WO2024082663A1 - Combined crucible and single crystal furnace using same - Google Patents

Combined crucible and single crystal furnace using same Download PDF

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Publication number
WO2024082663A1
WO2024082663A1 PCT/CN2023/100949 CN2023100949W WO2024082663A1 WO 2024082663 A1 WO2024082663 A1 WO 2024082663A1 CN 2023100949 W CN2023100949 W CN 2023100949W WO 2024082663 A1 WO2024082663 A1 WO 2024082663A1
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WO
WIPO (PCT)
Prior art keywords
crucible
mesh
carbon
graphite
combined
Prior art date
Application number
PCT/CN2023/100949
Other languages
French (fr)
Chinese (zh)
Inventor
申富强
张晶
孙亚林
牛龙祥
Original Assignee
上海骐杰碳素材料有限公司
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
Priority claimed from CN202211287328.7A external-priority patent/CN115595655A/en
Priority claimed from CN202222767072.1U external-priority patent/CN218539883U/en
Application filed by 上海骐杰碳素材料有限公司 filed Critical 上海骐杰碳素材料有限公司
Publication of WO2024082663A1 publication Critical patent/WO2024082663A1/en

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    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • 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

Definitions

  • the invention belongs to the technical field of single crystal silicon or polycrystalline silicon manufacturing, and in particular relates to a combined crucible and a single crystal furnace using the combined crucible.
  • a single crystal furnace is a device that uses a graphite heater to melt polycrystalline materials such as polycrystalline silicon in an inert gas environment and grows single crystals without dislocation using the Czochralski method.
  • Crystal pulling refers to the process in which the silicon atoms of molten silicon are arranged into many crystal nuclei in a diamond lattice when they solidify. If these crystal nuclei grow into grains with the same crystal plane orientation and combine in parallel, they will crystallize into single crystal silicon.
  • the crucible structure in the existing single crystal furnace is to wrap a graphite, carbon-carbon or ceramic crucible outside a quartz crucible, and the heater directly heats the graphite, carbon-carbon or ceramic crucible to melt the silicon in the quartz crucible.
  • the volatilized silicon monoxide is carried to the bottom of the furnace body by the argon flow and discharged from the exhaust pipe.
  • silicon monoxide flows through graphite parts, such as graphite, carbon-carbon or ceramic crucibles, heaters, insulation tubes, etc., it will react with them to form silicon carbide.
  • the present invention provides a combined crucible and a single crystal furnace using the crucible, which solves the above problems.
  • a combined crucible of the present invention comprises an inner crucible sleeved on the outside of a quartz crucible and a mesh crucible for covering the inner crucible, wherein the inner crucible is a graphite crucible, a carbon-carbon crucible or a ceramic crucible;
  • the mesh crucible and the inner crucible are bonded together by a mesh bag limiting structure or by graphite glue.
  • the net bag limiting structure includes using a protrusion arranged on the outer surface of the inner crucible to hang the mesh crucible or using a step structure arranged on the outer surface of the inner crucible to clamp the mesh crucible; the depth of the step structure is 1-10mm; the thickness of the protrusion is 1-10mm.
  • the inner crucible is a one-piece crucible or a split crucible
  • the split crucible includes a multi-petal crucible.
  • the mesh crucible is a hollow mesh body formed by weaving one or more carbon fiber ropes to cover the inner crucible, and the inner surface of the mesh crucible is in contact with the outer surface of the inner crucible.
  • the mesh crucible is specifically bowl-shaped or straight-cylindrical, with an opening at the bottom or covered by woven carbon fiber ropes, and the top of the mesh crucible is an opening.
  • the surface of the carbon fiber rope of the mesh crucible is coated or filled with a deposited carbon layer or a hardened material layer.
  • the material of the ceramic crucible includes any one or more of boron nitride, silicon carbide, tungsten carbide, zirconium oxide, aluminum oxide, aluminum nitride, titanium diboride, and tungsten carbide.
  • a single crystal furnace comprises the above-mentioned combined crucible.
