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WO2004111315A1 - Procede de production d'un composant en verre de quartz presentant une grande stabilite thermique - Google Patents

Procede de production d'un composant en verre de quartz presentant une grande stabilite thermique Download PDF

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Publication number
WO2004111315A1
WO2004111315A1 PCT/EP2004/006105 EP2004006105W WO2004111315A1 WO 2004111315 A1 WO2004111315 A1 WO 2004111315A1 EP 2004006105 W EP2004006105 W EP 2004006105W WO 2004111315 A1 WO2004111315 A1 WO 2004111315A1
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WO
WIPO (PCT)
Prior art keywords
layer
quartz glass
sol
compound
crystallization promoter
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.)
Ceased
Application number
PCT/EP2004/006105
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German (de)
English (en)
Inventor
Günther Heinz FRISCHAT
Kirsten Wilm
Martin Arndt
Gabriele Korus
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.)
Heraeus Quarzglas GmbH and Co KG
Original Assignee
Heraeus Quarzglas GmbH and Co KG
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 Heraeus Quarzglas GmbH and Co KG filed Critical Heraeus Quarzglas GmbH and Co KG
Publication of WO2004111315A1 publication Critical patent/WO2004111315A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
    • C03C1/008—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or coatings
    • 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
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • 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
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • 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
    • C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • 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
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/30—Doped silica-based glasses containing metals
    • C03C2201/54—Doped silica-based glasses containing metals containing beryllium, magnesium or alkaline earth metals
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/26—Wet processes, e.g. sol-gel process using alkoxides
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/26—Wet processes, e.g. sol-gel process using alkoxides
    • C03C2203/27—Wet processes, e.g. sol-gel process using alkoxides the alkoxides containing other organic groups, e.g. alkyl groups
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/30—Additives

