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WO2007039390A1 - Corps moule amorphe constitue de sio2, qui est partiellement ou entierement vitrifie et dont la zone vitrifiee cristallise a des temperatures elevees, procede de production de ce corps moule, et utilisation de celui-ci - Google Patents

Corps moule amorphe constitue de sio2, qui est partiellement ou entierement vitrifie et dont la zone vitrifiee cristallise a des temperatures elevees, procede de production de ce corps moule, et utilisation de celui-ci Download PDF

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Publication number
WO2007039390A1
WO2007039390A1 PCT/EP2006/066101 EP2006066101W WO2007039390A1 WO 2007039390 A1 WO2007039390 A1 WO 2007039390A1 EP 2006066101 W EP2006066101 W EP 2006066101W WO 2007039390 A1 WO2007039390 A1 WO 2007039390A1
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WO
WIPO (PCT)
Prior art keywords
vitrified
green body
glazed
amorphous
sio
Prior art date
Application number
PCT/EP2006/066101
Other languages
German (de)
English (en)
Inventor
Fritz Schwertfeger
Original Assignee
Wacker Chemie 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
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Publication of WO2007039390A1 publication Critical patent/WO2007039390A1/fr

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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
    • 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
    • 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
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/0025—Other surface treatment of glass not in the form of fibres or filaments by irradiation by a laser beam
    • 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
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
    • C30B1/023—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing from solids with amorphous structure
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/22—Wet processes, e.g. sol-gel process using colloidal silica sols
    • 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
    • C03C2203/36—Gel impregnation
    • 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
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/425—Coatings comprising at least one inhomogeneous layer consisting of a porous layer

