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WO2002016677A1 - Creuset en verre de quartz et procede de fabrication dudit creuset - Google Patents

Creuset en verre de quartz et procede de fabrication dudit creuset Download PDF

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Publication number
WO2002016677A1
WO2002016677A1 PCT/EP2001/008981 EP0108981W WO0216677A1 WO 2002016677 A1 WO2002016677 A1 WO 2002016677A1 EP 0108981 W EP0108981 W EP 0108981W WO 0216677 A1 WO0216677 A1 WO 0216677A1
Authority
WO
WIPO (PCT)
Prior art keywords
quartz glass
crucible
layer
crystallization
intermediate layer
Prior art date
Application number
PCT/EP2001/008981
Other languages
German (de)
English (en)
Inventor
Heinz Fabian
Johann Leist
Waltraud Werdecker
Original Assignee
Heraeus Quarzglas Gmbh & Co. Kg
Shin-Etsu Quartz Products Co., Ltd.
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 & Co. Kg, Shin-Etsu Quartz Products Co., Ltd. filed Critical Heraeus Quarzglas Gmbh & Co. Kg
Publication of WO2002016677A1 publication Critical patent/WO2002016677A1/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
    • 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
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles

Definitions

  • the invention relates to a quartz glass crucible, with a crucible wall, in which at least one SiO 2 intermediate layer containing a dopant is enclosed.
  • the invention further relates to a method for producing a quartz glass crucible by providing a crucible with a crucible wall made of quartz glass, in which at least one SiO 2 intermediate layer containing a dopant is enclosed.
  • Such a quartz glass crucible and a method for its production are known from DE-A-19710672.
  • An intermediate layer is then produced on the outer layer thus produced by dusting a second SiO 2 powder which either contains aluminum or is combined with an aluminum-containing component while the metal mold is rotating.
  • This aluminum-containing SiO 2 powder is deposited on the outer layer to form the intermediate layer.
  • an inner layer is formed on the intermediate layer by again scattering SiO 2 powder into the rotating metal mold and melting it as a transparent inner layer by means of an arc.
  • the inner layer then completely covers the intermediate layer.
  • the aluminum-containing intermediate layer serves as a diffusion barrier by preventing the migration of contaminants into the silicon melt.
  • EP-A 748 885 discloses a quartz glass crucible and a method for the same Manufacture known in which the inner or the outer wall of a commercially available quartz glass crucible is treated with a chemical solution which contains substances which, acting as nucleating agents, can promote the devitrification of quartz glass to cristobalite. Alkaline earth, boron and phosphorus compounds are proposed as substances that promote crystallization. Is preferred
  • the damage is particularly high in the case of rejects.
  • special measures are required when coating the outer wall of the crucible in order to avoid damage to the coating, for example during transport or when using the crucible.
  • the alkaline earth, boron and phosphorus compounds used as crystallization-promoting substances can get into the silicon melt and contaminate it.
  • the invention has for its object to provide a quartz glass crucible with high thermal stability, which releases little impurities to the melt contained therein and which is easy to handle, and to provide a simple and inexpensive method for producing such a quartz glass crucible.
  • the dopant contains at least one crystallization aid in a type and amount such that this causes cristobalite to form when the quartz glass crucible is heated to at least 1400.degree.
  • the quartz glass crucible is opened when used for pulling semiconductor crystals a temperature above the melting temperature of the respective semiconductor material is heated (1425 ° C. for silicon).
  • An essential aspect of the invention is to provide a quartz glass crucible for this purpose, which has an intermediate layer within the crucible wall, from which a crystallization of the quartz glass to cristobalite is intentionally caused during this use.
  • at least one crystallization promoting agent is introduced into the crucible wall in the area of the intermediate layer in a type and amount that is suitable for causing the crystallization of quartz glass to cristobalite at high temperatures.
  • Crystallization during the production of the quartz glass crucible is kept low or avoided entirely, with the onset of germ formation being beneficial with regard to the subsequent crystallization.
  • a once crystallized intermediate layer induces mechanical stresses when the quartz glass crucible cools due to the differences in the thermal expansion of quartz and cristobalite, which can lead to cracks or even breakage of the crucible.
  • the quartz glass crucible shows no crystallization after its production, but only crystal nuclei in the area of the intermediate layer. Only when the quartz glass crucible is used as intended does a crystallized zone form in the area of the intermediate layer, which then has several functions:
  • the crystallized intermediate layer contributes to the mechanical and thermal stabilization of the quartz glass crucible and extends its service life.
  • the intermediate layer becomes increasingly opaque in the course of crystallization, it contributes to a homogenization of the temperature field when using the quartz glass crucible.
  • the onset of crystallization in the area of the intermediate layer depends on the type of crystallization aid and its concentration in the area of the intermediate layer.
  • the required minimum concentration for a specific crystallization aid can be easily determined with just a few tests.
  • crystallization aid or the crystallization aid in the are included intermediate layer, they can not come into contact with the melt, so that contamination of the melt is excluded.
  • the crystallization aid preferably contains an aluminum compound.
  • aluminum not only promotes the formation of cristobalite in quartz glass, it also binds lithium-containing impurities and acts as a so-called "getter” for lithium ions.
  • aluminum diffuses only slowly in quartz glass and is therefore compared to others
  • Crystallization aids - which contain, for example, barium - are less critical for applications where high purity is important.
  • Aluminum nitrate is a commercially available substance and is inexpensively available in high purity; it is non-toxic and can be applied homogeneously in liquid form. In particular, aluminum nitrate effects a uniform and reproducible crystallization in quartz glass without the risk of contamination of the melt contained in the quartz glass crucible.
  • Crystallization with particularly fine particles being beneficial for this purpose. Since it is a "species-specific" substance (to quartz glass), contamination of the melt is excluded.
  • the crucible wall has an outer layer made of opaque quartz glass, which is at least partially provided with an inner layer made of transparent quartz glass, the intermediate layer being arranged in the region of the outer layer. Due to the different expansion coefficients of the cristobalite phase and the quartz glass of the crucible, cracks can occur during the manufacturing process for the quartz glass crucible, especially when cooling. Therefore, during the manufacture of the Quartz glass crucible strives for little or no cristobalite formation in the intermediate layer in order to avoid the development of stresses during cooling. In the preferred embodiment, this is achieved in that the crystallization conveyor is introduced into the outer region of the crucible wall, that is to say into the outer layer.
  • the outer region of the crucible wall is only exposed to high temperatures in the last phase, so that cristobalite formation does not start there or only begins late.
  • the intermediate layer is therefore preferably arranged in an outer region of the crucible wall, in which the crystallization aid contained therein is built into the quartz glass matrix sufficiently firmly during the melting process of the quartz glass crucible, but has not yet or only insignificantly started to form cristobalite.
  • the intermediate layer between the outer layer and the inner layer in a quartz glass crucible with a crucible wall which has an outer layer made of opaque quartz glass and which is at least partially provided with an inner layer made of transparent quartz glass.
  • the above-mentioned object is achieved according to the invention based on the method described at the outset in that the dopant contains at least one crystallization promoting agent in a type and amount such that cristobalite is formed when the quartz glass crucible is heated to at least 1400.degree.
  • the quartz glass crucible when pulling semiconductor crystals, the quartz glass crucible is heated to a temperature above the melting temperature of the respective semiconductor material. In the case of silicon, this is 1425 ° C.
  • a quartz glass crucible is provided which has an area within the crucible wall from which a crystallization of the quartz glass into cristobalite is deliberately caused during its intended use.
