WO2012143350A1 - Ensemble creuset - Google Patents

Ensemble creuset Download PDF

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Publication number
WO2012143350A1
WO2012143350A1 PCT/EP2012/056993 EP2012056993W WO2012143350A1 WO 2012143350 A1 WO2012143350 A1 WO 2012143350A1 EP 2012056993 W EP2012056993 W EP 2012056993W WO 2012143350 A1 WO2012143350 A1 WO 2012143350A1
Authority
WO
WIPO (PCT)
Prior art keywords
crucible
film
arrangement according
graphite
silicon
Prior art date
Application number
PCT/EP2012/056993
Other languages
German (de)
English (en)
Inventor
Martin Cadek
Johann Daimer
Bodo Frings
Hartwig Rauleder
Original Assignee
Sgl Carbon Se
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sgl Carbon Se filed Critical Sgl Carbon Se
Publication of WO2012143350A1 publication Critical patent/WO2012143350A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers

Definitions

  • the present invention relates to a crucible assembly for melting and crystallizing a substance, in particular a metal, such as silicon, as well as their use for melting and crystallizing preferably silicon.
  • crucibles In the production of crystalline silicon, as required for example for the semiconductor industry or photovoltaics, special crucibles are used to receive and crystallize the silicon melt.
  • molten silicon is crystallized in a directionally open manner in an open-topped crucible by controlled heat removal, the crystallization proceeding from the bottom of the crucible to the top.
  • the crucible is held by an outer support frame in the correct position.
  • the crucible including the associated support frame is usually arranged in a crystallization furnace.
  • the inner wall of such a crucible in contact with the silicon melt must have a high degree of purity.
  • crucibles of the aforementioned type can also be made by joining several items.
  • Corresponding crucibles of several joined graphite plates are e.g. known from US 2006/0219162 A1.
  • a problem with the type of silicon production described is the ever-present risk of leakage of molten silicon from the Horny pickup cavity of crucible. Such leakage may occur, for example, as a result of cracks in the crucible wall which usually form during the melting or solidification process, because silicon undergoes an increase in volume of about 1 1% during solidification, as a result of which enormous forces are exerted on the crucible wall.
  • molten silicon can escape in particular at the joints. Since molten silicon is highly reactive, it can in the event of leakage, the support frame and components of the crystallization furnace, such as its isolation, attack and damage, resulting in longer downtime of the associated manufacturing plant by itself.
  • this object is achieved by a crucible arrangement having the features of claim 1 and in particular by a crucible arrangement for melting and crystallizing a metal, in particular silicon, wherein the crucible arrangement comprises:
  • a graphite-containing film which is at least partially disposed between the outer wall of the crucible and the support frame.
  • the crucible arrangement thus comprises a graphite-containing film, which is arranged at least in regions between the outer wall of the crucible and the support frame.
  • the film acts as a flexible protective cover for the crucible, which absorbs and retains molten metal emerging from the crucible.
  • the foil prevents, in particular, the passage of molten metal leaving the crucible into contact with the support frame or with parts of the associated crystallization furnace. As a result, damage to the components of the furnace and in particular the furnace insulation and thus downtime of the manufacturing plant can be avoided.
  • the film is flexible and does not break even at thermal stresses, it can be used several times.
  • the support frame can basically be used several times.
  • a further advantage of the crucible arrangement according to the invention results from the fact that molten metal emerging from the crucible reacts with the graphite contained in the foil to form a metal carbide, whereby a barrier layer is formed.
  • the barrier layer is silicon and silicon carbide and is typically less than 1 mm thick. This barrier layer acts as a diffusion barrier, ie it impedes the diffusion-dependent The passage of contaminants and thus blocks the migration of impurities, such as silicon carbide, in the crucible during the melting and crystallization process. In this way, impurities of the silicon block produced can be reliably prevented or at least considerably reduced, whereby in particular a cutting off of the edge regions of the solidified silicon block can be dispensed with.
  • a graphite foil is further characterized by a relatively high thermal conductivity and therefore contributes to a more uniform heating and cooling of the crucible.