Definitions

  • the invention relates to a part-areas or completely glazed amorphous SiO 2 -form redesign, which becomes crystalline at higher temperatures in the vitrified area, a process for its preparation and its use.
  • Porous, amorphous SiO 2 ⁇ moldings are on many technical
  • Glass fibers or optical fibers serve.
  • crucibles for pulling single crystals, in particular silicon single crystals, can also be produced in this way.
  • the standard drawing process uses quartz glass crucibles, which are melted from crystalline SiO 2 particles (eg quartz sand) in a melting process, usually in the arc.
  • crystalline SiO 2 particles eg quartz sand
  • a closed, amorphous, glazed inner layer in which as few and as far as possible as small as possible bubbles should be included, and a fully glazed outer body with low porosity is formed.
  • Impurities of the inner surface of the crucible which are applied during the manufacturing process or diffuse from the starting material to the surface during the production and the subsequent CZ process, lead to corrosion of the inner surface during the CZ process. berflache.
  • the occurrence of corrosion in amorphous quartz glass crucibles is a limiting factor for the length of time within which the production of single crystal material is possible.
  • the crystalline quartz layer which is then produced in the CZ process only reaches a thickness of less than 1 mm when coating the inside of the crucible and less than 2 mm when coating the outside of the crucible. This means that when coating the outside of the crucible, increasing the stability of the crucible is strictly limited.
  • the very thin crystalline layer forming in the CZ process leads to mechanical stresses between the crystalline and the amorphous region of the quartz glass crucible. These are based on the different thermal expansion coefficients and the different mechanical stability of the amorphous and crystalline modifications of the crucible material as a function of the temperature. These stresses can cause quartz particles to peel off the inner surface of the crucible and pass through the Si melt to the growing crystal where they cause undesirable dislocations. In addition, under the thin crystalline layer of the inner surface of the crucible, the bubbles present in the amorphous starting material grow during the CZ process with undiminished speed and also contribute to the emission of quartz particles into the Si melt when bursting.
  • an amorphous SiO 2 -formed body which is characterized in that it is in a partial area or completely vitrified and is infiltrated in this area with at least one substance which upon heating of the
  • Shaped body to a temperature of 1000 0 C to 1800 0 C for crystallization of the vitrified area leads.
  • the vitrified area which takes place in the moldings according to the invention, it is preferably a cristobalite formation.
  • the substance which leads to the crystallization of the vitrified area upon heating it is preferably a compound selected from the group of barium, aluminum and boron compounds and mixtures thereof.
  • Particularly preferred are Ba (OH) 2 , barium oxide, barium carbonate or aluminum oxide.
  • Very particularly preferred is Ba (OH) 2 , barium oxide or barium carbonate.
  • This amorphous Si0 2 shaped body is obtained by means of a process in which a) an amorphous SiO 2 green body is infiltrated with a substance which initiates and / or promotes crystallization and b) subsequently while maintaining its amorphous state by contactless heating by means of a laser beam is sintered or glazed.
  • an amorphous SiO 2 green body is an amorphous SiO 2 particle (silica glass). to understand by means of shaping steps porous amorphous open-pore shaped body.
  • SiO 2 green bodies whose preparation is described in US Pat. No. 6,699,808 Bl or in DE 102005036746 are particularly suitable.
  • the SiO 2 green body preferably has a crucible shape.
  • such an amorphous porous open-pore SiO 2 green body such as described in US 6,699,808 Bl, wholly or partially added to a compound which promotes or effects a crystallization of the SiO 2 , preferably a cristobalite formation. Suitable for this purpose are all compounds known to the person skilled in the art. Examples which may be mentioned are the compounds described in US 5,980,629, US 5,053,359 or GB 1428788.
  • a compound is selected from the group of barium, aluminum and boron compounds and mixtures thereof.
  • Particularly preferred is Ba (OH) 2 , barium oxide, barium carbonate or aluminum oxide.
  • Very particularly preferred is Ba (OH) 2 , barium oxide or barium carbonate.
  • the compound may be added before and / or after the crucible formation to the starting material for producing the silica green body. This can be done by methods known in the art. If the addition is to take place after the crucible formation, it is an application to and / or penetration into the surface of the silica green body. This can be done both before drying and after drying of the silica green body.
  • the silica glass green body is previously subjected to a temperature treatment (sintering). Preferably, this is done at temperatures between 500 0 C and 1300 0 C, more preferably between 800 ° C and 1100 0 C for a time of 1 to 180 min., Preferably for a time of 1 to 60 min. This is a confluence the grain boundaries, whereby so-called grain necks form. This leads to an increased mechanical stability of the silica green body. In this temperature treatment, however, an open porosity of the silica green body must be maintained.
  • the addition of the compound takes place in liquid and / or solid form. If the compounds are added in liquid form, they are preferably solutions thereof. In principle, all solvents come into consideration as solvents in which the respective substance dissolves in a sufficient concentration. Preferred solvent is water.
  • the concentration of the compounds in the solution is preferably between 0.001 and 100% by weight, preferably between 0.001 and 10% by weight, more preferably between 0.001 and 1% by weight.
  • the solutions may be one or more times, preferably 1 to 3 times, targeted z. B. be applied by spraying, dipping or soaking. Since it is open-pore silica glass green body, penetrates the solution using the capillary forces in the pores in the silica green body and wets there preferably the surface of the pores. A single or multiple targeted electrophoretic deposition of the dissolved in the respective solvent substances in the pores of the silica green body is possible.
  • the fused silica green body is dried.
  • water preferably between 40 0 C and 100 0 C, more preferably between 70 0 C and 95 ° C.
  • the drying can also be done under vacuum.
  • one or more regions or layers can be produced in the silica glass green body in which the pore surface is completely or partially coated with the compounds mentioned. Further, the concentrations on the pore surface can be adjusted as desired.
  • a crucible wall with a connection-containing inner and / or outer layer of a respective desired thickness or also a connection-containing layer located completely in the interior of the crucible wall or else a silica glass green body completely penetrated with the compounds listed above can be produced.
  • the compounds are used in solid form, they are preferably already added to the SiO 2 -containing dispersion from which a crucible-shaped silica glass green body is formed.
  • the compounds can be used in all particle sizes and forms, but preference is given to using particles of the order of magnitude of the SiO 2 particles used for the dispersion. Preferably, all particles in the dispersion are distributed as homogeneously as possible.
  • the preparation of the dispersion and the addition to and distribution of the particulate compounds in the dispersion is carried out by methods known to those skilled in the art.
  • the preparation of the shaped article from this dispersion likewise takes place by means of the customary methods known to the person skilled in the art, as are known, for example, from US Pat. No. 6,699,808.
  • the compounds are not only on the surface of the Pores of the dried silica glass green body distributed, but also between the SiO 2 particles that form the crucible.
  • crystallization can be achieved when crystalline SiC> 2 particles are added to the dispersion and / or the porous silica glass green body.
  • the crystalline SiC> 2 particles should preferably have the same particle sizes as the amorphous particles which form the silica glass green body.
  • the resulting amorphous open-pore SiÜ 2 green body is sintered or glazed while maintaining its amorphous state by contactless heating by means of a laser beam.
  • it is a laser with a beam of a wavelength preferably greater than the absorption edge of the silica glass at 4.2 microns.
