DE3403131A1 - Process for refining silicon produced in an arc furnace - Google Patents

Process for refining silicon produced in an arc furnace

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Publication number
DE3403131A1
DE3403131A1 DE19843403131 DE3403131A DE3403131A1 DE 3403131 A1 DE3403131 A1 DE 3403131A1 DE 19843403131 DE19843403131 DE 19843403131 DE 3403131 A DE3403131 A DE 3403131A DE 3403131 A1 DE3403131 A1 DE 3403131A1
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DE
Germany
Prior art keywords
silicon
crucible
quartz
arc furnace
unreduced
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
DE19843403131
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German (de)
Inventor
Hans J. Dipl.-Ing. 8000 München Fenzl
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens AG
Original Assignee
Siemens AG
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Filing date
Publication date
Application filed by Siemens AG filed Critical Siemens AG
Priority to DE19843403131 priority Critical patent/DE3403131A1/en
Publication of DE3403131A1 publication Critical patent/DE3403131A1/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C01B33/037—Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention relates to a process for refining silicon produced in an arc furnace, removing non-reduced quartz or unreacted carbon. To this end, the silicon is fused in a highly compacted graphite crucible (4) or a quartz crucible, as a result of which the non-reduced quartz and the unreacted carbon collect on the crucible wall. If required, it is also possible to charge the graphite crucible with slag- or glass-forming fluxes. Subsequently, the silicon thus refined is processed further by means of zone drawing or, according to Czochralski, into single crystals. <IMAGE>

Description

Verfahren zum Reinigen von i-m Lichtbogenofen erzeugtemProcess for cleaning produced by i-m arc furnace

Silicium Die Erfindung betrifft ein Verfahren zum Reinigen von im Lichtbogenofen erzeugtem Silicium von nichtreduziertem Quarz und nichtreagierter Kohle.Silicon The invention relates to a method for cleaning im Arc furnace produced silicon from unreduced quartz and unreacted Money.

In der DE-OS 32 21 675 ist ein Lichtbogenofen zur Herstellung von Silicium beschrieben. In diesem Lichtbogenofen wird Quarz mit Kohle reduziert, um so Silicium zu gewinnen. Der Ofen selbst ist mit einer Auskleidungsschicht versehen, die den Boden und die Seitenwand des Innenraums des Ofens bedeckt. Zusätzlich ist auf der Innenseite der Auskleidungsschicht noch eine Pyrographitschicht vorgesehen, die möglichst von Verunreinigungen frei und gasundurchlässig bzw. gasdicht ist, um so das Silicium möglichst rein aus dem Quarz mittels der Kohle gewinnen zu können.In DE-OS 32 21 675 an arc furnace for the production of Silicon described. In this electric arc furnace, quartz is reduced to with carbon so to gain silicon. The furnace itself is provided with a lining layer, which covers the bottom and the side wall of the interior of the furnace. Additionally is a pyrographite layer is also provided on the inside of the lining layer, which is as free of impurities as possible and gas-impermeable or gas-tight, in order to be able to extract the silicon as pure as possible from the quartz by means of the coal.

Es hat sich aber gezeigt, daß das mit einem derartigen Lichtbogenofen erzeugte Silicium immer noch so stark mit Verunreinigungen angereichert ist, daß eine Weiterverarbeitung durch Kristallziehen nicht möglich ist. Insbesondere läßt sich Silicium mit einem großen Gehalt an nichtreduziertem Quarz und nichtreagierter Kohle nicht direkt in einer Tiegelziehmaschine schmelzen und zu den gewünschten Einkristallen ziehen.But it has been shown that that with such an arc furnace silicon produced is still so highly contaminated that further processing by crystal pulling is not possible. In particular, lets silicon with a large content of unreduced quartz and unreacted Do not melt coal directly in a crucible drawing machine and get the desired result Pulling single crystals.

Es ist daher Aufgabe der Erfindung, ein möglichst einfaches Verfahren zu schaffen, das eine Reinigung des aus einem Lichtbogenofen durch Reduktion von Quarz mit Kohle gewonnenem Siliciums erlaubt, so daß dieses nach einer derartigen Reinigung beispielsweise durch Zonenziehen oder nach Czochralski weiterverarbeitet werden kann.It is therefore the object of the invention to provide a method that is as simple as possible to create a cleaning of the from an electric arc furnace by reduction of Quarz with coal obtained silicon allowed, so that this after a such Cleaning, for example, by zone drawing or further processed according to Czochralski can be.

Diese Aufgabe wird bei einem Verfahren zum Reinigen von im Lichtbogenofen erzeugtem Silicium von nichtreduziertem Quarz und nichtreagierter Kohle erfindungsgemäß dadurch gelöst, daß das mit dem nichtreduzierten Quarz und der nichtreagierten Kohle verunreinigte Silicium in einem hochverdichteten Graphittiegel oder einem Quarztiegel aufgeschmolzen und das Silicium anschließend abgegossen wird.This task is performed in a method for cleaning in the electric arc furnace produced silicon from unreduced quartz and unreacted carbon according to the invention solved by that with the unreduced quartz and the unreacted carbon contaminated silicon in a high density graphite crucible or quartz crucible melted and the silicon is then poured off.