  • a crystal pulling method which uses the single crystal furnace to pull crystals.
  • the present invention has the following beneficial effects:
  • the technical solution divides the crucible into a two-layer structure of an inner crucible and a mesh crucible, and adopts a mesh crucible that is sleeved on the outside of a graphite, carbon-carbon or ceramic crucible that wraps a quartz crucible.
  • the mesh crucible is a hollow mesh body formed by weaving carbon fiber ropes to cover the graphite, carbon-carbon or ceramic crucible, and its inner surface fits the outer wall of the graphite, carbon-carbon or ceramic crucible; the mesh crucible can always maintain the structural stability of the graphite, carbon-carbon or ceramic crucible, making it possible to select a graphite, carbon-carbon or ceramic crucible with a thinner wall thickness than the existing one.
  • the strength of the combined crucible formed by the thin-walled graphite, carbon-carbon or ceramic crucible and the outer mesh crucible wrapping it is comparable to that of the original thick-walled single-layer There is no decrease compared to graphite, carbon-carbon or ceramic crucibles;
  • the technical solution adopts a two-layer structure of an inner crucible and a mesh crucible.
  • the inner crucible is corroded and the inner diameter becomes larger or cracks due to thermal expansion, only the inner crucible needs to be replaced, and the mesh crucible can be reused.
  • the replacement cost is lower;
  • the technical solution adopts a two-layer structure of an inner crucible and a mesh crucible.
  • the inner crucible has a thinner wall than the original thick-walled single-layer crucible, and the mesh crucible is hollow.
  • the overall heat conduction efficiency is improved, and the heating and cooling time is greatly shortened. Not only is the power requirement for the heater lower, but the crystal pulling efficiency can also be improved.
  • the mesh crucible used in this technical solution can facilitate the detachment of graphite, carbon-carbon or ceramic crucibles when they need to be replaced;
  • the technical solution adopts a combined structure in which a mesh crucible is used to cover and support the inner crucible.
  • the inner crucible can adopt a split crucible structure, such as a three-petal or multi-petal crucible, it can not only effectively reduce the impact of thermal expansion, but also has a good overall retention effect.
  • the two-layer structure composed of the inner crucible and the mesh crucible of the technical solution is a mesh bag limiting structure or bonding the two layers by graphite glue, wherein the mesh bag limiting structure specifically includes a protrusion arranged on the outer surface of the inner crucible to hang the mesh crucible or a step structure arranged on the outer surface of the inner crucible to clamp the mesh crucible.
  • the protrusion and step structure are simple in style, which can make the mesh crucible well combined with the inner crucible, and the installation and disassembly are simple and convenient.
  • FIG1 is a schematic structural diagram of a combined crucible according to a specific embodiment 1 of the present invention.
  • FIG2 is a schematic structural diagram of the mesh crucible in FIG1 ;
  • FIG3 is a schematic diagram of the structure of an inner crucible in FIG1 made of graphite, carbon-carbon or ceramic crucible;
  • FIG4 is a schematic structural diagram of a combined crucible according to a specific embodiment 2;
  • FIG5 is a schematic structural diagram of the inner crucible in FIG4 ;
  • FIG6 is a schematic structural diagram of a combined crucible according to a specific embodiment 3.
  • FIG7 is a schematic structural diagram of an inner crucible with a step structure corresponding to FIG6 ;
  • FIG8 is a schematic structural diagram of a mesh crucible according to a specific embodiment 4.
  • FIG9 is a schematic structural diagram of a mesh crucible of specific embodiment 5.
  • FIG10 is a schematic structural diagram of a mesh crucible of specific embodiment 6;
  • FIG11 is a schematic diagram of the structure of a three-petal graphite, carbon-carbon or ceramic crucible of specific embodiment 7;
  • FIG12 is a schematic diagram of the structure of a combined crucible using the three-petal graphite, carbon-carbon or ceramic crucible in FIG11;
  • FIG13 is a schematic diagram of one of the braiding methods of the carbon fiber rope
  • FIG14 is a second schematic diagram of the braiding method of the carbon fiber rope
  • FIG15 is a third schematic diagram of the braiding method of the carbon fiber rope.
