WO2006005416A1 - Procede pour realiser une coquille presentant un revetement anti-adhesif - Google Patents

Procede pour realiser une coquille presentant un revetement anti-adhesif Download PDF

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Publication number
WO2006005416A1
WO2006005416A1 PCT/EP2005/006675 EP2005006675W WO2006005416A1 WO 2006005416 A1 WO2006005416 A1 WO 2006005416A1 EP 2005006675 W EP2005006675 W EP 2005006675W WO 2006005416 A1 WO2006005416 A1 WO 2006005416A1
Authority
WO
WIPO (PCT)
Prior art keywords
silicon
container
indicates
wall
layer
Prior art date
Application number
PCT/EP2005/006675
Other languages
German (de)
English (en)
Inventor
Peter Woditsch
Armin Müller
Bert Geyer
Bernhard Freudenberg
Carsten Wobst
Gerd Schwichtenberg
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 WO2006005416A1 publication Critical patent/WO2006005416A1/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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/001—General methods for coating; Devices therefor
    • C03C17/003—General methods for coating; Devices therefor for hollow ware, e.g. containers
    • C03C17/004—Coating the inside
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/225—Nitrides
    • 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
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/28—Other inorganic materials
    • C03C2217/281—Nitrides

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.
  • silicon nitride as non-stick coating is known from EP 0 963 464 A.
  • the effectiveness of the coating as a reliable release and release layer depends on various factors.
  • organic binders are added thereto. Due to the high temperature of the liquid silicon, the added organic adhesion promoters but decomposes, so that it always comes back to a caking of the silicon on the mold wall.
  • the invention has for its object to provide a method for producing a container for melting and / or crystallizing Tinei ⁇ senmetallen and a corresponding container, in which there is no adhesion of the non-ferrous metal to the container inner wall.
  • the core of the invention consists of applying a silicon nitride powder-containing layer to the inner wall of the container blank.
  • the silicon nitride powder-containing layer is then burned ein ⁇ by a baking process in the inner wall of the container blank.
  • the baked-on layer acts as a non-stick coating for a silicon melt, which is not decomposed even at the high temperatures of the silicon melt.
  • the coating produced in this way offers a considerably higher resistance to caking and sticking between the solidified silicon and the container inner wall and has a substantially lower contamination of the crystallized block surface of the silicon with the coating.
  • molds designed as containers are used, which essentially have the shape of an upwardly open cuboid and a cuboidal interior limit five pages, that is not upwards.
  • round molds are used.
  • such containers are referred to as molds and container blanks as mold blanks.
  • the ingot blank is a green compact which is produced either by compression of silicon dioxide powder or by shaping and subsequent drying of sludge containing silicon dioxide powder.
  • a layer containing silicon nitride powder is subsequently applied to the inner wall of the green body.
  • the silicon nitride powder is preferably dispersed in a solvent with or without an organic or inorganic dispersant and / or an adhesion promoter.
  • the silicon nitride powder can be applied to the inner wall of the green body in dispersed or powdered state, for example by brushing, spraying, spraying, dipping or by electrostatic application as suspension, slip or powder. If required, several layers can be applied one after the other.
  • the layers of silicon nitride powder have a silicon dioxide content of ⁇ 70 wt .-%, in particular ⁇ 60 wt .-%, in particular ⁇ 45 wt .-%, an alkali and alkaline earth metal content of ⁇ 3000 ppm, in particular ⁇ 1000 ppm, a fluoride content of ⁇ 3000 ppm, in particular ⁇ 2000 ppm, a chloride content of ⁇ 3000 ppm, in particular
  • the layers of silicon nitride powder have an oxygen content of from 0.1% by weight to 10% by weight, in particular from 0.3% by weight to 5% by weight, in particular from 1% by weight to 3% by weight .-% on.
  • the ratio of length to diameter of the particles of the silicon nitride powder is less than 10.
  • the mean particle size of the silicon nitride powder is ⁇ 100 .mu.m, in particular ⁇ 50 .mu.m, in particular ⁇ 30 .mu.m.
  • the silicon nitride powder contains, in addition to other phases of the silicon nitride, 1% to 100%, in particular 1% to 5%, in the beta phase.
  • the silicon nitride powder may be amorphous.
  • the green compact is heat-treated, in particular sintered, with the layers burning into the inner wall of the green compact.
  • the baking of the layers into the inner wall and the burning of the green body preferably takes place simultaneously. Alternatively, separate method steps may be provided.
  • the baking is preferably carried out by means of a heating of the green body by an incoherent radiation and / or by convection.
  • the firing takes place in a furnace provided for this purpose, in particular in a tunnel kiln customary in the ceramics industry. Such burn-in is inexpensive compared to burn-in with laser radiation.
  • a stable silicon nitride layer is present as a non-stick coating on the inner wall of the finished mold.
  • the sintering process is preferably carried out at 1100 0 C and leads to a compaction and curing of the green compact.
  • the particles of the silicon dioxide powder of the green compact and of the silicon nitride powder applied thereto form fusions, so that the resulting non-stick coating is firmly bonded to the inner wall of the mold.
  • the particles of the silicon dioxide powder also form enamel with one another, as a result of which the sintered green body acquires its strength.
  • the non-stick-coated mold resulting from the firing process is particularly suitable for receiving liquid silicon and for crystallizing liquid silicon into silicon blocks, rods, billets or granules.
  • the non-stick coating according to the invention offers better resistance to caking and sticking than known methods.
  • the generated silicon can be used to produce silicon wafers.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Ceramic Products (AREA)