Definitions

  • the invention relates to a method for producing a quartz glass component with high thermal stability, in particular a quartz glass crucible for use in a crystal pulling process, by providing a base body, the surface of which is at least partially provided with a layer which contains a crystallization promoter ion in a silicate compound and from which a cristobalite formation arises when heated when the quartz glass component is used as intended.
  • Quartz glass crucibles are used, for example, to absorb the molten metal when pulling single crystals using the so-called Czochralski method.
  • a seed crystal with a given orientation is immersed in the melt and then slowly pulled up.
  • the seed crystal and the melt rotate in opposite directions.
  • the surface tension between the seed crystal and the melt means that the seed crystal is also used to pull off the melt, which gradually cools down and thereby solidifies into a single crystal which grows continuously.
  • the temperature stability of quartz glass is a limiting factor. In the literature, temperature values around 1150 ° C. are given as the lower softening point for quartz glass. However, the required process temperatures are often above this temperature, so that viscous deformation of the quartz glass crucible can occur.
  • the melting temperature when pulling a single crystal from a silicon melt is, for example, around 1480 ° C. It has therefore been proposed to increase the thermal stability of quartz glass components by providing them with a surface layer made of cristobalite.
  • the melting point of cristobalite is around 1720 0 C.
  • Such a quartz glass crucible and a generic method for its production are known from EP 0 748 885 A1.
  • the glassy outer wall of a commercial crucible made of opaque, bubble-containing quartz glass is covered with a treated chemical solution, which contains substances which, when the crucible is used as a nucleating agent, can cause devitrification from quartz glass to cristobalite.
  • the surface treated in this way therefore crystallizes out with the formation of cristobalite.
  • This crystallization of the outer wall leads to a higher mechanical and thermal strength of the quartz glass crucible.
  • this surface layer is also referred to as a “stabilization layer” and the nucleating agents as “crystallization promoters”.
  • crystal promoter ions alkaline earths, boron, and phosphorus are proposed, which are applied to the crucible surface as oxides, hydroxides, carbonates, silicates, etc.
  • silicate compounds it should be noted that these are generally present as solids with a low solubility in aqueous solutions, so that uniform coating of the crucible surface with such silicate compounds is problematic.
  • An inhomogeneous distribution of the crystallization promoter on the crucible surface leads to an uneven crystal growth and with it an uneven stabilization layer.
  • barium hydroxide is therefore preferably used, which can be applied uniformly to the crucible surface in the form of an aqueous solution containing barium hydroxide.
  • barium hydroxide tends to react with the carbon dioxide present to form barium carbonate. This makes it difficult to weigh this substance exactly and thus the reproducibility of the process.
  • the crystallization promoter can be rubbed off during transport or before using the quartz glass crucible. It is therefore usually not possible to predict whether the crystallization will occur in the desired manner.
  • the barium carbonate contained in the surface layer decomposes when heated, releasing carbon dioxide, which can impair the drawing process.
  • Powder layer tends to flake off and if the fusion is too strong, the stabilizing effect of the cristobalite powder is lost due to the conversion to the amorphous phase.
  • spraying on the cristobalite powder has the disadvantage that, with thin stabilizing layers, an uneven distribution of solids is easily obtained on the quartz glass surface, while thick crystalline layers easily flake off when heated.
  • a graphite crucible (a so-called “pBN crucible”) is provided with a layer of a boron oxide-containing SiO 2 in order to improve the wetting properties of the crucible surface with respect to the GaAs semiconductor melt contained therein.
  • the pBN crucible is immersed one or more times in an alcoholic sol solution containing Si (OC 2 Hs) and B (OCH 3 ), and the SoI-FiIm adhering to the surface is then heated, causing condensation a 2 mm thick
  • the object of the invention is to provide a simple and inexpensive method by means of which a stabilizing layer can be reproducibly produced on a quartz glass component, in particular on a quartz glass crucible.
  • this object is achieved according to the invention in that, by hydrolysis of a solution containing the crystallization promoter ion and a hydrolyzable silicon compound, a sol is formed in which colloidal particles of the hydrolyzed silicon compound and the crystallization promoter ion are present, that the sol is applied to the base body to form the layer, and that silicate formation in the layer then takes place by condensation of the hydrolyzed silicon compound with crosslinking of the colloidal particles.
  • the sol-gel method is used to produce a silicate-like layer which contains the crystallization promoter ion and from which a stabilization layer is formed in the sense of the present invention.
  • Liquid starting substances are used as the starting point, in particular a hydrolyzable organic silicon compound is used. Suitable compounds of this type are well known to the person skilled in the art. The greatest technical importance is given to alkoxy compounds, predominantly silicon alkoxides generally designated as silanes, with the structural formula:
  • OR stands for hydrolyzable groups which are split off as alcohols during the reaction. It is also known to use organically modified alkoxides, for example organosilanes with one or more organic groups instead of alkoxy groups:
  • R1 stands for: alkyl radical, aryl radical or a functional group (e.g. epoxy, methacrylic radical)