  • the crucible assembly according to the present invention reduces both the cost of materials and downtime in the crystallization of silicon, and thus, overall, enables more economical production of crystalline silicon.
  • the film is made entirely of graphite. In this way, impurities of the silicon melt are avoided by other film materials.
  • all common Graphitsorten can be used for the production of the film.
  • preforming of the film can be carried out by means of a tool which is known in principle.
  • the graphite is preferably expanded graphite.
  • the film consists of very pure graphite, preferably with an ash content of less than 500 ppm, namely preferably graphite, which has been purified by a halogen treatment.
  • a graphite material purified by a halogen treatment has a sufficiently high degree of purity to prevent contamination of melt leaving the crucible by the film itself, such as contamination with oxygen. In principle, however, it is also possible although less preferred to use an unpurified graphite foil.
  • the halogen treatment may for example be such that the graphite foil is charged with a halogen or with a halogen mixture and is left at a predetermined cleaning temperature of, for example, 2300 to 3000 ° C for a certain period of time. Contaminants present in the graphite react with the halogen (s) at the elevated temperature and volatilize, which is why the remaining graphite material has a particularly high degree of purity.
  • the halogens can be comparatively deep in the described cleaning process, i. up to 30 cm, penetrate into the graphite layers, so that the film is reliably cleaned in its entire volume.
  • a measure of the purity of the graphite is the ash content.
  • Commercially available material types have an ash value according to DIN 51903 of four percent to 0.15 percent or from 40,000 to 1,500 ppm.
  • the ash content of the graphite foil material is below 500 ppm, which can be obtained by the described cleaning of the graphite foil material.
  • the film is integrally formed. This ensures a secure collection of leaking melt through the film, as there are no seams or transitions as potential leaks.
  • the film is held by the support frame. That is, the support frame can hold both the crucible and the film, so that no attachment of the film to the crucible wall is necessary.
  • the one-piece film is folded in the form of several overlapping film layers. As a result, a further improved protective effect can be achieved.
  • the film can be folded along fold areas with rounded corners.
  • the outer wall of the crucible is completely enveloped by the film at least up to the filling level of the melt.
  • the area between the support frame and the crucible is completely lined by the film, so that any emerging from the crucible melt is reliably collected regardless of the exit location and therefore can not reach the support frame or can absorb impurities there.
  • the film may be at least partially spaced from the outer wall of the crucible. This has the advantage that any deformations of the crucible due to thermal expansion and contractions do not affect the film. Rather, the film envelops the crucible wall continuously.
  • the present invention is not limited in the thickness of the film.
  • good results are obtained especially when the single-layer film has a thickness between 0.2 mm and 5 mm, and preferably between 0.5 mm and 2 mm. This ensures sufficient stability, taking into account the required flexibility of the film.
  • the film has a density of 0.7 g / cm 3 to 1.0 g / cm 3 . This is generally sufficient in terms of a reliable sealing effect. In principle, a comparatively low density and thus a higher compressibility can contribute to compensate for a bulge of the crucible during the melting or crystallization process. This prevents Dangerous stresses in the support frame and thus increases its life or the number of feasible melting / crystallization cycles before replacement of the support frame is required.
  • expanded graphite is placed in a die of at least two parts and compacted and molded at a pressure of at least 10 MPa and at most 100 MPa.
  • the compacted and molded part is removed from the mold and placed in a mold of the same geometry of the forming surfaces of temperature resistant material and cleaned at a temperature above 2000 ° C in an atmosphere containing a halogen or in a halogen containing gas.
  • the thus obtained compacted, formed and cleaned expanded graphite part is taken out of the mold and used as the film according to the invention.
  • the ash value of the film thus produced is less than 500 ppm.
  • the film may be provided at least in regions with a coating comprising silicon nitride.
  • a coating comprising silicon nitride.
  • silicon nitride coating acts as a release agent, which allows easier removal of the film from the outer wall of the crucible after completion of the crystallization process. Due to the easy removability, the film is reusable, whereby the efficiency of the manufacturing process is improved.