  • FIG16 is a fourth schematic diagram of the braiding method of the carbon fiber rope.
  • FIG17 is a fifth schematic diagram of the braiding method of the carbon fiber rope.
  • FIG18 is a schematic diagram of another braiding method of a carbon fiber rope
  • FIG19 is a schematic diagram of the structure of the combined crucible of the present invention installed in a single crystal furnace
  • FIG20 is a schematic diagram of the structure of an existing single crystal furnace
  • FIG. 20 the internal structure of a single crystal furnace using a graphite, carbon-carbon or ceramic crucible is shown.
  • a single-layer integral graphite, carbon-carbon or ceramic crucible with thicker walls and heavier mass is used to wrap the outside of the quartz crucible. Because the thermal expansion coefficients of the graphite, carbon-carbon or ceramic crucible and the quartz crucible are inconsistent, the graphite, carbon-carbon or ceramic crucible will crack.
  • a combined crucible of the present invention comprises an inner crucible 1 sleeved on the outside of a quartz crucible and a mesh crucible 2 for covering the inner crucible 1, wherein the inner crucible 1 is made of graphite crucible, carbon-carbon crucible or ceramic crucible; a mesh bag limiting structure is used between the mesh crucible 2 and the inner crucible 1 or the mesh crucible 2 is bonded with graphite glue; the mesh bag limiting structure comprises a protrusion 101 provided on the outer surface of the inner crucible 1 to hang the mesh crucible 2 or a step structure A provided on the outer surface of the inner crucible 1 to clamp the mesh crucible 2;
  • the inner crucible 1 adopts an integral crucible or a split crucible, and the split crucible includes a multi-petal crucible.
  • the inner crucible 1 in the present technical solution does not need to adopt a graphite, carbon-carbon or ceramic crucible with a thicker wall thickness.
  • the thickness of the inner crucible 1 in the present technical solution can be 5 mm, 8 mm or 10 mm, which greatly reduces the specific thickness and brings about a reduction in weight and manufacturing cost.
  • the mesh crucible 2 is a hollow mesh body formed by weaving one or more carbon fiber ropes to cover the inner crucible 1, and its inner surface is in contact with the outer surface of the inner crucible 1.
  • the mesh crucible 2 is specifically bowl-shaped or straight-cylindrical, with an opening at the bottom or covered by woven carbon fiber ropes, and the top of the mesh crucible 2 is an opening; as a specific embodiment, the surface of the carbon fiber rope of the mesh crucible 2 can be coated or filled with a deposited carbon layer or a hardened material layer; the hardened material layer specifically includes silicon carbide, silicon nitride or other ceramic materials; the thickness of the mesh crucible 2 is greater than or equal to 1mm, preferably 5-18mm; the inner crucible 1 is a graphite, carbon-carbon or ceramic crucible, and its thickness is greater than or equal to 1mm, preferably 5-10mm; when a ceramic crucible is used, the material of the ceramic crucible includes any one or more of boron
  • the mesh crucible 2 is formed by weaving one or more carbon fiber ropes, wherein the specific structural form of the mesh crucible 2 is shown in FIG. 2 and FIG. 8-10, including a crucible-type mesh structure with an upper edge seal, a lower edge seal and a middle hollow net as shown in FIG. 2, in which the bottom can be set as an open hole or a braided rope for bottoming; a bowl-shaped structure with only a middle hollow net and a bottom with a lower edge seal as shown in FIG. 8, in which case the bottom can be set as an open hole or a braided rope for bottoming; as shown in FIG. 9, a bowl-shaped structure with only a middle hollow net bottom
  • the first part is an open bowl-shaped structure; as shown in FIG10 , it is a straight cylindrical structure with only a hollow net in the middle;
  • the combined crucible of the present technical solution adopts the form of a mesh crucible 2 wrapped around the outer surface of the inner crucible 1.
  • one cycle is 400 hours, which adds 2 more use cycles, greatly improving the service life of the crucible and saving costs.