  • the silane compounds are hydrolyzed, i.e. H. reacted with water in the presence of catalysts according to the following reaction equation.
  • the hydrolysis leads to a sol in which the hydrolyzed silicon compounds are present as colloidal particles.
  • the sol generally forms a low-viscosity, colorless liquid in which unreacted reactive monomeric silanes and silanols are present, as well as oligomers in the form of polysiloxanes which have already formed to a small extent at room temperature and which form precursors for a later crosslinking reaction.
  • the polysiloxanes in the SoI have a size of a few nanometers.
  • the sol in this colloidally dispersed state is used according to the invention for coating the base body.
  • the sol is converted to polysiloxanes (gel), which can be described using the following reaction equations.
  • condensation starts at room temperature or requires the supply of thermal energy.
  • the associated crosslinking reaction and thus the hardening of the layer produced - generally takes place by baking at higher temperatures and, depending on the starting materials used and the temperature, takes from a few minutes to a few hours. This creates inorganic polymer structures with a silicate, glass-like structure.
  • the crystallization promoter ion and the hydrolyzable silicon compound are contained in soluble form in the sol used to form the layer.
  • the liquid sol is applied to the surface to be coated, which enables a particularly uniform coating of the surface with the crystallization promoter ion - also at the molecular level. Such a homogeneous coating ensures a uniform crystallization P2004 / 006105
  • the sol-gel method also enables the production of layers with dry layer thicknesses in the millimeter range, if there is a risk of flaking or flaking, by adjusting the viscosity of the SoI or by repeatedly applying the SoIs is reduced during transport or use of the component.
  • the stabilizing layer also acts as a diffusion due to its three-dimensional design. on lock for the migration of impurities from the crucible base body in the direction of the melt contained in the quartz glass crucible.
  • Crystallization of the layer during the manufacture of the quartz glass component is avoided as far as possible.
  • a surface layer that has crystallized once induces mechanical stresses when the component cools due to the differences in the thermal expansion of quartz glass and cristobalite, which can lead to cracks or even breakage.
  • the component does not show any crystallization after it has been produced, but at most crystal nuclei in the area of the layer. Only when the quartz glass component is used as intended does cristobalite form with the formation of the stabilization layer.
  • the SoI is applied to the base body surface using customary methods such as spraying, electrostatically assisted spraying, dipping, flooding or spinning.
  • crystallization promoter ion is used in the form of a water-soluble and pH-neutral compound.
  • the pH value plays an important role in the sol-gel process. Changes in the pH, for example by adding the crystallization promoter ion in an acidic or in an alkaline compound such as the barium hydroxide proposed in the prior art, can impair the quality of the layer.
  • the addition of a crystallization promoter ion in the form of a pH-neutral compound does not significantly change the pH of the SoI, regardless of its concentration.
  • the crystallization promoter ion in the sol is not present as a solid, for example in the form of a silicate, but in the form of a water-soluble compound.
  • Perchlorate compounds of this type are generally water-soluble and pH-neutral and therefore show the advantages mentioned above with regard to a homogeneous distribution of the crystallization promoter and little impairment of the sol-gel process.
  • the crystallization promoter ion is preferably in the form of a barium compound.
  • Barium compounds are known to promote crystallization in quartz glass.
  • barium is characterized by a relatively low solubility coefficient in silicon.
  • the concentration of the crystallization promoter must always be set so that the desired cristobalite formation starts when the quartz glass crucible is heated to a temperature above 1400 ° C.
  • the concentration of barium is 33 mol% (based on the total molar number of silicon and barium in the layer).
  • the SoI is preferably applied to the base body surface by spraying.
  • the viscosity of the SoI when sprayed is in the range between 1 and 35 mPas, preferably in the range between 15 and 25 mPas.
  • the viscosity of the SoI in this range is a suitable compromise between a low viscosity, which makes application by spraying easier, and a high viscosity, which promotes the adhesion of the layer and, if necessary, the formation of a thick sol layer.
  • the condensation of the sol layer takes place by heating the layer to a temperature in the range between 300 ° C. and 700 ° C., preferably between 400 ° C. and 600 ° C.
  • the heating causes the layer to solidify, which contributes to a stable embedding of the crystallization promoter ion in a silicate, glass-like network.
  • the heating time ranges from a few minutes to about two hours.
  • the layer advantageously has a layer thickness in the range between 50 nm and 500 nm, preferably between 75 nm and 200 nm.
  • a stabilizing layer with a thickness in this area is characterized by a comparatively good mechanical stability, which prevents flaking or flaking when the quartz glass component is used as intended.
  • the layer is advantageously successively strengthened by repeatedly carrying out the method according to the invention.
  • Each application of a sol layer is preceded by condensation and thermal solidification of the layer underneath.
  • FIG. 1 shows a section through the wall of a quartz glass crucible with a surface layer produced according to the invention
  • 2 shows a section of a cross section through the wall of a quartz glass tube with a stabilizing layer
  • FIG. 3 shows a device suitable for carrying out the method according to the invention.
