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WO2011147860A1 - Creuset de verre quartzeux et son procédé de production - Google Patents

Creuset de verre quartzeux et son procédé de production Download PDF

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Publication number
WO2011147860A1
WO2011147860A1 PCT/EP2011/058530 EP2011058530W WO2011147860A1 WO 2011147860 A1 WO2011147860 A1 WO 2011147860A1 EP 2011058530 W EP2011058530 W EP 2011058530W WO 2011147860 A1 WO2011147860 A1 WO 2011147860A1
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WO
WIPO (PCT)
Prior art keywords
layer
region
quartz glass
bubble
crucible
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/EP2011/058530
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German (de)
English (en)
Inventor
Walter Lehmann
Thomas Kayser
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
Priority to JP2013511667A priority Critical patent/JP5639264B2/ja
Priority to CN201180025936.4A priority patent/CN102906037B/zh
Priority to DE112011101800.2T priority patent/DE112011101800B4/de
Publication of WO2011147860A1 publication Critical patent/WO2011147860A1/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
    • 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
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10—Crucibles or containers for supporting the melt
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C30B35/002—Crucibles or containers

Definitions

  • the invention relates to a quartz glass crucible for pulling single crystals, having a crucible height H and having an inner side crucible wall formed by a bottom and a quartz glass connected to the bottom side wall, the inside at least partially of a skin layer of dense quartz glass is covered. Furthermore, the invention relates to a method for producing a quartz glass crucible for pulling single crystals, comprising the following method steps:
  • Quartz glass crucibles are used to hold a silicon melt when pulling silicon single crystals by the so-called Czochralski method.
  • Czochralski method polycrystalline, metallic silicon in the quartz glass Gel melted and brought a seed crystal of silicon monocrystalline from above to the enamel surface, so that forms enamel meniscus between crystal and melt.
  • the monocrystal is slowly pulled up while rotating the crucible, whereby the silicon monocrystal grows on the seed crystal. This process is referred to below as the “startup process” or shortly as “startup”.
  • the quartz glass crucibles are usually designed with a transparent inner layer on a pore-containing, opaque outer layer.
  • the transparent inner layer is in contact with the silicon melt during the crystal pulling process and is subject to high mechanical, chemical and thermal loads.
  • the inner layer is as homogeneous as possible and low in bubbles.
  • crucible production methods with vacuum-assisted formation of the inner layer are known.
  • a vacuum melting mold is used, the wall of which has through holes, which is thus porous or provided with a plurality of through holes, so that upon application of a negative pressure on the outside of the melt, gases can be withdrawn from the SiO 2 grain layer to the outside.
  • Such a vacuum manufacturing method is known from the unpublished EP 2 236 469 A1.
  • a quartz glass crucible with bubble-free inner layer of indefinite thickness and bubble-containing outer layer is described. Bubble content and bubble size of the outer layer increase upward from the bottom of the crucible via the sidewall.
  • the transition between the area containing the high bubbles and the areas containing the low bubbles is not exactly defined, the embodiment schematically showing a division approximately at the center of the crucible.
  • the production of the bubble-free inner layer is carried out by applying a vacuum.
  • the use of different quartz glass grains as starting material is proposed. Due to the higher bubble content of the upper wall section is the Reduced weight, so that there is a lower deformation of the quartz glass crucible when used as intended.
  • a vacuum manufacturing method is known from DE 10 2008 030 310 B3.
  • an outer grain layer of relatively coarse-grained quartz grain is first produced on the inner wall of the melt.
  • another SiO 2 -grain layer of finely divided, synthetically produced SiO 2 powder is applied.
  • the granulation layers are then heated under the action of an arc from the inner wall, thereby sintering the SiO 2 granular layers into the quartz glass crucible with an opaque outer layer and a transparent inner layer.
  • the finely divided grain acts as a mechanical barrier layer by hindering the suction of atmosphere from the crucible interior when applying the vacuum on the outer mold wall, so that forms a dense, glassy sealing layer quickly and without local inhomogeneities, the rapid application allows a stronger vacuum.
  • the inner layer of synthetically produced quartz glass ensures a low concentration of impurities in the area close to the melting point and has a favorable effect on the yield of pure and dislocation-free silicon monocrystal. It has been found, however, that crucibles having an inner layer of synthetic quartz glass tend to cause oscillations of the enamel surface compared to quartz glass crucibles made of naturally occurring quartz sand. Such oscillations may be caused or enhanced, for example, by the rotation of the melt and seed crystal or by the immersion of the seed crystal. They are especially detrimental to the piecing process by making it difficult, delaying or even preventing nucleation.