  • At least one intermediate layer containing a dopant is enclosed in the crucible wall in the manufacture of the quartz glass crucible, into which at least one crystallization promoting agent is introduced, which causes the type and amount of crystallization of quartz glass to cristobalite at high temperatures (T> 1400 ° C.).
  • Crystallization during the manufacture of the quartz glass crucible itself is, however, avoided or kept as low as possible and limited to the onset of nucleation. The reasons for this have already been discussed above. Only when the quartz glass crucible is used as intended, does the crystallized zone form completely in the area of the intermediate layer.
  • the crystallized intermediate layer then has several functions:
  • the intermediate layer becomes increasingly opaque in the course of crystallization, it contributes to a homogenization of the temperature field when using the quartz glass crucible.
  • the onset of crystallization in the area of the intermediate layer depends on the type of crystallization aid and its concentration in the area of the intermediate layer.
  • the minimum concentration required for a particular crystallization aid can be easily determined using a few tests. Damage to the intermediate layer, for example during transport or when filling the melt, is also excluded.
  • the crystallization aid is introduced into the intermediate layer during the production of the crucible. Subsequent and separate treatment of the otherwise finished quartz glass crucible - as in the method according to the prior art described at the outset - is not necessary.
  • the glazing of the crucible wall is usually carried out by means of a heating source arranged inside the crucible, so that the melting front moves from the inside to the outside when the crucible wall is glazed.
  • the intermediate layer is preferably arranged in an outer region of the crucible wall, the crystallization aid contained therein is built into the glass matrix sufficiently firmly during the vitrification, but cristobalite formation is kept low or completely avoided, with the onset of nucleation being conducive to later crystallization ,
  • quartz glass crucible with an outer layer of opaque quartz glass, which is at least partially provided with an inner layer made of transparent quartz glass, the intermediate layer being formed between the outer layer and the inner layer.
  • the application of the crystallization conveyor is particularly simple by applying a liquid containing the crystallization conveyor, which is preferably applied to the rotating wall of the crucible by spraying.
  • the liquid is expediently applied by ultrasonic atomization. This results in a particularly fine and homogeneous distribution of the crystallization aid.
  • the liquid is applied by means of a nozzle which can be moved along the wall of the crucible.
  • the crystallization aid is applied to the crucible wall in liquid form, as a result of which uniform wetting of the SiO 2 grains and thus homogeneous crystallization is achieved.
  • the mobility of the nozzle makes it easier to maintain an equal distance from the crucible wall and to generate a predetermined layer thickness of the crystallization conveyor.
  • FIG. 1 shows a method for producing a quartz glass crucible according to the invention using a device suitable for carrying out the method
  • FIG. 2 shows a longitudinal section through the wall of a quartz glass crucible according to the invention before its use
  • 3 shows a longitudinal section through the wall of the quartz glass crucible according to FIG. 2 after its intended use.
  • the device according to FIG. 1 comprises a metallic melt mold 1, which rests on a carrier 3 with an outer flange 2.
  • the carrier 3 can be rotated about the central axis 4 in any direction of rotation 5.
  • the spray nozzle 9 can be tilted, as indicated by the directional arrow 11, so that every location within the melting mold 1 can be reached by the spray nozzle 9.
  • a first process step several grain layers of natural quartz are produced on the inner wall of the melting mold 1; namely an outer layer 6 with a layer thickness of approximately 7 mm and an intermediate layer 7.
  • a second process step with continuous rotation of the melt mold 1, 9 aluminum nitrate solution is sprayed uniformly onto the intermediate layer 7 by means of the spray nozzle.
  • the spray position and the intensity of the spraying can be set as indicated above.
  • a thin, essentially closed surface film is formed on the intermediate layer 7, excess liquid evaporating immediately and aluminum nitrate remaining.
  • the thickness of this surface film results from the size of the wetted SiO 2 grains and the depth of penetration during surface wetting and is therefore at least half the grain thickness.
  • quartz grain is again sprinkled into the melting mold 1 and an inner layer 8 made of quartz grain with a layer thickness of 6 mm is produced on the intermediate layer 7.
  • the individual grain layers (6, 7, 8) are then melted to form the quartz glass crucible.
  • the aluminum nitrate locally causes nucleation in the area of the intermediate layer 7, which, when the quartz glass crucible is heated again to a temperature of 1400 ° C. or more, leads to crystallization of the quartz glass in this area, so that it forms a wholly or partially crystalline stabilizing layer comes.
  • Stabilizing layer is predetermined by the layer thicknesses of outer layer 6 and inner layer 8 during the production of the quartz glass crucible.
  • FIG. 2 A section through the wall of a further quartz glass crucible is shown schematically in FIG. 2 in a longitudinal section.
  • the local position of the intermediate layer 21 within the crucible wall can be seen from this.
  • the outer layer 20 contains a large number of bubbles and therefore has an opaque effect.
  • the thickness of the opaque outer layer 20 is in the range between approximately 5 mm to approximately 15 mm, depending on whether measurements are made in the bottom region of the crucible or in the side region.
  • the intermediate layer 21 is formed within the outer layer 20 in the sense of the present invention.
  • the intermediate layer 21 consists only of SiO 2 particles wetted with aluminum nitrate, the wetting extending approximately over a grain layer. For the sake of illustration, it is drawn in excessively thick in FIG.
  • the intermediate layer 21 runs — seen radially over the wall — approximately in the middle of the outer layer 20.
  • a smooth, transparent inner layer 22 made of high-purity SiO 2 which has a thickness of approximately 2.5 mm, is formed on the outer layer 20.
  • the inner layer 22 is characterized by high mechanical, thermal and chemical strength.
  • FIG 3 shows a schematic representation of the same section through the wall of the quartz glass crucible as Figure 2, but after the use of the quartz glass crucible when pulling a silicon single crystal according to the Czochralski method.
  • the crucible is heated to a temperature above 1400 ° C for several hours.
  • a crystallization zone 30 which extends in the crucible wall substantially radially to both sides of the intermediate layer 21.
  • the crystallization zone 30 fulfills several functions in the course of the use of the quartz glass crucible: it contributes to the mechanical and thermal stabilization of the quartz glass crucible and thus extends its service life; it acts as
  • Diffusion barrier for the migration of impurities from the outer layer in the direction of the melt contained in the quartz glass crucible and it homogenizes the temperature field after it has become increasingly opaque due to the crystal growth.
  • a uniformly thick quartz grain layer is first formed, as in the first exemplary embodiment, and an aluminum nitrate solution is sprayed uniformly thereon in a second method step with continued rotation of the melting mold by means of the movable spray nozzle.
  • quartz sand is again introduced into the melting mold and shaped into a thin grain layer using a template.
  • Aluminum nitrate solution is then sprayed again uniformly onto this grain layer to form a second, inner intermediate layer.
  • quartz grain is again sprinkled into the enamel mold and a further quartz grain layer is formed on the inner intermediate layer.
  • the intermediate layer here comprises two separate films with crystallization conveyors which are enclosed in the wall of the crucible and from which crystallization proceeds when the quartz glass crucible is used as intended and which thereby produce a common crystallized area.
  • a uniformly thick quartz grain layer is first formed, as in the first exemplary embodiment. Then, high-purity SiO 2 grain is sprinkled into the rotating melting mold, melted at the same time by means of an arc, and a first area of a transparent quartz glass layer with a layer thickness of approx. 2 mm is gradually built up.
  • An intermediate layer in the sense of the present invention is produced on the quartz glass layer by sprinkling a grain wetted with an aluminum-containing solution into the melting mold and, like the transparent quartz glass layer, being glazed directly.
  • a second region of a transparent one is finally applied to the intermediate layer produced in this way using the litter method described
  • Quartz glass layer made of undoped SiO 2 particles with a thickness of 2 mm.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