Abstract

La présente invention concerne un procédé pour réaliser un récipient destiné à la fusion et/ou à la cristallisation de métaux non ferreux, comprenant les étapes suivantes: mise à disposition d'une ébauche de récipient présentant une paroi interne et une paroi externe; application d'au moins une couche contenant une poudre de nitrure de silicium, au moins sur la paroi interne de l'ébauche de récipient; cuisson de la/des couche(s) dans l'ébauche de récipient. Le revêtement anti-adhésif résultant de la cuisson, a une résistance améliorée à l'adhérence ou à la conglutination lors du captage de silicium liquide ou de la cristallisation de silicium liquide.
PCT/EP2005/006675 2004-07-08 2005-06-21 Procede pour realiser une coquille presentant un revetement anti-adhesif WO2006005416A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004033249.5 2004-07-08
DE102004033249 2004-07-08

Publications (1)

Publication Number Publication Date
WO2006005416A1 true WO2006005416A1 (fr) 2006-01-19

Family

ID=34972092

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2005/006675 WO2006005416A1 (fr) 2004-07-08 2005-06-21 Procede pour realiser une coquille presentant un revetement anti-adhesif

Country Status (1)

Country Link
WO (1) WO2006005416A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006003819A1 (de) * 2006-01-26 2007-08-02 Wacker Chemie Ag Keramischer Formkörper mit hochreiner Si3N4-Beschichtung, Verfahren zu seiner Herstellung und Verwendung
DE102008031766A1 (de) * 2008-07-04 2009-10-15 Schott Ag Verfahren zur Herstellung eines beschichteten Tiegels aus einem Tiegelgrünkörper oder aus einem zwischengebrannten Tiegelkörper sowie die Verwendung solch eines beschichteten Tiegels
CN101845666A (zh) * 2010-06-03 2010-09-29 王敬 一种掺氮晶体硅及其制备方法
US8048221B2 (en) 2006-01-20 2011-11-01 Stoddard Nathan G Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0963464A1 (fr) * 1997-02-06 1999-12-15 Bayer Ag Creuset muni de couches de protection en silicium, procede d'application la couche de protection en silicium et utilisation
US20020083886A1 (en) * 2000-12-01 2002-07-04 Nobuyuki Katoh Cruicible and growth method for polycrystal silicon using same
US20020146510A1 (en) * 2000-11-15 2002-10-10 Costantini Michael A. Release coating system for crucibles
US20030104920A1 (en) * 2001-11-29 2003-06-05 Wacker-Chemie Gmbh SiO2 shaped body which is vitrified in partial regions or completely, process for its production and use
DE10217647A1 (de) * 2002-04-19 2003-11-06 Scanwafer Gmbh Verfahren zur Herstellung von Schmelztiegeln für Silizium
WO2004053207A1 (fr) * 2002-12-06 2004-06-24 Vesuvius France S.A. Recipient destine a conserver du silicium et son procede de production
WO2005026067A1 (fr) * 2003-09-11 2005-03-24 Wacker Chemie Ag Procede de production d'un corps moule en sio2 recouvert de si3n4

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0963464A1 (fr) * 1997-02-06 1999-12-15 Bayer Ag Creuset muni de couches de protection en silicium, procede d'application la couche de protection en silicium et utilisation
US20020146510A1 (en) * 2000-11-15 2002-10-10 Costantini Michael A. Release coating system for crucibles
US20020083886A1 (en) * 2000-12-01 2002-07-04 Nobuyuki Katoh Cruicible and growth method for polycrystal silicon using same
US20030104920A1 (en) * 2001-11-29 2003-06-05 Wacker-Chemie Gmbh SiO2 shaped body which is vitrified in partial regions or completely, process for its production and use
DE10217647A1 (de) * 2002-04-19 2003-11-06 Scanwafer Gmbh Verfahren zur Herstellung von Schmelztiegeln für Silizium
WO2004053207A1 (fr) * 2002-12-06 2004-06-24 Vesuvius France S.A. Recipient destine a conserver du silicium et son procede de production
WO2005026067A1 (fr) * 2003-09-11 2005-03-24 Wacker Chemie Ag Procede de production d'un corps moule en sio2 recouvert de si3n4

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
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 *
PRAKASH P ET AL: "USE OF SILICON OXYNITRIDE AS A GRAPHITE MOLD RELEASING COATING FOR THE GROWTH OF SHAPED MULTICRYSTALLINE SILICON CRYSTALS", JOURNAL OF CRYSTAL GROWTH, NORTH-HOLLAND, AMSTERDAM, NL, vol. 144, no. 1/2, 1 November 1994 (1994-11-01), pages 41 - 47, XP000484426, ISSN: 0022-0248 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8048221B2 (en) 2006-01-20 2011-11-01 Stoddard Nathan G Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics
US8628614B2 (en) 2006-01-20 2014-01-14 Amg Idealcast Solar Corporation Methods and apparatus for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics
US8951344B2 (en) 2006-01-20 2015-02-10 Amg Idealcast Solar Corporation Methods and apparatuses for manufacturing geometric multicrystalline cast silicon and geometric multicrystalline cast silicon bodies for photovoltaics
DE102006003819A1 (de) * 2006-01-26 2007-08-02 Wacker Chemie Ag Keramischer Formkörper mit hochreiner Si3N4-Beschichtung, Verfahren zu seiner Herstellung und Verwendung
DE102008031766A1 (de) * 2008-07-04 2009-10-15 Schott Ag Verfahren zur Herstellung eines beschichteten Tiegels aus einem Tiegelgrünkörper oder aus einem zwischengebrannten Tiegelkörper sowie die Verwendung solch eines beschichteten Tiegels
CN101845666A (zh) * 2010-06-03 2010-09-29 王敬 一种掺氮晶体硅及其制备方法

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