  • the present technical solution adopts a 13mm thick graphite inner crucible 1 and a 2mm thick mesh crucible 2.
  • the inner diameter of the inner crucible 1 of the present technical solution is 951mm before crystal pulling, and expands to 953mm after the crystal pulling is completed, while the inner diameter of the ordinary monolithic graphite inner crucible 1 is 951mm before crystal pulling, and expands to 954mm after the crystal pulling is completed.
  • the crucible structure of the present technical solution has a smaller expansion degree;
  • each of the carbon fiber ropes contains multiple carbon fiber yarns, the center of the rope is a carbon fiber yarn parallel to the axis of the rope, and the carbon fiber yarn parallel to the axis is coated with a carbon fiber braided tube;
  • the edge sealing part and the lower edge sealing part are annular bodies, woven from one or more of the carbon fiber ropes, the braiding method of the upper edge sealing part and the lower edge sealing part is different from the braiding method of the middle ring part, and the braiding density of the upper edge sealing part and the lower edge sealing part is greater than the braiding density of the middle ring part;
  • the mesh body of the middle ring part is aligned along a first direction inclined at a first angle relative to the central axis by one or more carbon fiber ropes; aligned along a second direction inclined at a second angle relative to the central axis by one or more carbon fiber
  • the braiding method of this embodiment is called a cross braiding method; as shown in Figures 13-18, it is various braiding methods for braiding the corresponding upper and lower edge sealing parts, which are braided by one or more carbon fiber ropes.
  • another weaving method is used to weave the mesh crucible 2 with only a straight cylindrical structure in the middle, the middle ring portion includes a plurality of axial bars, one or more carbon fiber ropes are spirally woven around the axial bars, and the angle between the axial bars and the spiral weaving direction of the carbon fiber rope is greater than 70 degrees and less than 90 degrees.
  • the weaving method of this embodiment is called a spiral weaving method.
  • the middle ring portion includes the support of a plurality of axial bars, and there may be no edge sealing portion.
  • the mesh crucible 2 is specifically made by twisting 30k carbon fiber bundles into a carbon fiber rope, pre-impregnating the carbon fiber rope with resin, and then weaving it into a strip fabric as a carbon fiber rope.
  • the resin is specifically epoxy resin.
  • the mass of the epoxy resin is 6% of the total mass of the carbon fiber bundle or the carbon fiber rope and the resin; then weaving it into a mesh according to the above-mentioned weaving method and shape to obtain a carbon fiber mesh body as the above-mentioned weaving shape, and then the obtained carbon fiber mesh body is
  • a carbon fiber mesh preform is formed by die-assisted curing, wherein the curing and shaping conditions are: a curing temperature of 200°C, a time of 6 hours, and a heating rate of 8°C/min; the mold adopts a common graphite mold in the field, and the mold is consistent with the shape of the inner crucible; after removing the mold, vapor deposition is then carried out, and the obtained carbon fiber mesh preform is placed in
  • the carbon fiber constituting the carbon fiber rope asphalt-based carbon fiber, PAN-based carbon fiber, viscose-based carbon fiber, etc. can be used.
  • the carbon fibers constituting the carbon fiber rope can be the same material or different materials.
  • the mesh crucible 2 of the present application is woven with a carbon fiber rope made of a carbon fiber composite material, and does not need to make an embryo.
  • the shape of the mesh crucible 2 is not limited by the embryo and can be flexibly designed. Due to the uniform specifications of the raw materials, it can be mass-produced, improve the production efficiency of the fiber rope, and shorten the manufacturing time of the mesh crucible, so the cost is low, the delivery cycle is short, and it is easy to supply.
  • a single crystal furnace includes a combined crucible with the above technical features, which is installed in the inner furnace cavity of the single crystal furnace;
  • the invention discloses a crystal pulling method, in particular a crystal pulling method using the combined crucible.