  • EP 1 532 297 A1 proposes a quartz glass crucible which has a transparent inner layer made of synthetic quartz glass but which is interrupted at a height of the melt level at the beginning of the crystal pulling process by a transparent bubble zone of naturally occurring quartz glass is. This bubble zone extends in a range of at least 0.5 x H to 0.8 x H, where H represents the crucible height between the bottom of the bottom and the sidewall top edge.
  • the circumferential side wall region of the quartz glass crucible which is at the level of the melt level at the beginning of the crystal pulling process, is also referred to below as the "attachment zone”.
  • the inner wall in the region of the attachment zone is designed as a circumferential annular surface with a multiplicity of depressions.
  • a similar quartz glass crucible is also known from JP 2004-250304 A.
  • a circumferential annular surface is provided for suppressing vibrations of the silicon melt, are contained in the bubbles with a volume fraction of 0.01 to 0.2%.
  • the roughened surface around the region of the attachment zone can assume all possible contact angles with respect to the silicon melt, which prevents in-phase wetting or non-wetting of the quartz glass surface and thus counteracts the occurrence of vibrations.
  • contaminants may accumulate in the roughened area, which are released into the silicon melt during the crystal pulling process.
  • the invention has for its object to provide a quartz glass crucible, which facilitates the piecing process and in which the risk of contamination in the silicon melt is low. Furthermore, the invention has for its object to provide a method for the reproducible production of such a crucible.
  • this object is achieved on the basis of a method of the type mentioned above, that in an upper region of the granulation layer, which then extends to the lower part H to the full height, glazing below the skin layer and adjacent to this one Bubble zone is generated containing gas-filled bubbles with a specific bubble volume that is at least twice as large as the specific volume of gas-filled bubbles in low-bubble silica glass by applying the negative pressure in a lower region of the granulation layer, which extends from the bottom region to a maximum of 0, 8 times the crucible height H extends.
  • a circumferential bubble-containing zone (also referred to herein as a "bubble zone”) is created in the side wall of the quartz glass crucible, which is at the level of the melt surface at the beginning of the single-crystal drawing process - ie in the region of the attachment zone
  • the bubble-containing zone is covered by a - preferably thin - skin layer of dense quartz glass
  • the skin layer covers the entire inner wall of the granulation layer.
  • the skin layer prevents impurities in rough surface areas, for example, during cleaning or further processing steps of the crucible, during transport or during installation in the crystal pulling device.
  • the skin layer is so thin at least in the area of the attachment zone that, when the quartz glass crucible is used as intended, time is dissolved by the corrosive attack of the silicon melt, so that then the immediately adjacent bubble-containing zone of the side wall comes into direct contact with the surface of the silicon melt.
  • the bubble zone After exposure, the bubble zone shows the expected effect of reducing silicon melt oscillation.
  • the bubble zone serves as a roughened surface area, which can take all possible contact angles with the melt and thus minimizes oscillations.
  • the bubble zone extends above and below the attachment zone. That is, it is located at a height of the quartz glass crucible sidewall that corresponds to the melt level height at the beginning of the crystal pulling process. This height is known before the beginning of the drawing process due to the inner volume of the quartz glass crucible and the filling volume of silicon melt.
  • the specific bubble content (bubble volume / cm 3 ) in the bubble zone is at least twice as high as in low-bubble quartz glass, as is the case, for example, in the skin layer.
  • Bladder zone and low-bubble quartz glass are usually not directly adjacent to each other, but there is a smooth transition.
  • the lower edge of the bubble zone is in the region of the crucible side wall, ie above the bottom.
  • This upper bubble-containing partial area is also referred to here as the "upper area" of the side wall (or the grain layer), and the lower partial area as the "lower area" of the side wall (or the grain layer).
  • the bubble zone extends from its lower end, either over the entire remaining upper surface of the side wall or over only a part thereof.
  • the thickness of the bubble zone - viewed in the radial direction - corresponds to either the wall thickness of the quartz glass crucible in this area (minus the skin zone) or a part thereof.
