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WO2009141062A2 - Production and use of fine-particle silicon - Google Patents

Production and use of fine-particle silicon Download PDF

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Publication number
WO2009141062A2
WO2009141062A2 PCT/EP2009/003260 EP2009003260W WO2009141062A2 WO 2009141062 A2 WO2009141062 A2 WO 2009141062A2 EP 2009003260 W EP2009003260 W EP 2009003260W WO 2009141062 A2 WO2009141062 A2 WO 2009141062A2
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WO
WIPO (PCT)
Prior art keywords
particles
microns
starting material
silicon
range
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Ceased
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PCT/EP2009/003260
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German (de)
French (fr)
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WO2009141062A3 (en
Inventor
Armin Müller
Peter Woditsch
Christian Kusterer
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Sunicon AG
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Sunicon AG
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Publication date
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Publication of WO2009141062A2 publication Critical patent/WO2009141062A2/en
Publication of WO2009141062A3 publication Critical patent/WO2009141062A3/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
    • C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
    • C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
    • C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from 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
    • C01B33/04—Hydrides of silicon

Definitions

  • the invention relates to a process for the preparation of silanes.
  • the invention furthermore relates to the use of the silanes produced according to the method for the production of ultrapure silicon for photovoltaic purposes.
  • high-purity silicon is done for the most part by purification of silanes and their subsequent decomposition into high-purity silicon.
  • High purity silicon is needed as a raw material in both the electronics and photovoltaic industries.
  • the increasing global demand for high-purity silicon has led to a significant increase in prices.
  • the invention is therefore based on the object to provide a process for the preparation of silanes, which is particularly economical.
  • metallurgical silicon is comminuted by means of shock waves such that the diameter of the comminuted particles lies in a range of 0.1 .mu.m to 1 cm.
  • the particle size distribution of the particles has a maximum in the range of 3 ⁇ m to 8 ⁇ m, especially at about 5 microns.
  • the comminution is carried out in a gas atmosphere having a residual oxygen content of at most 1%, in particular at most 1%, in particular at most 0.25%.
  • the Wassert. Water vapor content of the gas atmosphere is at most 1% o, in particular at most 0.5% o, in particular at most 0.25% o.
  • An inert gas atmosphere is provided as the gas atmosphere, nitrogen (N 2 ), argon (Ar), hydrogen (H 2 ) or mixtures of these gases being provided as inert gases.
  • the device provided for generating the shock waves can be installed in an externally sealed housing, which allows the provision and maintenance of a controlled atmosphere.
  • the crushed silicon particles are stored in an intermediate bunker with a controlled atmosphere.
  • the water and / or oxygen content of the atmosphere in the intermediate bunker is reduced by at least 90%, in particular at least 99%, in particular at least 99.9%, preferably at least 99.99%, from the ambient atmospheric value.
  • the intermediate bunker in particular has an inert gas atmosphere. Inert gas is again nitrogen (N 2 ), argon (Ar), hydrogen (H 2 ) or mixtures of these gases.
  • the silicon particles are placed in a fluidized bed reactor where they are reacted with hydrogen chloride gas (HCl gas) to form a silane and / or silane derivative, in particular trichlorosilane (SiHCl 3 ).
  • HCl gas hydrogen chloride gas
  • the silane derivative may have a residual group of the group of halogen, alkyl, aryl, alkoxy or amine compounds.
  • the particle size distribution of the comminuted particles has a maximum in the range of 100 microns to 500 microns, in particular at about 250 microns.
  • dried copper chloride is added as catalyst before and / or during comminution. Both components are intimately mixed with each other during comminution.
  • the third embodiment substantially corresponds to the first embodiment, the description of which is hereby incorporated by reference.
  • the main difference from the first embodiment is that as starting material silicon alloys are used which contain catalytically active transition metals.
  • the starting material is in particular ferrosilicon.
  • the raw material is present before its comminution as granules with a granule size of up to a few centimeters in diameter.
  • the second embodiment during - A -
  • crushed copper chloride may be added as a catalyst.
  • silanes and / or silane derivatives prepared by one of the above processes are used for the production of ultrapure silicon for photovoltaic purposes. It is also possible to use the silanes prepared in this way for the preparation of linear and / or branched polysiloxanes.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention relates to a method for producing silanes in which a starting material comprising silicon is comminuted by means of shock waves.