  • the crucible is assembled from a plurality of, in particular plate-shaped, individual parts.
  • the size of the crucible and thus the size of the producible silicon block in wide ranges to the requirements of the respective Application to be customized.
  • such a Fügebau way allows easy extension of an existing crucible.
  • one-piece crucibles - which are conventionally manufactured, for example, in slip casting using appropriate molds - this is associated with a significant overhead, since for the production of a larger or differently shaped crucible only a corresponding mold must be created.
  • relatively flat-shaped crucible can be easily produced by the Fügebau way.
  • the film covers at least all joints to which the individual parts are joined.
  • the film is dimensioned and arranged in such a way that only the joints are protected.
  • the present invention is not limited.
  • the items may be joined together in particular by means of at least one connecting element made of temperature-resistant material.
  • connecting elements for example, pins, bolts, screws, clamps, dowels, Lamellos or the like may be provided.
  • form-fitting interlocking connection sections can be formed directly on the individual parts, such as combinations of tongue and groove or dovetail connections.
  • a temperature-resistant material in particular quartz, graphite, carbon fiber reinforced composites (CFC), silicon carbide (SiC), silicon nitride (S13N4), zirconium oxides and metals such as titanium, tungsten or molybdenum.
  • the crucible is cuboid in accordance with another embodiment of the present invention. This is particularly advantageous in a crucible production in joint construction, as a cuboid crucible can be easily assembled from prefabricated panels. If the application so requires, other crucible shapes can be realized by e.g. in a known manner, two complementary half-forms are joined together.
  • the crucible may be made of any material known to those skilled in the art, such as graphite, silica, or a mixture of silica with one or more other materials, such as silicon nitride. Good results are obtained, in particular, when the crucible is made of silicon dioxide and preferably of high-purity silicon dioxide.
  • high-purity silica is meant in this connection silicon dioxide with a SiO 2 content of at least 99%.
  • the amounts of impurities do not exceed those amounts described in claim 1 1 of WO 2010/037702 Al or in claim 12 of WO 2010/037705 Al, the disclosures of which are hereby incorporated by reference.
  • a crucible of such high purity silica is sufficiently resistant to molten silicon and prevents unwanted impurities from entering the melt.
  • starting materials for the silica to be provided for the production of crucibles it is possible in particular to use natural quartz, pyrogenic or precipitated silicic acid or fused silica in an electric arc furnace.
  • According to one embodiment of the invention are from Cast the mentioned starting materials silica shaped body, which are optionally sintered. In this way, in particular low-stress silicon dioxide plates for the assembly of a crucible base body can be manufactured.
  • an inner wall of the crucible with a sizing, which contains in particular silicon nitride.
  • a sizing which contains in particular silicon nitride.
  • Such a size can form a smoothing coating of the inner wall and in particular act as a sealant and / or as a release agent.
  • a silicon nitride size may provide additional protection against leaking silicon.
  • adhesion of the resulting silicon crystal to the crucible wall can be prevented. It is up to the particular application, whether the coating of the inner wall of the crucible with the sizing takes place before any assembly of the crucible of several individual parts or just before the use of the crucible for melting and crystallization.
  • a silicon nitride-containing sizing is applied as a spreadable mass of a silicon nitride-containing powder distributed in a binder on the inner wall of the crucible, for example by brushing or knife coating, and subsequently baked.
  • the burning-in can be carried out immediately prior to assembly or even before the individual parts are sintered, depending on the application.
  • the silicon nitride-containing layer could also be applied to the finished sintered items.
  • the sizing can only be applied to the joints in order to save material.
  • the entire inner wall of the crucible may also be coated with the size.
  • the support frame is made of graphite.
  • a graphite rack has sufficient thermal resistance to carry out the melting and crystallization process in a crystallization oven, and is also resistant to possible contact with molten silicon.
