WO2007141017A2 - Procédé de fabrication de silicium cristallin et d'hydrogène gazeux - Google Patents

Procédé de fabrication de silicium cristallin et d'hydrogène gazeux Download PDF

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Publication number
WO2007141017A2
WO2007141017A2 PCT/EP2007/005034 EP2007005034W WO2007141017A2 WO 2007141017 A2 WO2007141017 A2 WO 2007141017A2 EP 2007005034 W EP2007005034 W EP 2007005034W WO 2007141017 A2 WO2007141017 A2 WO 2007141017A2
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WIPO (PCT)
Prior art keywords
silicon
aluminum
hydrogen
fluorine
fluoride
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Ceased
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PCT/EP2007/005034
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German (de)
English (en)
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WO2007141017A8 (fr
Inventor
Peter Plichta
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/02—Production of hydrogen; Production of gaseous mixtures containing hydrogen
    • C01B3/22—Production of hydrogen; Production of gaseous mixtures containing hydrogen by decomposition of gaseous or liquid organic compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/984—Preparation from elemental silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/033—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by reduction of silicon halides or halosilanes with a metal or a metallic alloy as the only reducing agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/04—Hydrides of silicon
    • C01B33/043—Monosilane
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/20—Halides
    • C01F11/22—Fluorides
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/245—Fluorine; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step