Description

Herstellung und Verwendung von feinteiligem Silizium Production and use of finely divided silicon

Die Erfindung betrifft ein Verfahren zur Herstellung von Silanen. Die Erfindung betrifft weiterhin die Verwendung der verfahrensgemäß hergestell- ten Silane zur Herstellung von Reinstsilizium für photovoltaische Zwecke.The invention relates to a process for the preparation of silanes. The invention furthermore relates to the use of the silanes produced according to the method for the production of ultrapure silicon for photovoltaic purposes.

Die Herstellung von hochreinem Silizium geschieht zum überwiegenden Teil durch Reinigung von Silanen und deren anschließende Zersetzung in hochreines Silizium. Hochreines Silizium wird sowohl in der Elektronik- als auch in der Photovoltaikindustrie als Rohstoff benötigt. Der weltweit steigende Bedarf an hochreinem Silizium hat zu einer deutlichen Preissteigerung geführt.The production of high-purity silicon is done for the most part by purification of silanes and their subsequent decomposition into high-purity silicon. High purity silicon is needed as a raw material in both the electronics and photovoltaic industries. The increasing global demand for high-purity silicon has led to a significant increase in prices.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren zur Her- Stellung von Silanen zu schaffen, welches besonders wirtschaftlich ist.The invention is therefore based on the object to provide a process for the preparation of silanes, which is particularly economical.

Diese Aufgabe wird durch die Merkmale der Ansprüche 1 und 11 gelöst. Der Kern der Erfindung besteht darin, zur Zerkleinerung eines Silizium aufweisenden Ausgangsstoffes gepulste Stoßwellen einzusetzen. Weitere vorteilhafte Ausführungsformen ergeben sich aus den Unteransprüchen.This object is solved by the features of claims 1 and 11. The essence of the invention consists in using pulsed shock waves for comminuting a silicon-containing starting material. Further advantageous embodiments will become apparent from the dependent claims.

Details und Merkmale der Erfindung ergeben sich aus der Beschreibung mehrerer Ausführungsbeispiele.Details and features of the invention will become apparent from the description of several embodiments.

Gemäß einem ersten Ausführungsbeispiel wird metallurgisches Silizium mittels Stoßwellen so zerkleinert, dass der Durchmesser der zerkleinerten Partikel in einem Bereich von 0, 1 μm bis 1 cm liegt. Die Korngrößenverteilung der Partikel weist ein Maximum im Bereich von 3 μm bis 8 μm, insbesondere bei etwa 5 μm auf. Die Zerkleinerung wird in einer Gasatmosphäre mit einem Restsauerstoffgehalt von höchstens 1%, insbesondere höchstens 1 %o, insbesondere höchstens 0,25 %o durchgeführt. Der Wasserbzw. Wasserdampfgehalt der Gasatmosphäre beträgt höchstens 1 %o, insbe- sondere höchstens 0,5 %o, insbesondere höchstens 0,25 %o. Als Gasatmosphäre ist eine Inertgas-Atmosphäre vorgesehen, wobei als Inertgase Stickstoff (N2), Argon (Ar), Wasserstoff (H2) oder Mischungen dieser Gase vorgesehen sind. Hierzu kann die zur Erzeugung der Stoßwellen vorgesehene Einrichtung in einem nach außen abgeschlossenen Gehäuse, welches die Bereitstellung und Aufrechterhaltung einer kontrollierten Atmosphäre erlaubt, eingebaut sein.According to a first exemplary embodiment, metallurgical silicon is comminuted by means of shock waves such that the diameter of the comminuted particles lies in a range of 0.1 .mu.m to 1 cm. The particle size distribution of the particles has a maximum in the range of 3 μm to 8 μm, especially at about 5 microns. The comminution is carried out in a gas atmosphere having a residual oxygen content of at most 1%, in particular at most 1%, in particular at most 0.25%. The Wasserbzw. Water vapor content of the gas atmosphere is at most 1% o, in particular at most 0.5% o, in particular at most 0.25% o. An inert gas atmosphere is provided as the gas atmosphere, nitrogen (N 2 ), argon (Ar), hydrogen (H 2 ) or mixtures of these gases being provided as inert gases. For this purpose, the device provided for generating the shock waves can be installed in an externally sealed housing, which allows the provision and maintenance of a controlled atmosphere.