  • crucible height H - as usual - the distance between the bottom of the crucible bottom and the side wall top edge defined. Since the bubble zone has bubbles filled with gas, they can not disappear when the quartz glass crucible is heated.
  • the generation of the bubble zone initially covered by the skin layer is based on an inhomogeneous distribution of the suction over the crucible wall in the glazing process.
  • the negative pressure is exclusively or predominantly applied in a lower region of the granulation layer, which is defined by extending from the bottom region to a maximum of 0.8 times the crucible height H.
  • the gas-filled bubbles are produced in the upper region of the granulation layer by supplying a gas to the upper region during or before vitrification of the granulation layer or by allowing an inflow of gas into the upper region ,
  • a gas is supplied to the upper portion of the granulation layer, whereas gases present in the lower portion are withdrawn due to the negative pressure treatment.
  • the gas supply in the upper region of the granulation layer increases the gas content in this region, so that gas bubbles are produced underneath the skin layer during the simultaneous or subsequent glazing of this region.
  • gases for the gas supply are, for example, nitrogen, oxygen, argon, mixtures of these gases or air.
  • the gas is not actively supplied, but provisions are also made to prevent dense sintering of the upper edge of the granulation layer during vitrification and thus allow further inflow of gas into this region.
  • the free surface areas of the granulation layer generally sinter rapidly, which prevents the further supply of gas. This applies in particular to the upper edge of the graining layer.
  • the gas is supplied to the "backside" of the granulation layer facing away from the high-temperature atmosphere, namely via a gas-permeable wall section of the melt mold Graining layer preferably supplied by a adjacent to the upper region of the granulation layer, gas-permeable wall portion of the vacuum melt mold.
  • the gas permeability may advantageously be effected by bores in the molten wall ending at the granulation layer or by a ring of porous material, such as porous graphite, disposed in the upper region of the granulation layer and forming part of the melt mold.
  • a grain barrier layer is provided between the upper and the lower region of the granulation layer, which hinders gas flow from the upper to the lower region.
  • Gas is supplied continuously to the upper portion of the granulation layer during vitrification or once before or during vitrification.
  • gases and gas mixtures which diffuse slowly in quartz glass, in particular nitrogen, argon, oxygen or air.
  • the anti-graining layer increases the flow resistance to limit outflow of gas from the upper region to the lower region of the granulation layer underlying the suction.
  • the grit barrier layer is preferably designed as an annular intermediate layer within the granulation layer of SiO 2 powder, which has a higher bulk density than the remaining SiO 2 grain of the granulation layer.
  • the graining barrier layer forms a closed powder layer between the upper and lower regions of the granulation layer.
  • the powder layer consisting of particles with a comparatively higher bulk density sets the gas flow a higher flow resistance than coarser grain size. The outflow of gas from the upper region of the granulation layer as a result of the suction acting in the lower region is thus reduced.
  • the gas-filled bubbles in the upper region of the granulation layer are produced by replacing gas present in the lower region of the granulation layer with helium, and that this gas exchange is hindered in the upper region of the granulation layer.
  • a difference between the bubbles from the lower region of the side wall and the upper region of the side wall is created by exchanging gases which are present only or predominantly in the lower region of the granulation layer by helium.
  • Helium atoms are small in size and can diffuse comparatively quickly in quartz glass, which counteracts the formation of gas-filled pores in quartz glass.
  • Arrangements which prevent or prevent or reduce gas exchange in the upper region of the graining layer preferably consist of helium being supplied to the bottom region of the graining layer and, at the same time, being sucked off over the wall of the molten state due to the negative pressure applied in the lower region of the graining layer, before reaching it the upper portion of the graining layer.
  • the gas exchange is effected only or predominantly in the lower region of the granulation layer and avoided in the upper region of the granulation layer.
  • the lower, helium-laden or evacuated region of the graining layer sinters into low-bubble or bubble-free quartz glass, whereas gas-filled bubbles remain in the upper region.
  • the skin layer is on the one hand so thick that it is not simply rubbed off during handling and transport of the quartz glass crucible, but on the other hand so thin that it is already completely removed in the earliest possible stage of the melting process. In view of this, it has proved to be advantageous if a skin layer is produced which has a thickness in the upper region of the granulation layer in the range from 50 ⁇ m to 800 ⁇ m.