L'objet de la présente invention est d'améliorer la stabilité thermique et la maniabilité d'un creuset en verre de quart classique dont la paroi contient au moins une couche intermédiaire en SiO2 comportant une matière de dopage. A cet effet, ladite matière de dopage contient au moins un agent favorisant la cristallisation d'un type et en quantité tels qu'en cas de chauffe du creuset en verre de quartz à une température d'au moins 1400 °C, la matière de dopage entraîne une formation de cristobalite. La présente invention concerne également un procédé simple et peu onéreux de fabrication d'un creuset en verre de quartz selon la présente invention, selon lequel on utilise un creuset doté d'une paroi en verre de quartz dans laquelle est intégrée au moins une couche intermédiaire en SiO2 contenant une matière de dopage, ladite matière de dopage contenant au moins un agent favorisant la cristallisation d'un type et en quantité tels qu'en cas de chauffe du creuset en verre de quartz à une température d'au moins 1400 °C, la matière de dopage entraîne une formation de cristobalite.
PCT/EP2001/008981 2000-08-24 2001-08-02 Creuset en verre de quartz et procede de fabrication dudit creuset WO2002016677A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10041582.2 2000-08-24
DE2000141582 DE10041582B4 (de) 2000-08-24 2000-08-24 Quarzglastiegel sowie Verfahren zur Herstellung desselben