Für eine Apparatur zur Erzeugung der Stoßwellen wird auf die DE 10259456 B4 verwiesen.For an apparatus for generating the shock waves, reference is made to DE 10259456 B4.

Die zerkleinerten Silizium-Partikel werden in einem Zwischenbunker mit einer kontrollierten Atmosphäre aufbewahrt. Der Wasser- und/oder Sauerstoffgehalt der Atmosphäre im Zwischenbunker ist um mindestens 90 %, insbesondere mindestens 99 %, insbesondere mindestens 99,9 %, vorzugs- weise mindestens 99,99 % gegenüber dem Umgebungsatmosphärenwert reduziert. Der Zwischenbunker weist insbesondere eine Inertgas-Atmosphäre auf. Als Inertgas dienen wiederum Stickstoff (N2), Argon (Ar), Wasserstoff (H2) oder Mischungen dieser Gase.The crushed silicon particles are stored in an intermediate bunker with a controlled atmosphere. The water and / or oxygen content of the atmosphere in the intermediate bunker is reduced by at least 90%, in particular at least 99%, in particular at least 99.9%, preferably at least 99.99%, from the ambient atmospheric value. The intermediate bunker in particular has an inert gas atmosphere. Inert gas is again nitrogen (N 2 ), argon (Ar), hydrogen (H 2 ) or mixtures of these gases.

Vom Zwischenbunker werden die Silizium-Partikel in einen Fliesbettreaktor gegeben und dort mit Chlorwasserstoff-Gas (HCl-Gas) zu einem Silan und/oder Silan-Derviat, insbesondere zu Trichlorsilan (SiHCl3), umgesetzt. Allgemein kann das Silan-Derivat eine Restgruppe der Gruppe der Halogen-, Alkyl-, Aryl-, Alkoxy- oder Amin- Verbindungen aufweisen.From the intermediate bunker, the silicon particles are placed in a fluidized bed reactor where they are reacted with hydrogen chloride gas (HCl gas) to form a silane and / or silane derivative, in particular trichlorosilane (SiHCl 3 ). In general, the silane derivative may have a residual group of the group of halogen, alkyl, aryl, alkoxy or amine compounds.

Zur Umsetzung der Partikel zu einer S ilan- Verbindung in einem Reaktor ist ein dem Fachmann vertrautes Verfahren vorgesehen. Stellvertretend für ein derartiges Verfahren seien die Beispiele Ia bis 4 der DE 100 61 680 Al genannt, auf die hiermit verwiesen wird.To convert the particles into a silane compound in a reactor, a process familiar to the skilled worker is provided. Representative of such a process are examples Ia to 4 of DE 100 61 680 A1, to which reference is hereby made.

Im Folgenden wird ein weiteres Beispiel für ein Verfahren zur Herstellung von Silanen und/oder deren Derivate beschrieben. Das Verfahren entspricht im Wesentlichen dem ersten Ausführungsbeispiel, auf dessen Beschreibung hiermit verwiesen wird. Der zentrale Unterschied zum ersten Beispiel besteht darin, dass die Korngrößenverteilung der zerkleinerten Partikel ein Maximum im Bereich von 100 μm bis 500 μm, insbesondere bei etwa 250 μm hat. Außerdem wird vor und/oder während des Zerkleinerns getrocknetes Kupferchlorid als Katalysator zugegeben. Beide Komponenten werden bei der Zerkleinerung innig miteinander vermischt.In the following, another example of a process for producing silanes and / or their derivatives will be described. The method substantially corresponds to the first embodiment, to the description of which reference is hereby made. The central difference to the first example is that the particle size distribution of the comminuted particles has a maximum in the range of 100 microns to 500 microns, in particular at about 250 microns. In addition, dried copper chloride is added as catalyst before and / or during comminution. Both components are intimately mixed with each other during comminution.