  • the negative pressure in a lower region of the granulation layer which extends from the bottom region to a height which is at least 0.2 ⁇ H, preferably at least 0.4 ⁇ H.
  • a comparatively low-bubble quartz glass is obtained at least in the bottom and in the crucible side wall at a height of up to 0.2 ⁇ the crucible height H, preferably up to 0.4 ⁇ H.
  • the bubble zone or a transition zone to the bubble zone immediately follows.
  • the width of the bubble zone below the melt level is advantageously as narrow as possible and as wide as necessary. Since the height of the attachment zone in the finished quartz glass crucible is generally known in advance, the bubble zone can be limited to this height range of the quartz glass crucible.
  • the side wall region is assigned a fictitious attachment zone at a height of between 0.5 ⁇ H to 0.95 ⁇ H, the bubble zone not exceeding 10 cm, preferably not more than 5 cm, below this attachment zone enough.
  • the abovementioned object starting from a quartz glass crucible of the type specified at the outset is achieved according to the invention in that the skin layer extends at the bottom and in a lower region of the side wall which extends from the bottom to a maximum of 0.8 times the cone height H, to a bubble-poor quartz glass, and in a region adjoining the lower region up to the full crucible height H, the upper region of the side wall having a thickness in the range from 50 ⁇ m to 800 ⁇ m, to a blister. senzone from a bubble-rich, gas-filled bubbles containing quartz glass adjacent.
  • a thin skin layer of dense quartz glass covers a circumferential, bubble-containing zone in the wall of the quartz glass crucible, which lies at the level of the melt surface at the beginning of the single-crystal drawing process, ie in the region of the attachment zone.
  • the skin layer prevents impurities from accumulating in the bubbles, for example during cleaning or further treatment steps of the crucible, during transport or during installation in the crystal pulling device. It is so thin that it is dissolved in the intended use of the quartz glass crucible within a short time by the corrosive attack of the silicon melt, so that then the immediately adjacent bubble-containing zone of the side wall comes into direct contact with the surface of the silicon melt.
  • the bubble zone thus serves as a roughened surface area, which can take all possible contact angles with the melt and thus minimize oscillations.
  • the specific bubble volume in the bubble zone is at least twice as high as in low-bubble quartz glass of the skin layer Bladder content does not differ significantly or not at all from the skin layer and low-bubble quartz glass, and optically there is generally no difference between the low-bubble quartz glass of the skin layer and the low-bubble quartz glass in the bottom and the bottom side wall of the crucible.
  • the bubble zone lies in the region of the attachment zone, ie at a height of the quartz glass crucible sidewall which corresponds to the melt level height at the beginning of the crystal pulling process. This height is usually known before the beginning of the drawing process due to the inner volume of the quartz glass crucible and the volume of the silicon melt to be filled.
  • the bubble zone has bubbles filled with gas so that they do not disappear when the quartz glass crucible is heated.
  • the quartz glass crucible according to the invention can be produced by means of the above-explained method according to the invention. After removal of the quartz glass crucible from the melt mold, the top edge is uneven and is abraded or cut off.
  • the height H corresponds to the height of the crucible side wall after abrading or cutting off and also approximately to the height of the side wall region of the former granulation layer.
  • Skin layer has in the upper region of the side wall has a thickness in the range of 50 ⁇ to 800 ⁇ on.
  • the transition from the bubble zone to the adjacent lower-bubble areas of the sidewall is usually not sharp but fluid and there is a transition area.
  • the lower edge of the bubble zone lies in the crucible side wall, ie above the bottom of the crucible.
  • the bubble zone extends from its lower end, starting either over the entire upper partial surface of the side wall or only over a partial section thereof.
  • the bubble zone is helpful only at the beginning of the crystal pulling process to reduce melt oscillation. In the later stages of the crystal pulling process, a bubble-containing surface is rather undesirable.
  • the bubble zone ideally extends only at the height of the attachment zone, but not far below. In practice, it has been proven that the bubble zone extends at a height ranging from 0.4 x H to the upper edge of the pot.
  • an embodiment of the quartz glass crucible according to the invention is preferred in which the side wall is assigned a fictitious attachment zone in a height between 0.5 ⁇ H to 0.95 ⁇ H, wherein the bubble zone not more than 10 cm, preferably not more than 5 cm, below this attachment zone.
  • the strength of the bubble zone - viewed in the radial direction - corresponds either to the wall thickness of the quartz glass crucible in this area (minus the skin tone) or a part thereof.
  • Figure 1 shows a first embodiment of an apparatus for producing a
  • Figure 2 shows a second embodiment of an apparatus for producing a