Definitions

  • An object of the present invention is to name such possible raw materials and to describe their technical representation.
  • Oil-bearing sands / slates as starting materials are used for the preparation of large amounts of gaseous hydrogen and crystalline silicon, which can be used for the production of photosilicon or as a starting material for the preparation of silanes, silicon nitride and silicon carbide, oily sands here include mixtures of quartz sand with oils or tar products, which may also be caused by impurities.
  • A2) containing oil sands can be treated with the water formed during combustion very hot hydrogen fluoride (about 3,000 0 C), creating in the main silicon fluoride.
  • the resulting aluminum fluoride is known to be soluble neither in acids nor in alkalis and is combined with the AIF 3 produced in A1). After separation, it can be decomposed by electrolysis again in aluminum and fluorine.
  • A6 The heat released at the furnace during the thermal reaction of the main process can drive the turbine of a dynamo as strongly compressed water vapor.
  • the electric currents of the generators are bundled.
  • A7) The most important ceramics used in the art - silicon nitride (with its remarkable thermal conductivity) and silicon carbide (with its diamond-like hardness) - can be achieved at the same reaction start by different reaction conditions, as explained in A8) to A10).
  • the carbonaceous residue obtained in item A5) can be converted exothermically with the obtained crystalline silicon to silicon carbide.
  • the available crystalline silicon is surface-active and could be catalytically treated with hydrogen to produce monosilane.
  • Tv ⁇ onosTian can be taken from the TteaWion space and subjected to another catalytic pressure reaction at another location
  • Si + SiH 4 ⁇ (with cat as Pt oa) ⁇ Si (SiH 4 ) 4 + SiH n (SiH 4 ) m + Si n H m represent longer-chain silanes, both in the technology of the fuel cell, in ceramic-based engines, as can also be used with scramjet drives.
  • the invention is realized in a first basic idea that used in a process used oily sands and shale and their mixtures are used as starting materials for the preparation of crystalline silicon and hydrogen gas and for the production of silicon nitride, silicon carbide, monosilane and higher silanes by the Starting materials in stainless steel autoclave treated with the use of coming fluorine and hydrogen to the effect that the resulting very hot hydrogen fluoride rocks the silicate rocks in gaseous components such as silicon tetrafluoride and aluminum trifluoride to the very hot gaseous SiF 4 in the form of its salt potassium hexafluorosilicate with aluminum gries to release very to convert a lot of heat into crystalline silicon in the form of crystal lites, with the simultaneous accumulation of amorphous aluminum fluoride using is separated from a Abschwemmmethode and fine sieves and the thus obtained aluminum trifluoride is combined with the original already formed AIF 3 , and then converted back into metallic aluminum by fused-salt electrolysis -
  • crystalline silicon can take on a leading energy-efficient role in the future, because the silanes mentioned above provide atomic hydrogen at temperatures above 350 ° C, which has a half-life of half a second and thus forms the strongest reducing chemical agent, while the resulting silicon radicals are energetically compared with the oxidizing power of atomic oxygen, which can easily be observed in atmospheric thunderstorms.
  • the process is further developed that in schists a high calcium carbonate content provides calcium fluoride, which can be used in the production of fluorine.
  • the resulting CO 2 is not a hindrance to the further course of the reaction.
  • the flurosilane produced by the combustion is not obtained from expensive raw silicon - such as chlorosilanes in the silicone oil industry - but, as in the problem and in claim 1, from sand.
  • the primary energy to reiterate it, is provided by the hydrocarbon content of the oil sands and oil shale. In a summary consideration, the following becomes apparent in the first basic idea.
  • the crude oil stocks are calculable limited in time. Before the auto industry, aviation, the arms industry and space travel, for example, switch their combustion engines to silicon, which is known to burn atmospheric nitrogen in a hot chamber and deliver atomic hydrogen, a way must be found of coming down from the high oil prices.
  • the very large stocks of oily sands and slates provide the conditions for this.
  • the SiF 4 can now be converted with aluminum grit into crystalline silicon, again under the highest exothermic reaction aluminum fluoride is formed.
  • AIF 3 is broken down into aluminum and fluorine by electrolysis. Since in the aluminum fluoride representation be won, which makes the aluminum extraction process cheaper. Overall, this results in silicon in crystal sheets, which are either converted into photosilicon or in monosilane or in higher silanes.
  • the reaction process can also be controlled to switch to the production of silicon nitride or silicon carbide.
  • the hydrogen can be passed as a combustible gas, largely free of carbon monoxide, carbon dioxide and nitrogen in existing gas supply networks.
  • Another object of the present invention is to provide a cyclic process in which only a certain amount of fluorine and aluminum is used in addition to the oil sand.
  • the invention provides a process for the preparation, in particular in cyclic, large-scale, of crystalline silicon / photosilicon or the fuel silanes or ceramics silicon nitride or silicon carbide and gaseous hydrogen from oily sands and / or slates using aluminum and the mixture of fluorine and hydrogen, the 4,000 0 C hot hydrogen fluoride delivers when burning and are always used in a cycle again, so that only a subset of electric power must be fed.
  • Fig. 1 shows a series of large-scale production equipment that begins with the fact that oily sands / shale reach the mechanical decomposition plant I on mechanical transport routes.
  • Oil-bearing sands can be treated with the water formed during combustion very hot hydrogen fluoride (about 3,000 0 C), so that in the main silicon fluoride is produced (one, one). This is very much heat free. A necessary cooling process of the reactor chamber produces electricity using steam.
  • Crystalline silicon is currently being prepared by a complex process involving the use of coal, high electrical costs and fractionation of chlorosilanes followed by pyrolysis. The price is very high as it has been agreed worldwide. The new cyclic process would reduce the kilogram price for photosilicon to one hundredth.
  • the available crystalline silicon is surface-active and could be catalytically treated with hydrogen to produce monosilane.
  • This monosilane can be removed from the reaction space and converted into long-chain silanes in another patent application. These are to be used not only in the space travel, since they supply atomic hydrogen in the heat (Plichta).
  • the atomic hydrogen can also be used in a fuel cell.
  • the gaseous hydrogen (H 2 ) released by the heat can for the most part be converted into electricity by cooling with cold water via steam turbines and then fed into a gas network, while the remaining part of the hot hydrogen is burned with a certain amount of gaseous fluorine at a heat of about 4,000 ° C where the oil / pitch sands are pyrolyzed, so that the very hot hydrogen fluoride is immediately mixed with the silicon of the oily sands (see above). is converted into gaseous Siliziumtetrafiuohd and water vapor, wherein the hot SiF 4 , contaminated with HF, is passed directly into a combustion chamber, the aluminum grit is continuously supplied.
  • the aluminum is transformed into powdered aluminum fluoride, which is stable to aqueous bases and can be filtered off in order subsequently to be electrolytically reacted in the form of the anion [SiF 6 ] 2 ' , so that aluminum and fluorine are formed again.
  • the large stocks of oily sands and slates provide a basis for being able to produce cyclic crystalline silicon, photosilicon or the fuel silane, silicon nitride or silicon carbide.
  • the hydrocarbon of minerals By decomposing the hydrocarbon of minerals, supplying primary energy, into hydrogen and pure carbon / graphite, because hydrogen fluoride is used with the gases fluorine and hydrogen under the strongest exothermic reaction, the sands and siliceous schists can be converted to silicon fluoride and / or calcium fluoride.
  • the SiF 4 can be refined with aluminum grit into crystalline silicon, again producing aluminum fluoride under the highest exothermic reaction.
  • AIF 3 is now broken down again into aluminum and fluorine by electrolysis.
  • silicon is produced in crystal sheets, which are either converted into photosilicon or in monosilane.
  • the reaction process can also be controlled to switch to the production of silicon nitride or silicon carbide.
  • the hydrogen can be passed as a combustible gas, free of carbon monoxide, carbon dioxide and nitrogen in existing gas supply networks. In total, the primary energy of the hydrogen content of the oil pitch is determined using a -fee-süsa ⁇ nte ⁇ ! 44e!