Durch eine derartige Behandlung bilden sich die unerwünschten Verunreinigungen aus insbesondere nichtreduziertem Quarz und nichtreagierter Kohle an der Tiegelwand, so daß am Ende des Schmelzvorgangs das Silicium auf einfache Weise abgegossen werden kann. Dieses Silicium ist dann - wie Versuche gezeigt haben - soweit gereinigt, daß es entweder durch Zonenziehen oder nach Czochralski zu Einkristallen weiterverarbeitet werden kann.Such treatment creates the undesirable impurities in particular made of unreduced quartz and unreacted carbon on the crucible wall, so that at the end of the melting process the silicon can be poured off in a simple manner can. This silicon is then - as tests have shown - purified to the extent that that it is processed into single crystals either by zone pulling or according to Czochralski can be.

Die Ausbeute bei dem erfindungsgemäßen Verfahren ist wesentlich besser als bei dem herkömmlichen Verfahren, bei dem das im Lichtbogenofen gewonnene Silicium direkt einer Tiegelziehmaschine zugeführt wird. Wird eine Tiegelziehmaschine direkt zum Schmelzen des aus dem Lichtbogenofen gewonnenen Siliciums verwendet, dann können nur Bruchteile des Siliciums abgezogen werden, da der größere Anteil im Tiegel zurückbleibt, was äußerst unwirtschaftlich ist, da die im Tiegel zurückbleibende Restschmelzmenge beim Erstarren den Tiegel zerstören kann.The yield in the process according to the invention is significantly better than the conventional method in which the silicon obtained in the arc furnace is fed directly to a crucible drawing machine. Becomes a crucible drawing machine directly used to melt the silicon obtained from the arc furnace, then can only fractions of the silicon are withdrawn, since the greater part remains in the crucible, which is extremely uneconomical, since the residual amount of melt remaining in the crucible can destroy the crucible when solidifying.

In vorteilhafter Weise werden in den Graphittiegel bzw.Advantageously, the graphite crucible or

in den Quarztiegel schlacken- oder glasbildende Zuschlagstoffe zugegeben, die zusätzlich eine Reinigung des Sili- ciums bewirken. Solche Zuschlagstoffe sind beispielsweise MgO, CaO oder BaO.slag- or glass-forming additives are added to the quartz crucible, which also requires cleaning of the silicone cause ciums. Such aggregates are for example MgO, CaO or BaO.

Nachfolgend wird ein Ausführungsbeispiel der Erfindung an Hand der Zeichnung näher erläutert, in deren einziger Figur ein hochverdichteter Graphittiegel zur Durchführung des erfindungsgemäßen Verfahrens gezeigt ist.An exemplary embodiment of the invention is described below with reference to the Drawing explained in more detail, in the single figure a highly compressed graphite crucible for performing the method according to the invention is shown.

In der Figur ist in einem Ofen 1 ein Tiegel 4 aus Graphit oder Quarz dargestellt, der durch eine in einem feuerfesten Stoff 2 eingebettete Heizwendel 3 oder durch Hochfrequenz beheizt wird. Die Rückstände aus nichtreduziertem Quarz und nicht reduziertem Kohlenstoff scheiden sich an der Innenseite des Tiegels 4 ab.In the figure, a crucible 4 made of graphite or quartz is in a furnace 1 shown by a heating coil embedded in a refractory material 2 3 or heated by high frequency. The residues of unreduced quartz and non-reduced carbon are deposited on the inside of the crucible 4 away.

Der Ofen 1 kann beispielsweise auch in der in der DE-OS 32 21 675 beschriebenen Weise betrieben werden.The furnace 1 can, for example, also be described in DE-OS 32 21 675 operated manner.

In diesem Fall können die Heizschlangen 3 entfallen.In this case, the heating coils 3 can be omitted.

In den Tiegel 4 werden bevorzugt schlacken- oder glasbildende Zuschlagstoffe, wie beispielsweise MgO, CaO, BaO eingegeben, so daß sich metallische Verunreinigungen zusätzlich an diesen Zuschlagstoffen ansammeln und abscheiden. Slag- or glass-forming aggregates, such as MgO, CaO, BaO, are preferably added to the crucible 4, so that metallic impurities also collect and deposit on these aggregates.