  • FIG. 3 shows a third embodiment of a device for producing a
  • Quartz glass crucible according to the invention and Figure 4 shows an embodiment of the quartz glass crucible according to the invention in a side view in section.
  • the melting apparatus shown schematically in Figure 1 comprises a
  • melt form 1 made of metal with an inside diameter of 68 cm, a curved bottom and a side wall with a height of 50 cm.
  • the melt mold 1 is rotatably mounted about its central axis 2.
  • In the interior 3 of the mold 1 protrude electrodes 4 made of graphite, which are movable within the interior 3 in all directions in space indicated.
  • a plurality of passages 6 are provided, through which a vacuum applied to the outside of the molten mold 1 can pass through into the interior 3.
  • the upper third wall 17 of the mold 1 further passages 7 are present. seen, over which a gas can be directed towards the mold réelleraunn 3.
  • the passages 7 open into a common annular groove 16 which is inserted into the upper side of the melt mold wall.
  • the passages 6; 7 are each closed with a plug 1 1 of porous graphite, which prevents the escape of SiO 2 grain from the interior 3.
  • crystalline granules of natural quartz sand purified by means of hot chlorination are introduced into the melt mold 1.
  • the quartz sand has a grain size in the range of 90 ⁇ to 315 ⁇ .
  • a rotationally symmetrical, garnet-shaped granulation layer 12 of mechanically solidified quartz sand is formed on the inner wall of the melt mold 1 rotating about the longitudinal axis 2.
  • the layer thickness of the graining layer is approximately equal in the bottom area 8 and in the lower and upper side area 9, 10 and is approximately 12 mm.
  • the height of the graining layer in the sidewall area corresponds to the height of the melt shape, ie 50 cm.
  • the electrodes 4 are positioned in the further about its longitudinal axis 2 rotating mold 1 in the vicinity of the granulation layer 12 and between the electrodes 4 ignited an arc 13.
  • the electrodes are thereby subjected to a power of 600 kW (300 V, 2000 A), so that a high-temperature atmosphere is established in the mold interior 3.
  • a skin layer 14 of dense, transparent quartz glass with a thickness of about 0.5 mm is produced on the quartz granulation layer 12.
  • the free top 5 of the granulation layer 12 is compressed.
  • a vacuum (100 mbar absolute pressure) is applied to the granulation layer 12 in a third method step via the passages 6 created in the bottom region 8 and in the lower wall region 9.
  • air is introduced via the passages 7 into the upper third 10 of the still porous granulation layer 12.
  • the respective gas flows during the aspiration and introduction of air are indicated in FIGS. 1 to 3 by arrows.
  • the air essentially remains in the upper third 10 of the granulation layer.
  • relatively high loading of the SiO 2 grain with air occurs in the upper region 10 of the granulation layer.
  • the flow resistance of the granulation layer 12 in conjunction with the applied vacuum prevents the ingress of air into these regions 8; 9th
  • the expected attachment zone is in the height range - this is a height of 2/3 H, where "H" is the final crucible height is - an annular intermediate layer 15 is provided, which consists of particularly fine-grained grain size with grain sizes in the range of 80 ⁇ and which is characterized by a high flow resistance.
  • Bim vitrifying wanders a melt front from inside to outside through the granular layer 12.
  • the height H-a continuously bubble-containing, glazed zone (FIG. 4, bubble zone 41) is formed as a result of the greater air charge. This extends over the entire upper third of the wall, so a length of about 17 cm and it is completely covered by the inner skin 14.
  • the lower region 9 and the bottom region of the granulation layer 12 initially glaze without appreciable bubble formation. With regard to transparency, there is no noticeable difference between the quartz glass of the skin layer 14 and the low-bubble quartz glass of the bottom and side wall.
  • evacuation is stopped.
  • the rear side of the granulation layer 12 also glazes in the bottom and lower side wall region to form opaque, bubble-containing quartz glass. Vitrification is stopped shortly before the enamel front reaches the enamel mold.
  • the former liner 15 marks a relatively sharp transition from bubble containing fused silica to a low bubble region.
  • the bubble zone is considered to be the area in which the specific bubble volume below the skin layer is twice as high as in the skin layer. The lower edge of this zone is about 3 cm below the expected attachment zone.
  • FIGS. 2 to 4 identical or equivalent components and components are referred to, as explained in more detail above with reference to FIG.
  • a melt mold 21 which consists of a lower metal lower part 22, which defines the domed bottom and the two lower thirds of the side wall with a total height of 50 cm, which is also approximately the Height "H" of the produced quartz glass crucible corresponds.
  • an upper part in the form of a graphite ring 23 is fixed with a height of 17 cm and an inner diameter of 68 cm.
  • the graphite ring 23 is made of porous graphite with a porosity of 25%.