  • the mesh crucible 2 of the combined crucible specifically adopts a mesh crucible 2 structure with an upper sealing edge, a lower sealing edge and a middle mesh woven portion, and the upper sealing edge and the lower sealing edge are specifically any one of the above-mentioned weaving methods; and the inner crucible 1 in the specific embodiment specifically adopts a monolithic graphite, carbon-carbon or ceramic crucible, and its height is consistent with the height of the mesh crucible 2;
  • a mesh bag limiting structure is provided on the outer surface of the inner crucible 1.
  • the mesh bag limiting structure specifically adopts a protrusion 101 arranged around the upper surface of the outer surface of the inner crucible 1 to limit and suspend the mesh crucible 2, so that the protrusions 101 on the outer peripheral side of the inner crucible 1 correspond to the mesh bag holes on the upper part of the mesh crucible 2 to achieve suspension.
  • the number of protrusions 101 is not limited.
  • a surrounding arrangement is adopted and corresponds to the number and position of a single row of mesh bag holes, or is arranged corresponding to the gap between the single row of mesh bag holes.
  • the shape of the protrusion 101 is a triangle, and a protrusion 101 is arranged at a spacing of 50 mm.
  • a circle, a quadrilateral or other polygon can also produce the same technical effect, and should also belong to the protection scope of the present technical solution; after protruding, the mesh crucible 2 is suspended and limited; the thickness of the protrusion 101 is 5 mm, in the present specific embodiment Only one thickness data is listed, and any thickness in the range of 1-10 mm can achieve the same technical effect, and the mesh crucible 2 can be well and firmly fixed to the inner crucible 1, which should all fall within the protection scope of the present technical solution.
  • the difference between this specific embodiment and specific embodiment 1 is that the mesh bag limiting structure arranged on the outer surface of the inner crucible 1 of this specific embodiment specifically adopts a step structure A, and the step structure A is specifically that the outer surface of the inner crucible 1 is arranged with step-type limiting rings 102 in sequence from top to bottom, and the diameter of the step-type limiting rings 102 decreases from top to bottom, so that the mesh bag structure of the same diameter on the upper part of the mesh crucible 2 can be clamped on the step structure A; in this specific embodiment, four step-type limiting rings 102 are arranged, the outer diameter of the topmost step-type limiting ring 102 is 10mm longer than the inner crucible 1, and the outer diameter of the bottommost step-type limiting ring 102 is 4mm longer than the inner crucible 1, and the diameter decreases from the top to the bottom by 2mm; after the crystal pulling is completed, the corresponding step limiting rings 102 are not damaged or fall off.
  • the net bag limiting structure provided on the outer surface of the inner crucible 1 in this specific embodiment specifically adopts the step structure A shown in the position A in FIG. 7.
  • the step structure A is specifically a single-layer step provided on the outer surface of the inner crucible 1.
  • the depth of the step is 5 mm, that is, the outer diameter of the step structure A before crystal pulling is 955 mm less than the inner diameter of the inner crucible 1 before crystal pulling by 10 mm, that is, 945 mm.
  • the step structure A is located at a height of 3/4 of the upper part of the outer surface of the inner crucible 1.
  • the mesh crucible 2 is directly mounted on the step structure A.
  • the mesh crucible 2 in this specific embodiment specifically adopts the mesh crucible shown in Figure 10; after the crystal pulling is completed, the corresponding step structure A is not damaged or detached.
  • the difference between this specific embodiment and the specific embodiment 1 is that the mesh crucible 2 has only a lower edge seal and a middle mesh woven portion; and in this specific embodiment, the inner crucible 1 is a graphite crucible, and the mesh crucible 2 and the inner crucible 1 are bonded by coating a graphite glue with a mesh bag.
  • the graphite glue is applied with a thickness of 1 mm, which enables the mesh crucible 2 to adhere well after coating.
  • the mesh crucible 2 in this specific embodiment can also adopt the structure of limiting and hanging the mesh crucible 2 by surrounding the protrusion 101 above the outer surface of the inner crucible 1 as in the specific embodiment 1, or adopt the structure of arranging stepped limiting rings 102 in sequence from top to bottom on the outer surface of the inner crucible 1 as in the specific embodiment 2.