  • the energy required for sintering or glazing is preferably coupled into the shaped body by means of a CO 2 laser.
  • CO 2 laser with a beam of a wavelength of 10.6 microns.
  • the inside and the outside of the SiO 2 green body are irradiated by a laser beam with a focal spot diameter of at least 2 cm and thereby sintered or glazed.
  • the irradiation is preferably carried out with a radiation power density of 10 W to 500 W per square centimeter, more preferably from 30 W to 200 W and most preferably from 40 to 120 W / cm 2 .
  • the irradiation preferably takes place uniformly and continuously on the inside and the outside of the SiO 2 green body.
  • the uniform, continuous irradiation of the inside and the outside of the SiO 2 green body for sintering or vitrification can be carried out in principle by a movable laser optics and / or a corresponding movement of the crucible in the beam of the laser.
  • the movement of the green body in the laser beam is preferred. It can be carried out by all methods known to the person skilled in the art. It is particularly preferred by means of a robot.
  • the process is preferably performed at pressures below the pressure at which the single crystal is pulled in the later drawing process. This will, should there be a small number of gas bubbles, a subsequent increase of these avoided.
  • the SiO 2 green body to be sintered or glazed is kept under reduced pressure or vacuum during the entire process.
  • the pressure is below the normal pressure of 1013.25 mbar, particularly preferably between 0.01 and 100 mbar, very particularly preferably between 0.01 and 1 mbar.
  • the required laser power is up to 30% lower than the o. G. Values, since the encapsulation of the sample in the vacuum chamber results in less energy exchange with the environment.
  • the SiO 2 shaped body to be sintered or glazed can be kept under a gas atmosphere during the entire process. If the gas or gases can diffuse well in the molten glass, this leads to a significant reduction of the gas bubbles.
  • a helium atmosphere is suitable as the gas, since helium can diffuse particularly well in molten glass.
  • a combination of gas atmosphere and reduced pressure is possible. Particularly preferred is a reduced helium atmosphere.
  • a closed, pore-free, bubble-free and crack-free ⁇ -morphic SiO 2 surface is produced during the sintering or glazing of the green body.
  • the amorphous SiC> 2 is brought to sintering or melting by absorption of the laser radiation.
  • the thickness of the glazed inside or outside is controlled at each location via the entry of laser power.
  • the glazing or sintering of the surface of the SiC> 2 green body is carried out at temperatures between 1000 0 C and 2500 0 C, preferably between 1300 ° C and 1800 0 C, more preferably between 1400 ° C and 1500 ° C.
  • a variant of the method according to the invention enables a spatially limited, defined vitrification or sintering of a SiC> 2 green body.
  • the parameters and procedure preferably correspond to the method already described with the restriction that only one side of the shaped body is irradiated.
  • moldings can be glazed on one side in this way.
  • the invention thus also relates to an inside completely glazed, outside open-pored Si ⁇ 2 ⁇ Formkorper and an outside completely glazed, inside porous Si ⁇ 2 -Formkorper.
  • the inside completely glazed, outside open-porous Si ⁇ 2 -Formkorper is preferably a silica glass crucible for the pulling of silicon single crystals according to the CZ method.
  • Another advantage of the inventive method is the good focusability of the laser, whereby a very high local energy density can be achieved.
  • An internally vitrified silica glass crucible is preferably used for single crystal pulling by the CZ method.
  • Example 1 Preparation of a silica glass green body according to the invention a) Preparation of a SiC> 2 dispersion
  • the dispersion thus prepared consisted of 5119 g of solid, which corresponds to a solids content of 70% by weight (with a proportion of 3.5% of fumed silica based on the amount of solids).
  • Part of the SiO 2 dispersion is pressed from a storage tank at a pressure of 5 bar through a conduit system between two open-pored plastic membranes made of methyl methacrylate.
  • the membranes have a porosity of 30% by volume and an average pore radius of 20 ⁇ m.
  • the distance between the two membranes to each other allows the formation of a 10 mm thick cullet.
  • the two diaphragms are subjected to a closing pressure of 60 bar.
  • the pressure in the receiver is reduced to 0 bar overpressure.
  • Special air and water pipes laid in the membrane make it possible to apply air or water to the shaped body through the porous membrane for final shaping.
  • the shaped body separates from the membrane.
  • the shaped body is released from the outer membrane.
  • the inner membrane is moved upwards.
  • the mold now hangs on the inner membrane.
  • An interlocking pad is positioned under the mold.
  • the Formkorper is deposited on the pad and dissolved by the inner membrane.
  • the inner membrane is in turn moved upwards.
  • the produced amorphous open-pore porous shaped body with a body thickness of 10 mm has a solids content of 78% by weight and a residual water content of 22% by weight. After drying at 90 0 C for 3 hours, the molded article is completely dry.
  • the amorphous open-pore porous shaped body is filled with 20 g of a
  • Aqueous BaOH solution inside evenly sprayed using a commercial spray gun.
  • an inner layer of 3 mm layer thickness was infiltrated with barium hydroxide.
  • the concentration of barium in these layers was 46 ⁇ g per gram of SiO 2 .
  • the crucible was dried at 200 ° C. for 4 hours.
  • the infiltrated green body is produced in a vacuum laser system consisting essentially of a moving part realized by an ABB robot (type IRB 2400), a vacuum chamber, a special vacuum rotary union and a CO 2 laser (type TLF 3000 Turbo) with 3 kW beam power (see Fig. 1) irradiated.
  • the vacuum rotary feedthrough connects the freely movable vacuum chamber in three axes with the optics of the laser.
  • the vacuum chamber is evacuated to a pressure of 2 * 10 ⁇ 2 mbar.
  • the laser is equipped with a rigid beam guidance system and all degrees of freedom of movement have been provided by the robot.
  • the beam guide is equipped with optics for widening the primary beam.
  • the primary jet has a diameter of 16 mm. After the parallel primary beam has passed the expansion optics, a divergent beam path results.
  • the focal spot on the 14 "crucible has a diameter of 50 mm with a distance of about 450 mm between the optics and the crucible .
  • the robot is controlled by a program adapted to the crucible geometry With the crucible rotating (angular velocity 0.15 ° / s), the top of the crucible is first swept by the laser over an angle of 375 °, then the remainder of the inside surface is formed as a screw The speed of rotation and the speed of advancement of the ink on an axis from the edge of the crucible to the middle are accelerated in such a way that the swept area per unit of time is constant.
  • the laser radiation does not hit the sample surface at a constant angle during blanket scanning. Nevertheless, one To achieve uniform glazing, the focal spot temperature is determined during the process with a pyrometer integrated in the beam path of the laser and used as a control variable for a process-integrated power control of the laser. The irradiation takes place on average with about 55 W / cm 2 .
  • a sintering of the SiO 2 shaped body is achieved by heat conduction from the hot inner surface into the interior of the shaped body.
  • the Si ⁇ 2 ⁇ crucible After the laser irradiation, the Si ⁇ 2 ⁇ crucible, while maintaining its original, outer geometry in a thickness of 3 mm inside the entire area, glazed and crack-free.
  • the transparent glass layer is 100% amorphous (see Figs. 2a and 2b).
  • Example 2 Temperature treatment of a shard prepared according to Example 1 for the detection of cristobalite formation in the glass layer.
  • a green body shard (prepared according to Example Ia and Ib) is infiltrated in a partial area with Ba (OH) 2 (as described in Example Ic) and glazed by laser in this area 3 mm (as described in Example Id) (see FIG. 3)
  • this sherd is heated in a sintering furnace under a nitrogen atmosphere of 1 bar at a heating rate of 10 0 C per minute at 1600 0 C, held for 2 hours at 1600 ° C and within 10 hours at 25 ° C. cooled.
  • the shard shows a cristobalite formation after the temperature treatment in the previously glazed area, while it is transparent and amorphous in the remaining area (see FIGS. 4a and 4b).
  • the temperature of 1600 0 C corresponds approximately to the temperature, which undergoes a crucible in the drawing system in the pulling of silicon monocrystals according to the Czochralski method.