  • the vacuum is applied, air is sucked into the upper granulation region 10 via the porous graphite ring 23.
  • the graphite ring 23 which in this respect has a similar function as the annular groove 16 and the passages 7 of the melting device of Figure 1, the first and second embodiments of the melting device do not differ.
  • a procedure for producing a quartz glass crucible will be explained in more detail with reference to the melting device shown in FIG.
  • a granulation layer 12 is formed in the melt mold 21 and provided with a skin layer 14 in a second method step, as described with reference to FIG.
  • a vacuum (100 mbar absolute pressure) is applied to the granulation layer 12 in the bottom region 8 and in the lower wall region 9 via the passages 6, and at the same time air passes through the porous graphite ring 23 into the upper wall region 10 due to the negative pressure air
  • the graphite ring 23 not only serves as a molding element in forming the granulation layer 12, but also shields it against the heat of the arc 13, so that dense sintering of the granulation layer 12 from its side facing away from the plasma 13 is prevented.
  • a continuously vesicular zone is formed in the upper region 10 as a result of the stronger air charge, which extends downwards over the upper third of the crucible height H, ie over a length of approximately 17 cm, and that of the inner skin 14 completely covered.
  • the lower region 9 and the bottom region 8 of the granulation layer 12 vitrify without appreciable bubble formation as long as the vacuum is applied.
  • the outer region of the quartz glass crucible is produced opaque throughout, as described above with reference to FIG. The transition of the bubble zone into the low-bubble or bubble-free area is fluid.
  • the bubble zone is considered to be the area in which the specific bubble volume of the Skin layer 14 adjacent quartz glass is twice as high as in low-bubble silica glass of the skin layer 14th
  • the melting device shown schematically in FIG. 3 comprises a
  • Melt mold 31 made of metal with an inner diameter of 68 cm, a curved bottom and a side wall with a height "H" of 50 cm .
  • the mold 31 is rotatably mounted about its center axis 2.
  • electrodes 4 made Graphite in all spatial directions movable, as indicated by the directional arrows 5.
  • a plurality of passages 6 are provided, through which a vacuum applied to the outside of the mold 31 can pass inwards. Via a central opening 32 at the bottom of the melt mold 31, which is closed with a plug 33 made of porous graphite, the melt mold 31 helium can be supplied.
  • a granulation layer 12 is formed in the melt mold 21 and provided with a skin layer 14 in a second method step, as described with reference to FIG.
  • a vacuum is applied to the granulation layer 12 via the passages 6 in the lower wall region 9, and at the same time the granulation layer 12 is flooded without pressure via the central opening 32 with a gas mixture of helium.
  • the supply of the gas mixture and the simultaneous suction cause an exchange of air through the He / H 2 -Gasgemsich in the bottom and lower side region 8; 9 of the graining layer 12.
  • the rinsing process is continued during the glazing.
  • substantially the air previously contained remains.
  • vitrifying the granulation layer 12 is formed in the upper region 10 due to the strong air charge from a consistently blistering bubble zone, which is about a height of about 17 cm from the upper edge extends downwards and which is completely covered by the inner skin 14.
  • the lower region 9 and the bottom region of the granulation layer 12 initially glaze without appreciable bubble formation. With regard to transparency, there is no noticeable difference between the quartz glass of the skin layer 14 and the low-bubble quartz glass of the bottom 8 and lower side wall region 9.
  • a quartz glass crucible 40 having a bubble zone 41 is obtained with all variants of the method explained in greater detail above. Its lower edge extends approximately 2 to 3 cm below a fictitious attachment zone which runs at a height "A.”
  • the bubble zone 41 is visually easily recognizable as an opaque region, and its specific bubble content is at least twice as high as in the skin layer 14. In this area, which is designated by "B", the skin layer 14 thus adjoins the bubble zone 41.
  • the bubble zone 41 extends to the upper edge of the pot and extends over the entire wall
  • the skin layer 14 adjoins a quartz glass having a similar low bubble content, as is present in the skin layer 14.
  • This bubble-poor region is designated by the reference numeral 44 in FIG.
  • the outer wall region of the quartz glass crucible 40 also consists of opaque, bubble-containing quartz glass in the bottom and lower side wall region.
  • the crucible height "H" is shown as a distance between the bottom of the bottom 42 and the upper edge 44 of the side wall.
  • the quartz glass crucible When the quartz glass crucible is used as intended, the gas-filled bubbles are subject to bubble growth. After dissolution of the skin layer 14, a rough or wavy crucible surface is exposed in the region of the surface of the silicon melt. Because of this roughened crucible surface, any contact angle between the silicon melt and the wall results, so that melting vibrations are suppressed.