  • the crucible may have a size (BxLxH) of at least 400 mm ⁇ 400 mm ⁇ 250 mm, preferably of at least 600 mm x 600 mm ⁇ 350 mm and particularly preferably of at least 700 mm ⁇ 700 mm x 380 mm.
  • the size specifications refer to the outer dimensions of the length, the width and the height of a rectangular crucible. In the case of a crucible with non-cuboid external dimensions, the details given refer to the smallest cuboid circumscribing the crucible.
  • Such large crucibles can traditionally only be produced with unacceptably high costs and also have a relatively high risk of failure.
  • Another object of the present invention is the use of a previously described crucible arrangement for melting and crystallizing metals, and preferably of silicon.
  • FIG. 1 is a side sectional view of a crucible assembly according to the invention comprising a crucible, a support frame and a film,
  • FIG. 2 is a perspective view of two parts to be joined together of a support frame for the crucible arrangement according to FIG. 1,
  • Fig. 3 is a plan view of the items according to FIG. 2, which shows these in the assembled state, and
  • FIG. 4 shows a film to be folded for the crucible arrangement according to FIG. 1.
  • a crucible arrangement according to the invention is constructed as a layer composite and comprises, viewed from the outside inwards, a support frame 1 1 made of graphite, a flexible graphite foil 13, a crucible 15 made of silicon dioxide and a crucible coating 17 in the form of a silicon nitride sizing.
  • the crucible 15 is cuboid and has an upper opening 23.
  • the inner wall 16 of the crucible 15, which defines a receiving cavity for a silicon melt, is completely covered by the crucible coating 17.
  • the outer wall 18 of the crucible 15 is completely enveloped by the graphite foil 13, which is arranged between the crucible 15 and the support frame 1 1 and in turn is completely enveloped by the support frame 1 1.
  • the support frame 1 1 thus forms a holder for both the crucible 15 and the graphite foil 13th
  • the graphite foil 13 is made entirely of expanded graphite, which is purified by a halogen treatment and has a correspondingly high degree of purity.
  • the graphite foil preferably has a uniform thickness. between 0.5 mm and 2 mm.
  • the support frame 1 1 is made of several parts. Specifically, a bottom plate 19 is connected by means of a threaded pin connection 25 with a plurality of side plates 21 - of which only one is shown in FIGS. 2 and 3 - connected.
  • the crucible 15 shown in FIG. 1 is also assembled from a plurality of plate-shaped components made of high-purity silica by casting and subsequent sintering and joined together using high-temperature-resistant bonding agents.
  • the graphite foil 13 is manufactured in one piece and is folded along predetermined fold lines 30 into a cuboid mold surrounding the crucible 15 and open on one side.
  • predetermined fold lines 30 into a cuboid mold surrounding the crucible 15 and open on one side.
  • respective overlapping regions 35 located between the lateral regions 33 are produced, which are each folded as additional film layers under or over one of the adjacent lateral regions 33.
  • the crucible assembly of Fig. 1 is placed in a crystallization furnace and silicon present in the crucible 15 is melted and subsequently solidified, as is well known in the art. Should it come to a leakage of molten silicon from the crucible 15, for example, by a resulting crack or a joint gap, the outflowing melt is safely collected by the graphite foil 13 and thus can not penetrate to the support frame 1 1. By a reaction of the leaked silicon with the graphite foil 13 This results in the formation of a barrier layer of silicon carbide (SiC), which prevents back diffusion of impurities in the crucible 15.
  • SiC silicon carbide
  • the crystallized silicon is removed from the crucible 15 and the usually cracked crucible 15 is replaced by a new one.
  • the graphite foil 13, on the other hand, can be reused for the next production process. However, if the graphite foil 13 is excessively attacked and flakes, for example, it is also replaced. Such replacement is usually required after about 5 manufacturing operations. Also, the support frame 1 1 can be reused in principle.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne un ensemble creuset pour la fusion et la cristallisation d'une matière, notamment d'un métal, par exemple du silicium, comprenant un creuset (15) pour recevoir un bain fondu, un creuset-support (11) externe pour maintenir le creuset (15) et un film (13) qui contient un graphite et qui est disposé au moins dans certaines zones entre la paroi externe (18) du creuset (15) et le creuset-support (11).
PCT/EP2012/056993 2011-04-19 2012-04-17 Ensemble creuset WO2012143350A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011007708A DE102011007708A1 (de) 2011-04-19 2011-04-19 Tiegelanordnung
DE102011007708.1 2011-04-19