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  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Metallurgy (AREA)
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  • Optics & Photonics (AREA)
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  • Toxicology (AREA)
  • Composite Materials (AREA)
  • Dispersion Chemistry (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un corps moulé amorphe constitué de SiO2 caractérisé en ce qu'une partie ou la totalité de ce corps moulé est vitrifiée, et en ce qu'au moins une substance est introduite dans la zone vitrifiée dudit corps, cette substance entraînant la cristallisation de la zone vitrifiée lorsque le corps moulé est chauffé à une température comprise entre 1000 °C et 1800 °C.
PCT/EP2006/066101 2005-09-30 2006-09-07 Corps moule amorphe constitue de sio2, qui est partiellement ou entierement vitrifie et dont la zone vitrifiee cristallise a des temperatures elevees, procede de production de ce corps moule, et utilisation de celui-ci WO2007039390A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200510047112 DE102005047112A1 (de) 2005-09-30 2005-09-30 In Teilbereichen oder vollständig verglaster amorpher SiO2-Formkörper, der bei höheren Temperaturen im verglasten Bereich kristallin wird, Verfahren zu seiner Herstellung und Verwendung
DE102005047112.9 2005-09-30

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WO2007039390A1 true WO2007039390A1 (fr) 2007-04-12

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DE102017100242A1 (de) * 2017-01-09 2018-07-12 Schott Ag Verfahren zur Herstellung einer Glaskeramik-Kochfläche mit lokal erhöhter Transmission und verfahrensgemäß herstellbare Glaskeramik-Kochfläche

Citations (8)

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DE10041582A1 (de) * 2000-08-24 2002-03-14 Heraeus Quarzglas Quarzglastiegel sowie Verfahren zur Herstellung desselben
DE10139648A1 (de) * 2001-03-08 2002-10-02 Heraeus Quarzglas Verfahren zur Herstellung eines Quarzglastiegels
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