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Geology (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne l'utilisation des ressources importantes en ardoise et sable contenant de l'huile pour la fabrication de silicium cristallin, de photosilicium ou de carburant silane, ou encore de nitrure de silicium ou de carbure de silicium. L'hydrocarbure des minéraux, fournissant une énergie primaire, étant réparti entre l'hydrogène et le graphite/carbone pur, et du fluorure d'hydrogène étant utilisé avec les gaz fluor et hydrogène par réaction fortement exothermique, le sable et l'ardoise contenant du silicium peuvent être transformés en fluorure de silicium et/ou en fluorure de calcium. Selon un nouveau procédé cyclique, le SiF<SUB>4</SUB> peut être purifié en silicium cristallin avec des grains d'aluminium, du fluorure d'aluminium étant obtenu par une réaction fortement exothermique. AlF<SUB>3</SUB> est maintenant réparti en aluminium et en fluor par électrolyse. La fabrication de fluorure d'aluminium, ainsi que la fluoration par HF et la pyrolyse nécessitant un refroidissement, il est possible d'économiser de l'électricité en utilisant de la vapeur d'eau surchauffée, ce qui rend le procédé d'obtention d'aluminium plus économique. Du silicium est également obtenu sous forme de plaquettes cristallines, qui peuvent soit être transformées en photosilicium, soit en monosilane.
PCT/EP2007/005034 2006-06-10 2007-06-06 Procédé de fabrication de silicium cristallin et d'hydrogène gazeux Ceased WO2007141017A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006029282A DE102006029282A1 (de) 2006-06-10 2006-06-10 Zyklische großtechnische Darstellung von kristallinem Silizium/Fotosilizium oder dem Treibstoff Silane.., einem Kreislauf immer erneut zum Einsatz kommen, so dass nur eine Teilmenge von elektrischem Strom eingespeist werden muss
DE102006029282.0 2006-06-10

Publications (2)

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WO2007141017A2 true WO2007141017A2 (fr) 2007-12-13
WO2007141017A8 WO2007141017A8 (fr) 2008-04-10

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PCT/EP2007/005034 Ceased WO2007141017A2 (fr) 2006-06-10 2007-06-06 Procédé de fabrication de silicium cristallin et d'hydrogène gazeux

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DE (1) DE102006029282A1 (fr)
WO (1) WO2007141017A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399618A (zh) * 2011-10-08 2012-04-04 江苏佳宇资源利用股份有限公司 一种从晶硅切割废砂浆中资源化回收碳化硅组份的方法
DE102013020962A1 (de) 2013-12-12 2015-06-18 Daimler Ag System und Verfahren zur Bereitstellung von elektrischer Energie in einem Kraftfahrzeug unter Verwendung einer AMTEC-Einrichtung

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5552284B2 (ja) * 2009-09-14 2014-07-16 信越化学工業株式会社 多結晶シリコン製造システム、多結晶シリコン製造装置および多結晶シリコンの製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399618A (zh) * 2011-10-08 2012-04-04 江苏佳宇资源利用股份有限公司 一种从晶硅切割废砂浆中资源化回收碳化硅组份的方法
DE102013020962A1 (de) 2013-12-12 2015-06-18 Daimler Ag System und Verfahren zur Bereitstellung von elektrischer Energie in einem Kraftfahrzeug unter Verwendung einer AMTEC-Einrichtung

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WO2007141017A8 (fr) 2008-04-10
DE102006029282A1 (de) 2007-12-13

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