Publications (1)

Publication Number Publication Date
WO2002016677A1 true WO2002016677A1 (fr) 2002-02-28

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002070414A1 (fr) * 2001-03-08 2002-09-12 Heraeus Quarzglas Gmbh & Co. Kg Procede de fabrication d'un creuset en verre de quartz
EP1304399A1 (fr) * 2001-10-16 2003-04-23 Japan Super Quartz Corporation Procédé pour la modification d' une surface d'un creuset en verre de quartz
WO2003089693A1 (fr) * 2002-04-22 2003-10-30 Heraeus Quarzglas Gmbh & Co. Kg Creuset en verre de quartz et procede permettant de le produire
WO2003095384A1 (fr) * 2002-05-10 2003-11-20 General Electric Company Article de quartz fondu a devitrification maitrisee
US6755049B2 (en) 2001-03-08 2004-06-29 Heraeus Quarzglas Gmbh & Co. Kg Method of producing a quartz glass crucible
CN102482137A (zh) * 2009-10-14 2012-05-30 信越石英株式会社 二氧化硅粉、二氧化硅容器及该粉或容器的制造方法
EP2141131A3 (fr) * 2008-06-30 2013-12-25 Heraeus Quarzglas GmbH & Co. KG Procédé de fabrication d'un creuset de silice vitreuse
EP2194166A4 (fr) * 2007-09-28 2014-05-21 Japan Super Quartz Corp Creuset en verre de silice, procédé de production de celui-ci, et procédé de tirage