Im Folgenden wird ein drittes Ausführungsbeispiel des Verfahrens be- schrieben. Das dritte Ausführungsbeispiel entspricht im Wesentlichen dem ersten Ausführungsbeispiel, auf dessen Beschreibung hiermit verwiesen wird. Der zentrale Unterschied zum ersten Ausführungsbeispiel besteht darin, dass als Ausgangsstoff Siliziumlegierungen eingesetzt werden, welche katalytisch aktive Übergangsmetalle enthalten. Als Ausgangsstoff dient insbesondere Ferrosilizium. Der Ausgangsstoff liegt vor seiner Zerkleinerung als Granulat mit einer Granulatgröße von bis zu einigen Zentimetern Durchmesser vor. Wie beim zweiten Ausführungsbeispiel kann während - A -In the following, a third embodiment of the method will be described. The third embodiment substantially corresponds to the first embodiment, the description of which is hereby incorporated by reference. The main difference from the first embodiment is that as starting material silicon alloys are used which contain catalytically active transition metals. The starting material is in particular ferrosilicon. The raw material is present before its comminution as granules with a granule size of up to a few centimeters in diameter. As in the second embodiment, during - A -

des Zerkleinerns getrocknetes Kupferchlorid als Katalysator zugegeben werden.crushed copper chloride may be added as a catalyst.

Die nach einem der obigen Verfahren hergestellten Silane und/oder Silan- Derivate werden zur Herstellung von Reinstsilizium für photovoltaische Zwecke verwendet. Es ist ebenso möglich, die derart hergestellten Silane zur Herstellung linearer und/oder verzweigter Polysiloxane zu verwenden. The silanes and / or silane derivatives prepared by one of the above processes are used for the production of ultrapure silicon for photovoltaic purposes. It is also possible to use the silanes prepared in this way for the preparation of linear and / or branched polysiloxanes.