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

Abstract

L'invention concerne un procédé connu de production d'un creuset de verre quartzeux, selon lequel on prend un moule de fusion sous vide, sur la face interne duquel est façonnée une couche de granulation en SiO2 en forme de creuset, ladite couche comportant une zone fond et une zone paroi latérale. Sur au moins une partie de la couche de granulation poreuse, est formée une couche formant peau en verre quartzeux pauvre en bulles. Par application d'un vide partiel, des composantes gazeuses sont éliminées au moins d'une partie de la couche de granulation adjacente à la couche formant peau, et la couche de granulation est vitrifiée sur une hauteur de creuset H pour ainsi former le creuset en verre quartzeux. Pour produire un tel creuset en verre quartzeux qui facilite le processus de préparation et qui présente un faible risque d'introduction d'impuretés dans le silicium en fusion, l'invention propose que, lors de la vitrification en-deçà de la couche formant peau et adjacente à cette dernière, soit produite une zone de bulles dans une zone supérieure de la couche de granulation, ladite zone supérieure s'étendant dans le prolongement de la zone inférieure jusqu'à la hauteur H totale; ladite zone de bulles contenant des bulles, d'un volume spécifique, remplies de gaz, ledit volume spécifique étant est au moins deux fois supérieur au volume spécifique des bulles remplies de gaz du verre quartzeux pauvre en bulles; le vide partiel étant appliqué seulement ou de manière prépondérante dans une zone inférieure de la couche de granulation, ladite zone inférieure s'étendant de la zone fond jusqu'à maximum 0,8 fois la hauteur H du creuset.
PCT/EP2011/058530 2010-05-27 2011-05-25 Creuset de verre quartzeux et son procédé de production Ceased WO2011147860A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2013511667A JP5639264B2 (ja) 2010-05-27 2011-05-25 石英ガラスルツボを製造する方法
CN201180025936.4A CN102906037B (zh) 2010-05-27 2011-05-25 石英玻璃坩埚及其制造方法
DE112011101800.2T DE112011101800B4 (de) 2010-05-27 2011-05-25 Verfahren zur Herstellung eines Quarzglastiegels

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102010021694A DE102010021694A1 (de) 2010-05-27 2010-05-27 Quarzglastiegel und Verfahren für dessen Herstellung
DE102010021694.1 2010-05-27

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WO2011147860A1 true WO2011147860A1 (fr) 2011-12-01

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WO (1) WO2011147860A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014065621A (ja) * 2012-09-25 2014-04-17 Covalent Materials Corp シリコン単結晶引上げ用シリカガラスルツボの製造方法およびその製造装置
JP2015534537A (ja) * 2012-09-27 2015-12-03 ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ チョクラルスキー法による半導体単結晶の引き上げ及び該引き上げに適した石英ガラスるつぼ
CN115557678A (zh) * 2022-10-31 2023-01-03 浙江美晶新材料有限公司 一种石英坩埚的生产工艺
CN115572050A (zh) * 2022-10-31 2023-01-06 浙江美晶新材料有限公司 一种用于生产石英坩埚的模具

