WO2006002779A1 - Procede de production d'une coquille a revetement antiadhesif - Google Patents

Procede de production d'une coquille a revetement antiadhesif Download PDF

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Publication number
WO2006002779A1
WO2006002779A1 PCT/EP2005/006534 EP2005006534W WO2006002779A1 WO 2006002779 A1 WO2006002779 A1 WO 2006002779A1 EP 2005006534 W EP2005006534 W EP 2005006534W WO 2006002779 A1 WO2006002779 A1 WO 2006002779A1
Authority
WO
WIPO (PCT)
Prior art keywords
silicon
weight
container
silicon nitride
nitride powder
Prior art date
Application number
PCT/EP2005/006534
Other languages
German (de)
English (en)
Inventor
Armin Müller
Bert Geyer
Carsten Wobst
Peter Woditsch
Original Assignee
Deutsche Solar Ag
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 Deutsche Solar Ag filed Critical Deutsche Solar Ag
Publication of WO2006002779A1 publication Critical patent/WO2006002779A1/fr

Links

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
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—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 invention relates to a method for producing a container for melting and / or crystallizing non-ferrous metals, in particular of silicon.
  • the invention further relates to a container produced by the erfindungsge ⁇ MAESSEN container.
  • the invention relates to Weite ⁇ Ren the use of a container according to the invention for receiving silicon melt.
  • WO 2004/053207 A1 discloses a container for receiving silicon and a production method for such a container, wherein a coating comprising metallic silicon, silicon nitride and silicon dioxide is sprayed onto the inner walls of the container.
  • the metallic silicon serves as a binder for the silicon nitride and silicon dioxide and is an essential component of the coating.
  • a disadvantage of containers coated in this way is that they are costly to produce as a result of the required finely dispersed and highly pure silicon powder having a particle size distribution corresponding to the silicon nitride powder and the silicon dioxide powder.
  • the metallic silicon furthermore contains metallic impurities, which in turn contaminate the silicon absorbed in the container, which has a negative effect on its quality.
  • the invention has for its object to provide a method for producing a container for melting and / or crystallizing non-ferrous metals and a corresponding container which is pondere ⁇ low and in which there is no adhesion of the non-ferrous metal to the container interior wall.
  • the essence of the invention is to apply a layer of silicon nitride powder and an inorganic, heat-resistant binder to the inner wall of the container.
  • the inorganic binder has no metallic silicon, which conversely means that the inorganic binder essentially comprises chemical compounds of at least two different chemical elements.
  • the term "essentially” is to be understood here as meaning that chemical elements or chemical compounds from a chemical element may be present in the context of unavoidable impurities, but their addition or presence is not intentionally introduced or desired.
  • the inorganic binder nevertheless providing the desired adhesion and inertness of the layer to non-ferrous metals accommodated in the container , such as iron or titanium, is reduced in the layer, which leads to an improvement in the quality of the non-ferrous metal crystallizing in the container
  • the binder binds the silicon nitride to the inner wall of the container
  • An example of the binder l is silicon dioxide.
  • the binder acts as an inorganic adhesion promoter, which is not decomposed even at the high temperatures of a silicon melt.
  • the coating produced in this way offers a substantially higher resistance to caking and sticking between the solidified silicon and the container wall and has a substantially lower contamination of the crystallized block surface of the silicon with the coating.
  • the mold blank is provided with a non-stick layer at least on its inner walls.
  • the non-stick layer consists of a mixture of silicon nitride powder and finely dispersed silica as an inorganic binder.
  • the mixture may contain 1 to 50% by weight of silicon dioxide and a corresponding proportion of silicon nitride powder.
  • the silicon dioxide powder is finely dispersed silicon dioxide, which may be hydrophilic or hydrophobic.
  • the Siliziumnitridpul ⁇ ver and the silica powder are dispersed in a solvent.
  • the inorganic binder has no, in particular less than 1 wt .-%, in particular less than 0, 1 wt .-%, in particular less than 0.01 wt .-%, and in particular less than 0.001 wt .-% of metallic silicon.
  • the application of the mixture of silicon nitride powder, silica powder and solvent is carried out, for example, by brushing, spraying, spraying, dipping or by electrostatic application of a suspension or a slurry. It is also possible to apply the mixture of silicon nitride powder and silicon dioxide in powder form to the mold inner walls.
  • the finely dispersed silicon dioxide powder and / or the silicon nitride powder have an alkali and alkaline earth metal content of ⁇ 2000 ppm, in particular ⁇ 1000 ppm, a fluoride content of ⁇ 3000 ppm, in particular ⁇ 2000 ppm, a chloride content of ⁇ 3000 ppm, in particular ⁇ 2000 ppm, a total carbon content of ⁇ 3000 ppm, in particular ⁇ 2000 ppm, and an iron, chromium, cobalt, nickel, tungsten and / or titanium content of ⁇ 1000 ppm, in particular ⁇ 500 ppm
  • the silicon dioxide powder used has a silicon dioxide concentration of at least 95% by weight, in particular at least 99% by weight, in particular at least 99.8% by weight.
  • the finely dispersed silicon dioxide has a specific surface area of at most 300 m 2 / g and an average size of the primary particles of at least 5 nm.
  • the silicon nitride powder has an oxygen content of 0.1 wt .-% to 10 wt .-%, in particular 0.3 wt .-% to 5 wt .-%, in particular 1 wt .-% to 3 wt .-% to ,
  • the ratio of length to diameter of the particles of the silicon nitride powder is less than 10.
  • the particle size of the silicon nitride powder is .ltoreq.100 .mu.m, in particular ⁇ 50 .mu.m, in particular ⁇ 30 .mu.m.
  • the silicon nitride powder contains, among other phases of silicon nitride 1% to 100% in the beta phase.
  • the silicon nitride powder may be amorphous.
  • the resulting non-stick coated molds are particularly suitable for receiving liquid silicon and for crystallization of liquid silicon to silicon ingots, rods, billets or granules.
  • the silicon produced can be used to produce silicon wafers.