Claims

Patentansprüche claims 1. Verfahren zur Herstellung von Silanen und/oder deren Derivaten mit einer Restgruppe aus der Gruppe der Halogen-, Alkyl-, Aryl-, Alkoxy- oder Amin- Verbindungen, umfassend die folgenden Schritte:1. A process for the preparation of silanes and / or derivatives thereof with a radical group from the group of halogen, alkyl, aryl, alkoxy or amine compounds, comprising the following steps: - Bereitstellen eines Silizium aufweisenden Ausgangsstoffes,Providing a silicon-containing starting material, - Zerkleinern des Ausgangsstoffes zu Partikeln mit einem Durchmesser im Bereich von 0.1 μm bis 1 cm, wobei die Zerkleinerung des Ausgangsstoffes mittels gepulster Stoßwellen geschieht, und- crushing of the starting material into particles having a diameter in the range of 0.1 .mu.m to 1 cm, wherein the comminution of the starting material is done by means of pulsed shock waves, and Umsetzen der Partikel in einem Reaktor.Reacting the particles in a reactor. 2. Verfahren gemäß Anspruch 1, dadurch gekennzeichnet, dass die Korngrößenverteilung der Partikel ein Maximum im Bereich von 1 μm bis 500 μm aufweist.2. The method according to claim 1, characterized in that the particle size distribution of the particles has a maximum in the range of 1 micron to 500 microns. 3. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Korngrößenverteilung der Partikel ein Maximum im Bereich von 3 μm bis 8 μm aufweist.3. The method according to any one of the preceding claims, characterized in that the particle size distribution of the particles has a maximum in the range of 3 microns to 8 microns. 4. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Korngrößenverteilung der Partikel ein Maximum im Bereich von 100 μm bis 300 μm aufweist.4. The method according to any one of the preceding claims, characterized in that the particle size distribution of the particles has a maximum in the range of 100 microns to 300 microns. 5. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Zerkleinerung in einer Gasatmosphäre mit einem Restsauerstoffgehalt von höchstens 1 %, insbesondere höchstens 1 %o, insbesondere höchstens 0.25 %o geschieht. 5. The method according to any one of the preceding claims, characterized in that the comminution takes place in a gas atmosphere with a residual oxygen content of at most 1%, in particular at most 1% o, in particular at most 0.25% o. 6. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Zerkleinerung in einer Gasatmosphäre mit einem Restwassergehalt von höchstens 1 %o, insbesondere höchstens 0,1 %o, insbesondere höchstens 0.01 %o geschieht.6. The method according to any one of the preceding claims, characterized in that the comminution in a gas atmosphere with a residual water content of at most 1% o, in particular at most 0.1% o, in particular at most 0.01% o happens. 7. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Zerkleinerung in einer Inertgas-Atmosphäre geschieht.7. The method according to any one of the preceding claims, characterized in that the comminution takes place in an inert gas atmosphere. 8. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass vor dem Zerkleinern und/oder vor dem Umsetzen des Ausgangsstoffes ein Katalysator zugegeben wird.8. The method according to any one of the preceding claims, characterized in that a catalyst is added before crushing and / or before reacting the starting material. 9. Verfahren gemäß Anspruch 5, dadurch gekennzeichnet, dass als Kata- lysator Kupferchlorid, insbesondere getrocknetes Kupferchlorid, vorgesehen ist.9. Process according to claim 5, characterized in that copper chloride, in particular dried copper chloride, is provided as the catalyst. 10. Verfahren gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass als Ausgangsstoff metallurgisches Silizium und/oder Ferrosilizium vorgesehen ist.10. The method according to any one of the preceding claims, characterized in that as starting material metallurgical silicon and / or ferrosilicon is provided. 11. Verwendung der Silane hergestellt nach einem der vorhergehenden Ansprüche zur Herstellung von Reinstsilizium für photovoltaische Zwecke. 11. Use of the silanes prepared according to one of the preceding claims for the production of ultrapure silicon for photovoltaic purposes.
PCT/EP2009/003260 2008-05-20 2009-05-07 Production and use of fine-particle silicon Ceased WO2009141062A2 (en)

Applications Claiming Priority (2)

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DE102008024411.2 2008-05-20
DE102008024411A DE102008024411A1 (en) 2008-05-20 2008-05-20 Production and use of finely divided silicon

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8939336B2 (en) 2011-12-21 2015-01-27 Wacker Chemie Ag Polycrystalline silicon portion and method for breaking a silicon body

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4676967A (en) * 1978-08-23 1987-06-30 Union Carbide Corporation High purity silane and silicon production
DE4218283A1 (en) * 1992-05-27 1993-12-02 Wacker Chemitronic Process for the contamination-free comminution of semiconductor material, in particular silicon
DE10061680A1 (en) 2000-12-11 2002-06-20 Solarworld Ag Process for the production of silane
DE10259456B4 (en) 2002-12-19 2005-02-03 Baron, Alfred, Dr.-Ing. Process and apparatus for disintegration and tribochemical activation of inorganic substances
DE102006027273B3 (en) * 2006-06-09 2007-10-25 Adensis Gmbh Production of ultra-clean silicon to manufacture solar cells, comprises melting impurities contained in metallurgical silicon using solidification on a casting mold surface and mechanically removing the impurities from the mold

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8939336B2 (en) 2011-12-21 2015-01-27 Wacker Chemie Ag Polycrystalline silicon portion and method for breaking a silicon body

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WO2009141062A3 (en) 2010-05-06

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