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103526280A (zh) * 2013-10-12 2014-01-22 南通路博石英材料有限公司 一种内表面具有凹槽拉晶用石英玻璃坩埚的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4713104A (en) * 1986-03-31 1987-12-15 Gte Products Corporation Quartz glass crucibles
EP1045046A2 (fr) 1999-04-16 2000-10-18 Heraeus Quarzglas GmbH & Co. KG Creuset en verre de quartz et procédé de sa fabrication
JP2004250304A (ja) 2003-02-21 2004-09-09 Japan Siper Quarts Corp 湯面振動を抑制した石英ガラスルツボ
EP1532297A1 (fr) 2002-07-31 2005-05-25 Heraeus Quarzglas GmbH & Co. KG Creuset en verre de quartz pour tirer un monocristal de silicium et procede de production de celui-ci
DE102007015184A1 (de) * 2006-03-30 2007-10-11 Toshiba Ceramics Co., Ltd. Silicaglastiegel
DE102008030310B3 (de) 2008-06-30 2009-06-18 Heraeus Quarzglas Gmbh & Co. Kg Verfahren zur Herstellung eines Quarzglastiegels
EP2236469A1 (fr) 2009-04-02 2010-10-06 Japan Super Quartz Corporation Creuset en verre de silice pour étirer du silicone monocristallin

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0920586A (ja) * 1995-06-30 1997-01-21 Toshiba Ceramics Co Ltd シリコン単結晶引上げ用石英ガラスルツボの製造方法
JP2002003228A (ja) * 2000-06-19 2002-01-09 Toshiba Ceramics Co Ltd 石英ガラスルツボ製造装置
JP5273512B2 (ja) * 2007-10-25 2013-08-28 株式会社Ｓｕｍｃｏ 石英ガラスルツボとその製造方法および用途

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4713104A (en) * 1986-03-31 1987-12-15 Gte Products Corporation Quartz glass crucibles
EP1045046A2 (fr) 1999-04-16 2000-10-18 Heraeus Quarzglas GmbH & Co. KG Creuset en verre de quartz et procédé de sa fabrication
EP1532297A1 (fr) 2002-07-31 2005-05-25 Heraeus Quarzglas GmbH & Co. KG Creuset en verre de quartz pour tirer un monocristal de silicium et procede de production de celui-ci
JP2004250304A (ja) 2003-02-21 2004-09-09 Japan Siper Quarts Corp 湯面振動を抑制した石英ガラスルツボ
DE102007015184A1 (de) * 2006-03-30 2007-10-11 Toshiba Ceramics Co., Ltd. Silicaglastiegel
DE102008030310B3 (de) 2008-06-30 2009-06-18 Heraeus Quarzglas Gmbh & Co. Kg Verfahren zur Herstellung eines Quarzglastiegels
EP2236469A1 (fr) 2009-04-02 2010-10-06 Japan Super Quartz Corporation Creuset en verre de silice pour étirer du silicone monocristallin

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014065621A (ja) * 2012-09-25 2014-04-17 Covalent Materials Corp シリコン単結晶引上げ用シリカガラスルツボの製造方法およびその製造装置
JP2015534537A (ja) * 2012-09-27 2015-12-03 ヘレーウス クヴァルツグラース ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフトＨｅｒａｅｕｓ Ｑｕａｒｚｇｌａｓ ＧｍｂＨ ＆ Ｃｏ． ＫＧ チョクラルスキー法による半導体単結晶の引き上げ及び該引き上げに適した石英ガラスるつぼ
CN115557678A (zh) * 2022-10-31 2023-01-03 浙江美晶新材料有限公司 一种石英坩埚的生产工艺
CN115572050A (zh) * 2022-10-31 2023-01-06 浙江美晶新材料有限公司 一种用于生产石英坩埚的模具

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DE112011101800A5 (de) 2013-05-08
CN102906037B (zh) 2015-06-17
JP2013527113A (ja) 2013-06-27
CN102906037A (zh) 2013-01-30
DE112011101800B4 (de) 2016-01-21
JP5639264B2 (ja) 2014-12-10
DE102010021694A1 (de) 2011-12-01

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