  • the middle mesh woven portion is a bowl-shaped structure with an open bottom and no lower edge sealing
  • the mesh crucible 2 in this specific embodiment may also adopt a structure in which the protrusions 101 arranged around the outer surface of the inner crucible 1 are used to limit and suspend the mesh crucible 2 as in the specific embodiment 1, or adopt a structure in which stepped limiting rings 102 are arranged around the outer surface of the inner crucible 1 in sequence from top to bottom as in the specific embodiment 2.
  • the middle mesh woven portion is a straight cylindrical structure;
  • the mesh crucible 2 adopts a structure in which a protrusion 101 arranged around the outer surface of the inner crucible 1 is used to limit and suspend the mesh crucible 2, or adopts a structure in which stepped limiting rings 102 are arranged around the outer surface of the inner crucible 1 from top to bottom in sequence as in the specific embodiment 2.
  • the difference between this specific embodiment and any one of specific embodiments 1-6 is that the inner crucible 1 adopts a split crucible, specifically a three-petal crucible, and the surface of the inner crucible 1 in contact with the mesh crucible 2 is coated with graphite glue to form a whole; this specific embodiment only lists three-petal graphite, carbon-carbon or ceramic crucibles, and of course multi-petal crucibles still fall within the protection scope of this technical solution.
  • the technical solution adopts a mesh crucible sleeved on the outside of the graphite, carbon-carbon or ceramic crucible that wraps the quartz crucible.
  • the mesh crucible is a hollow mesh body formed by weaving carbon fiber ropes to cover the graphite, carbon-carbon or ceramic crucible, and the inner surface is in contact with the outer wall of the graphite, carbon-carbon or ceramic crucible.
  • the crucible that wraps the quartz crucible adopts a two-layer structure, which not only takes advantage of the woven mesh structure to always maintain the structural stability of the graphite, carbon-carbon or ceramic crucible, but also makes it possible to choose a graphite, carbon-carbon or ceramic crucible with a thinner wall thickness than the existing one.
  • the strength of the combined crucible formed by the thin-walled graphite, carbon-carbon or ceramic crucible and the mesh crucible that wraps it is not reduced compared with the original thick-walled graphite, carbon-carbon or ceramic crucible; after the graphite, carbon-carbon or ceramic crucible is corroded to increase its inner diameter or cracks due to thermal expansion, only the inner crucible needs to be replaced, and the mesh crucible can be replaced. It is reusable and has a lower replacement cost than the original thick-walled graphite, carbon-carbon or ceramic crucible.
  • the overall heat conduction efficiency is higher and the heating and cooling time is greatly shortened, which not only reduces the power requirement for the heater but also improves the crystal pulling efficiency.
  • the use of a mesh crucible can facilitate the detachment of the graphite, carbon-carbon or ceramic crucible when it needs to be replaced.
  • the mesh crucible is used to cover and support the inner crucible.
  • the inner crucible adopts a split crucible structure, such as a three-petal or multi-petal crucible, it can not only effectively reduce the impact of thermal expansion, but also has a good overall retention effect.

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

Abstract

A combined crucible and a single crystal furnace using same, relating to the technical field of single crystal silicon manufacturing. The combined crucible comprises an inner crucible sleeved outside a quartz crucible and a mesh crucible used for covering the inner crucible, and the inner crucible is a graphite crucible, a carbon/carbon crucible or a ceramic crucible; the mesh crucible and the inner crucible are bonded using a net bag limiting structure is used or by means of graphite glue; and the mesh crucible is a hollow mesh body formed by weaving one or more carbon fiber ropes and used for covering the graphite, carbon/carbon or ceramic crucible. Compared with the original graphite, carbon/carbon or ceramic crucible having a large thickness, the replacement cost after corrosion damage is low; the mesh crucible can maintain the strength and stable structure of the graphite, carbon/carbon or ceramic crucible; due to the reduction of thickness, the product has higher heat conduction efficiency, improved heating and cooling efficiency, and lower energy consumption; and the mesh crucible can be repeatedly used and is easy to install and remove.

