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US 2012/0082610 A1 Channon (43) Pub US 20120082610A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2012/0082610 A1 Channon (43) Pub. Date: Apr. 5, 2012 (54) FLUORSPAR/IODIDE PROCESS FOR (52) U.S. Cl. ......................................... 423/342; 423/349 REDUCTION.PURIFICATION, AND (57) ABSTRACT CRYSTALLIZATION OF SILICON Method and apparatus for producing molten purified crystal line silicon from low-grade siliceous fluorspar ore, Sulfur (76) Inventor: Matthew J. Channon, trioxide gas, and a metallic iodide salt. Method involves: (1) Albuquerque, NM (US) initially reacting silicon dioxide-bearing fluorspar ore and Sulfur trioxide gas in Sulfuric acid to create silicon tetrafluo ride gas and fluorogypsum; (2) reacting the product gas with (21) Appl. No.: 12/924,667 a heated iodide salt to form a fluoride salt and silicon tetraio dide; (3) isolating silicon tetraiodide from impurities and purifying it by washing steps and distillation in a series of (22) Filed: Oct. 2, 2010 distillation columns; (4) heating the silicon tetraiodide to its decomposition temperature in a silicon crystal casting machine, producing pure molten silicon metal ready for crys Publication Classification tallization; and pure iodine gas, extracted as liquid in a cold wall chamber. The system is batch process-based, with con (51) Int. Cl. tinuous elements. The system operates largely at atmospheric COIB33/023 (2006.01) pressure, requiring limited inert gas purges during batch COIB33/08 (2006.01) changes. Patent Application Publication Apr. 5, 2012 Sheet 1 of 5 US 2012/008261.0 A1 Do a 2 OO 5 Patent Application Publication Apr. 5, 2012 Sheet 2 of 5 US 2012/008261.0 A1 Patent Application Publication Apr. 5, 2012 Sheet 3 of 5 US 2012/008261.0 A1 s Patent Application Publication Apr. 5, 2012 Sheet 4 of 5 US 2012/008261.0 A1 (ºouoo)OSÁH (I?leuIOI?)ºO!”,S (6)*OS · JOdeA)·( )~~~~);(s )!!!!"OsºH(6 (s)VOSeO Patent Application Publication Apr. 5, 2012 Sheet 5 of 5 US 2012/008261.0 A1 o m i o - US 2012/008261.0 A1 Apr. 5, 2012 FLUORSPAR/ODIDE PROCESS FOR No. 1,665.588) first patented this process. Most fluorspar REDUCTION.PURIFICATIOIN, AND deposits contain significant fractions of silicon dioxide CRYSTALLIZATION OF SILICON (known as gangue), and ore processing is required in order to reduce the percentage of silicon dioxide in the final product. FIELD OF THE INVENTION If silicon dioxide is retained in the fluorspar, the reaction with sulfuric acid produces the typically undesirable intermediate 0001. The present invention pertains generally to produc product fluosilicic acid. ing silicon feedstock for the aluminum, chemical, and semi 0007 If fluosilicic acid, which only occurs in aqueous conductor industries. The present invention pertains specifi form, is dried, silicon tetrafluoride gas is evolved. Molstad cally to reaction of crude fluorspar, Sulfuric gases, and iodide (U.S. Pat. No. 2,833,628) produced a method to dry fluosilicic salts to produce pure silicon feedstock for use in fabricating acid with concentrated sulfuric acid. Silicon tetrafluoride gas photovoltaic and other semiconductor devices, and producing provides an alternate set of paths to achieve a reduced silicon impure silicon metal, gypsum, fluoride salts, and pure iodine. metal product without the need for carbon. Because of this synergistic relationship between fluorides and silicon diox BACKGROUND OF THE INVENTION ide, impure fluorspar poses a Superior alternative to quartzite 0002. Over three-quarters of the photovoltaic modules sand as a naturally occurring source of silicon. sold annually are made from silicon. Manufacturers have 0008 Metallurgical-grade silicon is a poor choice as a repeatedly expressed concern about the future Supply of low starting material for further refinement, since its metallic cost silicon feedstock as this market continues to grow at a nature requires high processing temperatures and/or at least rate exceeding 30% each year. As photovoltaics continue to two chemical reactions (one to a gaseous form and one back grow in popularity, the amount of silicon consumed by pho to metal) in order for cost-effective purification to take place. tovoltaics has exceeded the amount consumed by other semi This is routinely achieved in existing processes by reacting conductor applications, and if current trends continue, will the metallurgical grade silicon with acid to form gaseous become the leading use of silicon, exceeding the Supply capa chlorosilanes and then reducing the chlorosilanes back to bilities not only of the silicon purification industry, but those silicon metal. By starting with a material form that is easy to of the far larger silicon metal reduction industry. purify, and making the conversion to reduced silicon metal 0003. Although photovoltaic modules themselves pro only once, one can achieve significant time, plant, and energy duce no pollution, the current state of the art process to make savings. silicon for photovoltaic modules, carbothermic reduction, 0009 Silicon tetraiodide is an easily-purified form of sili utilizes coke or other cheap carbon Sources