1 Figur1 figure

Claims (3)

Patentansprüche 1. Verfahren zum Reinigen von im Lichtbogenofen erzeugtem Silicium von nichtreduziertem Quarz und nichtreagierter Kohle, d a d u r c h g e k e n n z e i c h n e t daß das mit dem nichtreduzierten Quarz und der nichtreagierten Kohle verunreinigte Silicium in einem hochverdichteten Graphittiegel (4) oder einem Quarztiegel aufgeschmolzen und das Silicium anschließend abgegossen wird.Claims 1. A method for cleaning generated in the arc furnace Silicon of unreduced quartz and unreacted carbon, d a d u r c h g e I do not know that the one with the unreduced quartz and the unreacted one Coal contaminated silicon in a highly compressed graphite crucible (4) or a Quartz crucible is melted and the silicon is then poured off. 2. Verfahren nach Anspruch 1, d a d u r c h g e -k e n n z e i c h n e t , daß in den Graphittiegel (4) bzw. in den Quarztiegel schlacken- oder glasbildende Zuschlagstoffe zugegeben werden.2. The method according to claim 1, d a d u r c h g e -k e n n z e i c h n e t that slag or glass-forming in the graphite crucible (4) or in the quartz crucible Aggregates are added. 3. Verfahren nach Anspruch 2, d a d u r c h g e -k e n n z e i c h n e t , daß als Zuschlagstoffe MgO, CaO oder BaO verwendet werden.3. The method according to claim 2, d a d u r c h g e -k e n n z e i c h n e t that MgO, CaO or BaO are used as additives.
DE19843403131 1984-01-30 1984-01-30 Process for refining silicon produced in an arc furnace Withdrawn DE3403131A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE19843403131 DE3403131A1 (en) 1984-01-30 1984-01-30 Process for refining silicon produced in an arc furnace

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3726171A1 (en) * 1986-08-07 1988-02-11 Showa Aluminum Corp METHOD AND DEVICE FOR CLEANING SILICON
DE3627624A1 (en) * 1986-08-14 1988-02-18 Bayer Ag METHOD FOR PRODUCING LOW CARBON SILICON
DE4122190A1 (en) * 1991-07-04 1993-01-14 Wacker Chemie Gmbh METHOD AND DEVICE FOR THE CONTINUOUS TREATMENT OF SILICIUM
WO1998011018A1 (en) * 1996-09-10 1998-03-19 Elkem Metals Company L.P. Silicon refining process
US6090361A (en) * 1997-03-24 2000-07-18 Kawasaki Steel Corporation Method for producing silicon for use in solar cells
US6231826B1 (en) 1996-03-19 2001-05-15 Kawasaki Steel Corporation Process and apparatus for refining silicon
DE10358452A1 (en) * 2003-12-13 2005-07-21 Fiolitakis, Emmanuel, Dr. Preparation of high-quality silicon, useful e.g. as solar or semiconductor silicon, by high-temperature reaction of lime, carbon and silicate, then purification and thermal decomposition of the calcium silicide formed
DE102010001094A1 (en) 2010-01-21 2011-07-28 Evonik Degussa GmbH, 45128 Method for decarburizing a silicon melt
DE102010001093A1 (en) 2010-01-21 2011-07-28 Evonik Degussa GmbH, 45128 Process for the coarse decarburization of a silicon melt

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3726171A1 (en) * 1986-08-07 1988-02-11 Showa Aluminum Corp METHOD AND DEVICE FOR CLEANING SILICON
DE3627624A1 (en) * 1986-08-14 1988-02-18 Bayer Ag METHOD FOR PRODUCING LOW CARBON SILICON
DE4122190A1 (en) * 1991-07-04 1993-01-14 Wacker Chemie Gmbh METHOD AND DEVICE FOR THE CONTINUOUS TREATMENT OF SILICIUM
US6231826B1 (en) 1996-03-19 2001-05-15 Kawasaki Steel Corporation Process and apparatus for refining silicon
WO1998011018A1 (en) * 1996-09-10 1998-03-19 Elkem Metals Company L.P. Silicon refining process
US5820842A (en) * 1996-09-10 1998-10-13 Elkem Metals Company L.P. Silicon refining process
US6090361A (en) * 1997-03-24 2000-07-18 Kawasaki Steel Corporation Method for producing silicon for use in solar cells
DE10358452A1 (en) * 2003-12-13 2005-07-21 Fiolitakis, Emmanuel, Dr. Preparation of high-quality silicon, useful e.g. as solar or semiconductor silicon, by high-temperature reaction of lime, carbon and silicate, then purification and thermal decomposition of the calcium silicide formed
DE10358452B4 (en) * 2003-12-13 2005-09-15 Fiolitakis, Emmanuel, Dr. Preparation of high-quality silicon, useful e.g. as solar or semiconductor silicon, by high-temperature reaction of lime, carbon and silicate, then purification and thermal decomposition of the calcium silicide formed
DE102010001094A1 (en) 2010-01-21 2011-07-28 Evonik Degussa GmbH, 45128 Method for decarburizing a silicon melt
WO2011088953A1 (en) 2010-01-21 2011-07-28 Evonik Degussa Gmbh Process for decarburization of a silicon melt
DE102010001093A1 (en) 2010-01-21 2011-07-28 Evonik Degussa GmbH, 45128 Process for the coarse decarburization of a silicon melt
WO2011088952A1 (en) 2010-01-21 2011-07-28 Evonik Degussa Gmbh Process for coarse decarburization of a silicon melt

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