 4 through the inlet Thus, a need presently exists for a leSS complex and more flange 14 thereof; at least one initial product trap 16 for cost effective method for producing high purity germanium receiving the reaction product gas from reactor 4 and for tetrafluoride. Such method will also preferably provide a condensing and retaining at least a portion of the germanium high product yield. A need particularly exists for a much leSS 40 tetrafluoride product; a cooling device Such as a coolant complicated and more cost effective approach for producing dewar 18 which is removably positionable over at least a ultra high purity germanium tetrafluoride Suitable for use in portion of the exterior of product trap 16, a reaction product photovoltaic cells, in nanocrystals, as an ion implantation conduit 20 extending from reactor 4 to product trap 16; and dopant, or in other Semiconductor applications. an effluent gas conduit 22 extending from product trap 16. 45 During the reaction and recovery process, as described SUMMARY OF THE INVENTION hereinbelow, the initial product trap 16 is preferably main The present invention provides a method of producing tained at a temperature effective for condensing at least a high purity germanium tetrafluoride which Satisfies the portion of the germanium tetrafluoride contained in the needs and alleviates the problems discussed above. The reaction product gas Stream Such that a Solid germanium inventive method comprises the Step of flowing a gas 50 tetrafluoride product is formed and retained in product trap mixture comprising fluorine gas and an inert gas through a 16. In a particularly preferred embodiment, the reactor and reactor having germanium therein. The fluorine gas con recovery System 2 will include one or more product traps 16 tained in the gas mixture reacts with the germanium to which are cooled using dry ice in coolant dewar(s) 18 Such produce germanium tetrafluoride which is included in the that the product trap(s) 16 is/are maintained at about -78°C. reactor product gas Stream. The inventive method preferably 55 In addition to product trap(S) 16, the reactor and recovery also includes the Step, prior to flowing the gas mixture System 2 preferably also includes a final product trap 24 through the reactor, of purifying the fluorine gas by cryo which receives effluent gas from trap(s) 16 via conduit 22. genically chilling to a temperature of less than -150° C. and Final trap 24 is maintained at a temperature effective for contacting the chilled fluorine gas with Sodium fluoride. condensing additional germanium tetrafluoride product from The inventive method also preferably comprises the Step 60 the reaction product Stream. Final product trap 24 will of conducting the reactor product Stream through at least one preferably be cooled using liquid oxygen or liquid argon. In product trap maintained at a temperature effective for con a particularly preferred embodiment, the final product trap densing at least a portion of the germanium tetrafluoride 24 is cooled using liquid oxygen in an exterior coolant from the reactor product Stream. The condensed germanium container 26 Such that the final trap 24 is maintained at a tetrafluoride is preferably retained in the product trap. 65 temperature of about -182.9° C. An effluent conduit 28 In addition, the inventive method preferably includes the extending from final trap 24 delivers inert gas used in the Step of purifying the condensed germanium tetrafluoride to inventive proceSS and other noncondensed material to a US 6,780,390 B2 3 4 Scrubber and a vacuum pump (not shown) or other device other hand, is preferably warmed to a temperature in the capable of evacuating reactor and recovery System 2. range of from about 125 C. to about 200 C. using the As will be understood by those skilled in the art, fluorine reactor heating System 10. Also, inert gas flow through the gas is highly reactive with many metal materials, particu System is resumed.
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