  • the reference number 1 is assigned to a crucible overall.
  • the crucible 1 consists of a raw form 2 made of opaque quartz glass, the inner wall of which is provided in the side area with a glassy, dense and crack-free surface layer made of barium-doped SiO 2 (hereinafter referred to as “barium disilicate layer”).
  • the barium disilicate layer 3 has an average thickness of about 100 nm.
  • a crude form of the quartz glass crucible is produced by filling grain from natural quartz into a metallic melting mold rotating about its central axis and forming a uniformly thick layer of quartz grains on the inside of the melting mold by means of a screw-on template. This is stabilized due to centrifugal forces on the inner wall of the melting mold and melted under continuous rotation by means of an arc, which is lowered into the melting mold from above.
  • the quartz grain layer melts to form the raw form 2 shown in FIG. 1 and a smooth inner wall of dense quartz glass is formed. Adhesive quartz grains are removed from the outer wall of the raw mold 2 thus produced and then ground.
  • the barium disilicate layer 3 is produced on the smooth inner wall of the raw form by means of the sol-gel method.
  • TEOS tetraethyl orthosilicate
  • hydrolyzable silicon compound For The following components and quantities are used to prepare a basic solution from the SoI:
  • the base solution can be diluted.
  • a comparatively thin-bodied sol is required for the spray coating used here, so that the base solution is diluted to a total mass of 40 g with methanol.
  • the SoI can then also be applied to the outer wall of the crucible raw form.
  • the crucible 1 is mounted on a holding device which can be rotated about an axis of rotation, as will be explained in more detail below with reference to FIG. 3. While rotating the crucible 1 around its central axis, the liquid sol is sprayed onto the outer wall by means of a spray nozzle. The spraying process ends as soon as the surface is evenly coated.
  • the SoI dries very quickly, the layer thickness of the SoI layer produced in this way is approximately 100 nm.
  • the crucible coated in this way is introduced into a drying oven preheated to 60 ° C. within 3 minutes and then heated to a temperature of around 500 ° C. while gradually condensing and crosslinking the TEOS and at the same time thermally solidified.
  • the barium disilicate layer 3 produced in this way has a glass-like structure and an average thickness of approximately 100 nm.
  • the quartz glass tube 4 according to FIG. 2 has a base layer 5 of opaque quartz glass which surrounds the inner bore and is surrounded by a first barium disilicate layer 6 and this is surrounded by a second barium disilicate layer 7.
  • the two barium disilicate layers 6; 7 together have a thickness of 200 nm.
  • crystalline grains made of natural quartz with a grain size of 90 to 315 ⁇ m are cleaned by hot chlorination and filled into a tubular metal mold that rotates about their longitudinal axis.
  • a rotationally symmetrical hollow cylinder is formed from the bed on the inner wall of the metal mold.
  • the hollow cylinder has a layer thickness of approximately 100 mm in the bed and an inner bore in the form of a through bore with an inner diameter of approximately 180 mm.
  • the bed is slightly solidified by the centrifugal force before the subsequent process steps are carried out.
  • the mechanically precompressed hollow cylinder is melted zone by zone from the inner bore by means of an arc.
  • a pair of electrodes is inserted into the inner bore from one end of the hollow cylinder and continuously moved towards the opposite end of the hollow cylinder.
  • the grain is melted by the temperature of the arc.
  • a maximum temperature of over 2100 ° C. is reached on the inner wall of the hollow cylinder. This creates a melting front that progresses outwards in the direction of the metal mold. The melting process ends before the melting front reaches the metal mold.
  • the tube made of opaque quartz glass is removed from the metal mold, ground and then etched in hydrofluoric acid and elongated in a hot forming step while reducing the wall thickness. After elongation, the outside diameter is 245 mm and the inside diameter is 233 mm. The outer surface is blasted with frozen CO 2 pellets, creating a fine surface roughness.
  • this tube forms the base layer 5 made of opaque quartz glass. Especially with such The stabilizing layer has a particularly advantageous effect on thin-walled tubes as in this exemplary embodiment.
  • a sol the manufacture of which is described above with reference to Example 1 (crucible) is sprayed onto the outer wall of the tube pretreated in this way.
  • the layer produced in this way is dried and solidified to form the first barium disilicate layer 6, as described with reference to Example 1.
  • the outer, second barium disilicate layer 7 is sprayed onto the first barium disilicate layer 6 using the same coating method and then solidified.
  • Crystallization of the quartz glass starts from the two barium disilicate layers 6 and 7 when the tube is heated to a temperature above 1400 ° C., with the formation of a homogeneous stabilizing layer containing cristobalite, which contributes to a high mechanical and thermal stability of the tube.
  • FIG. 3 schematically shows a device which is suitable for applying a sol layer on the outer wall of a quartz glass crucible 31.
  • the quartz glass crucible 31 is mounted on a clamping device 33 which can be rotated about its central axis 32.
  • a spray nozzle 34 is fixed to a holder 35 which is movable in the horizontal and in the vertical direction.
  • the spray nozzle 34 can be tilted so that it can reach any position of the outer wall of the crucible.
  • Liquid sol solution is supplied to the spray nozzle 34 by means of a liquid pump via a supply line.
  • sol solution is applied to the outer wall of the quartz glass crucible 31.
  • sol layers of a predetermined thickness and from different starting materials can be produced without great effort.