to remove the con, melting at 120 C and boiling at 287 C Silicon tetraiodide oxygen from quartzite sand, requiring energy-intensive pro also decomposes into silicon and iodine at elevated tempera cess temperatures up to 2000 C and producing significant tures, without the need for other reactants, making it an excel quantities of greenhouse gases, primarily carbon monoxide. lent source material in situations where the purity of the end 0004. The current state of the art process of pure silicon product is paramount. crystal manufacture is complex and convoluted, involving 0010 Silicon tetrafluoride is easily converted to silicon raw material extraction at one site, carbothermic reduction at tetraiodide through a double-replacement reaction with an another, purification at another, crystallization at another, and iodide Salt, though this is a novel method for making silicon PV cell and module fabrication at yet another. During every tetraiodide. Moates (U.S. Pat. No. 3,006,737) was the first step except extraction, the silicon is heated to very high pro patent to mention using silicon tetraiodide as a means of cessing temperatures, and the heat is wasted in order to trans purification of silicon, but never mentioned a specific starting port the material to the next site, where it must be heated material. Herrick (U.S. Pat. No. 3,020,129) used metallurgi again. During later steps, additional measures must be taken cal-grade silicon as a source material for silicon tetraiodide, to avoid contamination or damage during transport. even though this requires the extra steps of creating metallur 0005. Although multiple avenues exist for the purification gical grade silicon, and converting metallurgical-grade sili of silicon, none have been commercially marketed that do not con into a gas. Wang (U.S. Pat. Nos. 6,468,886 and 6,712, begin with metallurgical-grade silicon or carbothermic 908) and Fallavolita (CA-2,661,036) likewise used reduction in one form or another. Although quartzite sand is metallurgical-grade or other impure silicon metal as a starting the preferred mineral source of silicon dioxide for existing point to manufacture silicon tetraiodide. processes, since it contains the fewest impurities, nearly 0011. At the end of state of the art silicon purification every mineral deposit on Earth contains significant quantities processes, whether they rely on chlorosilanes or silicon tet of impure silicon dioxide. raiodide, amorphous solid silicon is produced, typically in the 0006 Silicon in a useful form can not be derived from any form of chunks. These amorphous silicon chunks must be natural Source without removing the oxygen atoms it is remelted in order to crystallize them and form them into a bonded to. Although this is conventionally accomplished by shape Suitable for manufacture of semiconductor devices. the introduction of carbon and heat and removal of the oxide Sylvania (GB-787,043), Moates, Ling (U.S. Pat. No. 3,012, through a gas phase, as described by Kuhlmann (U.S. Pat. No. 861), Herrick, Lord (U.S. Pat. No. 5,810,934), Wang, and 3.215.522), other chemical processes can achieve removal of Fallavolita never addressed the possibility of combining the the oxygen atoms, most notably reaction with acidic fluo tetraiodide thermal decomposition process with further heat rides. Acidic fluorides, most notably hydrofluoric acid, have ing in order to achieve a pure liquid silicon product Suitable been in use for decades to remove oxide layers from silicon for crystallization and eliminate the need for amorphous wafers in the manufacture of semiconductor devices. Hydrof chunks. luoric acid is conventionally produced from a reaction 0012. Whereupon the silicon has reached its melting between Sulfuric acid and calcium fluoride ore, also known as point, it must be cooled in a slow and tightly-controlled fash fluorspar. Meyerhofer (GB-222,836) and Harshaw (U.S. Pat. ion to make crystalline silicon. Competing processes to US 2012/008261.0 A1 Apr. 5, 2012 achieve this include heat-exchanger-method (HEM) bulk 0018. Another object of the present invention is to provide crystallization, Czochralski (CZ)-based crystal pulling, float a high tonnage process for producing lower grade silicon Zone (FZ)-based crystal pulling, edge-defined film growth metal and gypsum from silicon-bearing fluorspar ore. (EFG), and string ribbon growth. Each crystal growth tech 0019. Another object of the present invention is to provide nology requires a charge of pure molten silicon, and typically a method for producing silicon metal without consuming includes an energy-intensive melting and vacuum purge stage carbon fuels or producing carbon-bearing waste gases. to bring the cool silicon chunk source material up to tempera 0020. Additional objects, advantages and novel features of ture in a contamination-controlled fashion. the invention shall be set forth in part in the description that follows, and in part will become apparent to those skilled in the art upon examination of the following or may be learned SUMMARY OF THE INVENTION by the practice of the invention.
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