Publications (1)

Publication Number Publication Date
WO2012143350A1 true WO2012143350A1 (fr) 2012-10-26

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ID=45976397

Family Applications (1)

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PCT/EP2012/056993 WO2012143350A1 (fr) 2011-04-19 2012-04-17 Ensemble creuset

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DE (1) DE102011007708A1 (fr)
WO (1) WO2012143350A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109402733A (zh) * 2018-09-26 2019-03-01 江苏美科硅能源有限公司 一种低金属污染的全熔高效硅锭的制备方法
CN115261798A (zh) * 2021-04-30 2022-11-01 云谷（固安）科技有限公司 一种坩埚和蒸镀装置

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JPH0421509A (ja) * 1990-05-16 1992-01-24 Toyo Tanso Kk 高純度可撓性膨張黒鉛シート及びその製造方法
US20030113488A1 (en) * 2001-12-19 2003-06-19 Wacker Siltronic Ag Device for holding a molten semiconductor material
US20060219162A1 (en) 2005-04-01 2006-10-05 G.T. Equipment Technologies, Inc. Solidification of crystalline silicon from reusable crucible molds
EP2143830A1 (fr) * 2007-04-06 2010-01-13 Toyo Tanso Co., Ltd. Procédé de protection d'un creuset carboné et dispositif de tirage de monocristal
WO2010037702A1 (fr) 2008-09-30 2010-04-08 Evonik Degussa Gmbh Procédé de préparation de sio2 de grande pureté à partir de solutions silicate
WO2010037705A1 (fr) 2008-09-30 2010-04-08 Evonik Degussa Gmbh Procédé de préparation de sio2 de grande pureté à partir de solutions silicate
WO2010112259A1 (fr) * 2009-04-01 2010-10-07 H.C. Starck Gmbh Creuset pour le silicium convenant à la fabrication de semi-conducteurs

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DE10250824A1 (de) * 2001-12-19 2003-07-10 Wacker Siltronic Halbleitermat Vorrichtung zum Aufnehmen einer Schmelze aus Halbleitermaterial
DE10204468C1 (de) * 2002-02-05 2003-06-18 Sgl Carbon Ag Verfahren zur Herstellung von hochreinen Verschleißeinlagen, nach dem Verfahren erhältliche Verschleißeinlage und deren Verwendung
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US4888242A (en) * 1986-05-27 1989-12-19 Toyo Tanson Co., Ltd. Graphite sheet material
JPH0421509A (ja) * 1990-05-16 1992-01-24 Toyo Tanso Kk 高純度可撓性膨張黒鉛シート及びその製造方法
US20030113488A1 (en) * 2001-12-19 2003-06-19 Wacker Siltronic Ag Device for holding a molten semiconductor material
US20060219162A1 (en) 2005-04-01 2006-10-05 G.T. Equipment Technologies, Inc. Solidification of crystalline silicon from reusable crucible molds
EP2143830A1 (fr) * 2007-04-06 2010-01-13 Toyo Tanso Co., Ltd. Procédé de protection d'un creuset carboné et dispositif de tirage de monocristal
WO2010037702A1 (fr) 2008-09-30 2010-04-08 Evonik Degussa Gmbh Procédé de préparation de sio2 de grande pureté à partir de solutions silicate
WO2010037705A1 (fr) 2008-09-30 2010-04-08 Evonik Degussa Gmbh Procédé de préparation de sio2 de grande pureté à partir de solutions silicate
WO2010112259A1 (fr) * 2009-04-01 2010-10-07 H.C. Starck Gmbh Creuset pour le silicium convenant à la fabrication de semi-conducteurs

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109402733A (zh) * 2018-09-26 2019-03-01 江苏美科硅能源有限公司 一种低金属污染的全熔高效硅锭的制备方法
CN115261798A (zh) * 2021-04-30 2022-11-01 云谷（固安）科技有限公司 一种坩埚和蒸镀装置

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