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Dispersion Chemistry (AREA)
  • Composite Materials (AREA)
  • Ceramic Engineering (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

Un procédé connu de production d'un composant en verre de quartz présentant une stabilité élevée comprend la préparation d'un corps de base, dont la surface est pourvue, au moins partiellement, d'une couche qui contient un ion promoteur de cristallisation dans un composé de silicate, une formation de cristobalite se faisant à partir de la couche sous l'effet du réchauffement lors de l'utilisation conforme aux prescriptions du composant en verre de quartz. Pour que ce procédé soit amélioré en ce qui concerne sa reproductibilité et sa rentabilité, il est proposé, selon l'invention, qu'un sol soit formé par hydrolyse d'une solution contenant l'ion promoteur de cristallisation et un composant de silicium hydrolysable, sol dans lequel se trouve des particules colloïdales du composé de silicium hydrolysé et de l'ion promoteur de cristallisation, que ce sol soit déposé sur la surface du corps de base en formant une couche et qu'ensuite, sous l'effet de la condensation du composé de silicium hydrolysé, avec réticulation des particules colloïdales, du silicate se forme dans ladite couche.
PCT/EP2004/006105 2003-06-17 2004-06-07 Procede de production d'un composant en verre de quartz presentant une grande stabilite thermique Ceased WO2004111315A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2003127496 DE10327496A1 (de) 2003-06-17 2003-06-17 Verfahren zur Herstellung eines Quarzglasbauteils mit hoher thermischer Stabilität
DE10327496.0 2003-06-17

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WO2004111315A1 true WO2004111315A1 (fr) 2004-12-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113213970A (zh) * 2021-04-20 2021-08-06 广东先导微电子科技有限公司 一种pbn坩埚氧化硼润湿装置、方法及其应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015009423B4 (de) 2015-07-20 2024-05-16 Qsil Gmbh Quarzschmelze Ilmenau Formstabile Silikatglaskeramik

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001046077A1 (fr) * 1999-12-22 2001-06-28 Heraeus Quarzglas Gmbh & Co. Kg Creuset en verre de quartz et son procede de fabrication
US20010032580A1 (en) * 1999-03-15 2001-10-25 Phillips Richard J. Barium doping of molten silicon for use in crystal growing process
US20030012899A1 (en) * 2001-07-16 2003-01-16 Heraeus Shin-Etsu America Doped silica glass crucible for making a silicon ingot
US20030094131A1 (en) * 2001-10-16 2003-05-22 Japan Super Quartz Corporation Surface modification process of quartz glass crucible
US20030183161A1 (en) * 2002-03-29 2003-10-02 Japan Super Quartz Corporation Surface modified quartz glass crucible and its modification process

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5976247A (en) * 1995-06-14 1999-11-02 Memc Electronic Materials, Inc. Surface-treated crucibles for improved zero dislocation performance
JP4288646B2 (ja) * 2001-10-16 2009-07-01 ジャパンスーパークォーツ株式会社 石英ガラスルツボの表面改質方法と表面改質ルツボ

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010032580A1 (en) * 1999-03-15 2001-10-25 Phillips Richard J. Barium doping of molten silicon for use in crystal growing process
WO2001046077A1 (fr) * 1999-12-22 2001-06-28 Heraeus Quarzglas Gmbh & Co. Kg Creuset en verre de quartz et son procede de fabrication
US20030012899A1 (en) * 2001-07-16 2003-01-16 Heraeus Shin-Etsu America Doped silica glass crucible for making a silicon ingot
US20030094131A1 (en) * 2001-10-16 2003-05-22 Japan Super Quartz Corporation Surface modification process of quartz glass crucible
US20030183161A1 (en) * 2002-03-29 2003-10-02 Japan Super Quartz Corporation Surface modified quartz glass crucible and its modification process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113213970A (zh) * 2021-04-20 2021-08-06 广东先导微电子科技有限公司 一种pbn坩埚氧化硼润湿装置、方法及其应用

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