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050120945A1 (en) * 2003-12-03 2005-06-09 General Electric Company Quartz crucibles having reduced bubble content and method of making thereof
DE102005047112A1 (de) * 2005-09-30 2007-04-05 Wacker Chemie Ag In Teilbereichen oder vollständig verglaster amorpher SiO2-Formkörper, der bei höheren Temperaturen im verglasten Bereich kristallin wird, Verfahren zu seiner Herstellung und Verwendung
DE102015009423B4 (de) * 2015-07-20 2024-05-16 Qsil Gmbh Quarzschmelze Ilmenau Formstabile Silikatglaskeramik

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US4102666A (en) * 1968-02-22 1978-07-25 Heraeus-Schott Quarzschmelze Gmbh Method of surface crystallizing quartz
US5053359A (en) * 1989-03-24 1991-10-01 Pyromatics, Inc. Cristobalite reinforcement of high silica glass
US5885071A (en) * 1996-03-18 1999-03-23 Watanabe; Hiroyuki Quartz glass crucible for pulling single crystal
EP0911429A1 (fr) * 1997-09-30 1999-04-28 Heraeus Quarzglas GmbH Creuset en verre de quartz pour la production du silicium monocristallin et procédé pour sa fabrication

Family Cites Families (1)

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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

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
US4102666A (en) * 1968-02-22 1978-07-25 Heraeus-Schott Quarzschmelze Gmbh Method of surface crystallizing quartz
US5053359A (en) * 1989-03-24 1991-10-01 Pyromatics, Inc. Cristobalite reinforcement of high silica glass
US5885071A (en) * 1996-03-18 1999-03-23 Watanabe; Hiroyuki Quartz glass crucible for pulling single crystal
EP0911429A1 (fr) * 1997-09-30 1999-04-28 Heraeus Quarzglas GmbH Creuset en verre de quartz pour la production du silicium monocristallin et procédé pour sa fabrication

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002070414A1 (fr) * 2001-03-08 2002-09-12 Heraeus Quarzglas Gmbh & Co. Kg Procede de fabrication d'un creuset en verre de quartz
US6755049B2 (en) 2001-03-08 2004-06-29 Heraeus Quarzglas Gmbh & Co. Kg Method of producing a quartz glass crucible
KR100897016B1 (ko) * 2001-10-16 2009-05-14 재팬수퍼쿼츠 가부시키가이샤 석영 유리 도가니의 표면 개질 방법 및 표면개질 도가니
EP1304399A1 (fr) * 2001-10-16 2003-04-23 Japan Super Quartz Corporation Procédé pour la modification d' une surface d'un creuset en verre de quartz
WO2003089693A1 (fr) * 2002-04-22 2003-10-30 Heraeus Quarzglas Gmbh & Co. Kg Creuset en verre de quartz et procede permettant de le produire
CN1316073C (zh) * 2002-04-22 2007-05-16 赫罗伊斯石英玻璃股份有限两合公司 石英玻璃坩埚及其制造方法
US7226508B2 (en) 2002-04-22 2007-06-05 Heraeus Quarzglas Gmbh & Co. Kg Quartz glass crucible and method for the production thereof
WO2003095384A1 (fr) * 2002-05-10 2003-11-20 General Electric Company Article de quartz fondu a devitrification maitrisee
EP2194166A4 (fr) * 2007-09-28 2014-05-21 Japan Super Quartz Corp Creuset en verre de silice, procédé de production de celui-ci, et procédé de tirage
EP2141131A3 (fr) * 2008-06-30 2013-12-25 Heraeus Quarzglas GmbH & Co. KG Procédé de fabrication d'un creuset de silice vitreuse
CN102482137A (zh) * 2009-10-14 2012-05-30 信越石英株式会社 二氧化硅粉、二氧化硅容器及该粉或容器的制造方法
EP2489642A4 (fr) * 2009-10-14 2013-10-30 Shinetsu Quartz Prod Poudre de silice, contenant en silice, et procédé de production de la poudre de silice et du contenant
CN102482137B (zh) * 2009-10-14 2014-09-10 信越石英株式会社 二氧化硅粉、二氧化硅容器及该粉或容器的制造方法

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Publication number Publication date
DE10041582B4 (de) 2007-01-18
DE10041582A1 (de) 2002-03-14

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