Landscapes

  • 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)

Abstract

L'invention concerne un procédé de production d'un contenant destiné à la fusion et/ou à la cristallisation de métaux non ferreux, ce procédé consistant à préparer une ébauche de contenant présentant une paroi intérieure et une paroi extérieure et à appliquer une couche comprenant un mélange de poudre de nitrure de silicium et d'un liant inorganique au moins sur la paroi intérieure du contenant.
PCT/EP2005/006534 2004-06-30 2005-06-17 Procede de production d'une coquille a revetement antiadhesif WO2006002779A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004031880 2004-06-30
DE102004031880.8 2004-06-30

Publications (1)

Publication Number Publication Date
WO2006002779A1 true WO2006002779A1 (fr) 2006-01-12

Family

ID=34970498

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2005/006534 WO2006002779A1 (fr) 2004-06-30 2005-06-17 Procede de production d'une coquille a revetement antiadhesif

Country Status (1)

Country Link
WO (1) WO2006002779A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009048741A1 (de) 2009-03-20 2010-09-30 Access E.V. Tiegel zum Schmelzen und Kristallisieren eines Metalls, eines Halbleiters oder einer Metalllegierung, Bauteil für einen Tiegelgrundkörper eines Tiegels und Verfahren zum Herstellen eines Bauteils
WO2013160603A1 (fr) 2012-04-24 2013-10-31 Saint-Gobain Centre De Recherches Et D'etudes Europeen Creuset en nitrure de silicium et son procédé de fabrication
WO2014068230A1 (fr) 2012-10-31 2014-05-08 Saint-Gobain Centre De Recherches Et D'etudes Europeen Creuset incorporant un revetement sialon

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0963464B1 (fr) * 1997-02-06 2001-07-18 Deutsche Solar GmbH Creuset muni de couches de protection en silicium, procede d'application la couche de protection en silicium et utilisation
WO2002040182A1 (fr) * 2000-11-15 2002-05-23 G.T. Equipment Technologies Inc. Revetement antiadherent pour creusets
JP2003041357A (ja) * 2001-07-27 2003-02-13 Tocalo Co Ltd シリコン保持容器およびその製造方法
WO2004053207A1 (fr) * 2002-12-06 2004-06-24 Vesuvius France S.A. Recipient destine a conserver du silicium et son procede de production

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0963464B1 (fr) * 1997-02-06 2001-07-18 Deutsche Solar GmbH Creuset muni de couches de protection en silicium, procede d'application la couche de protection en silicium et utilisation
WO2002040182A1 (fr) * 2000-11-15 2002-05-23 G.T. Equipment Technologies Inc. Revetement antiadherent pour creusets
JP2003041357A (ja) * 2001-07-27 2003-02-13 Tocalo Co Ltd シリコン保持容器およびその製造方法
WO2004053207A1 (fr) * 2002-12-06 2004-06-24 Vesuvius France S.A. Recipient destine a conserver du silicium et son procede de production

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS + INDEXES, AMERICAN CHEMICAL SOCIETY. COLUMBUS, US, vol. 105, no. 4, 28 July 1986 (1986-07-28), XP000185916, ISSN: 0009-2258 *
HIDE I ET AL: "Mould shaping silicon crystal growth with a mould coating material by the spinning method", JOURNAL OF CRYSTAL GROWTH, NORTH-HOLLAND, AMSTERDAM, NL, vol. 79, no. 1-3, December 1986 (1986-12-01), pages 583 - 589, XP002252583, ISSN: 0022-0248 *
PATENT ABSTRACTS OF JAPAN vol. 2003, no. 06 3 June 2003 (2003-06-03) *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009048741A1 (de) 2009-03-20 2010-09-30 Access E.V. Tiegel zum Schmelzen und Kristallisieren eines Metalls, eines Halbleiters oder einer Metalllegierung, Bauteil für einen Tiegelgrundkörper eines Tiegels und Verfahren zum Herstellen eines Bauteils
WO2013160603A1 (fr) 2012-04-24 2013-10-31 Saint-Gobain Centre De Recherches Et D'etudes Europeen Creuset en nitrure de silicium et son procédé de fabrication
WO2014068230A1 (fr) 2012-10-31 2014-05-08 Saint-Gobain Centre De Recherches Et D'etudes Europeen Creuset incorporant un revetement sialon

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