Description

一种组合式坩埚及利用该坩埚的单晶炉Combined crucible and single crystal furnace using the same 技术领域Technical Field
本发明属于单晶硅或多晶硅制造技术领域，特别是涉及一种组合式坩埚以及使用该组合式坩埚的单晶炉。The invention belongs to the technical field of single crystal silicon or polycrystalline silicon manufacturing, and in particular relates to a combined crucible and a single crystal furnace using the combined crucible.
背景技术Background technique
单晶炉是一种在惰性气体环境中，用石墨加热器将多晶硅等多晶材料融化，用直拉法生长无错位单晶的设备。拉晶是指熔融的单质硅在凝固时硅原子以金刚石晶格排列成许多晶核，如果这些晶核长成晶面取向相同的晶粒并平行结合起来便结晶成单晶硅。A single crystal furnace is a device that uses a graphite heater to melt polycrystalline materials such as polycrystalline silicon in an inert gas environment and grows single crystals without dislocation using the Czochralski method. Crystal pulling refers to the process in which the silicon atoms of molten silicon are arranged into many crystal nuclei in a diamond lattice when they solidify. If these crystal nuclei grow into grains with the same crystal plane orientation and combine in parallel, they will crystallize into single crystal silicon.
现有的单晶炉中的坩埚结构是在石英坩埚外包裹石墨、碳碳或陶瓷坩埚，加热器直接加热该石墨、碳碳或陶瓷坩埚使石英坩埚内的硅融化，这一过程中，硅融化后在石英坩埚内会产生大量的一氧化硅，挥发出的一氧化硅被氩气流带到炉体的下方，从排气管排出。一氧化硅流经石墨件时，如石墨、碳碳或陶瓷坩埚、加热器、保温筒等，会与之发生反应生成碳化硅。每次产生的碳化硅经清炉吸除后，无论是石墨、碳碳或陶瓷坩埚还是加热器其原有的厚度都不可避免的减薄了，使用寿命将会不可避免的大大缩减。另外，在单晶炉中使用直拉法制造单晶硅的过程中，由于石墨、碳碳或陶瓷坩埚与包裹的石英坩埚的膨胀系数不同，可能还会导致石墨、碳碳或陶瓷坩埚的龟裂问题。在出现一定程度的龟裂以及内壁腐蚀后，会造成石墨、碳碳或陶瓷坩埚的报废。随着单晶硅生长的晶体直径越来越粗，相应的单晶炉的直径也越做越大，对于热场的可靠性要求也越来越高，对应地，石墨、碳碳或陶瓷坩埚壁厚增大、重量增加，进而要求加热器加大功率提高加热温度以达到石英坩埚内硅液热熔温度的要求，这都导致耗能增加以及石墨、碳碳或陶瓷坩埚的制造成本提升。为此专利号为200910118210.X公开了一种中空网状体的石英坩埚保持件，其加入了粘结剂、高温碳化、气相沉积的加工步骤，其直接套设于石英坩埚的外部并对石英坩埚进行保持，但是其仍然没有解决对应的自身坩埚保持件本体易被腐蚀的问题，一经腐蚀后便可造成保持件整体的报废，使用成本依旧很高。 The crucible structure in the existing single crystal furnace is to wrap a graphite, carbon-carbon or ceramic crucible outside a quartz crucible, and the heater directly heats the graphite, carbon-carbon or ceramic crucible to melt the silicon in the quartz crucible. In this process, a large amount of silicon monoxide will be produced in the quartz crucible after the silicon melts. The volatilized silicon monoxide is carried to the bottom of the furnace body by the argon flow and discharged from the exhaust pipe. When silicon monoxide flows through graphite parts, such as graphite, carbon-carbon or ceramic crucibles, heaters, insulation tubes, etc., it will react with them to form silicon carbide. After each generation of silicon carbide is removed by furnace cleaning, the original thickness of the graphite, carbon-carbon or ceramic crucible or the heater will inevitably be thinned, and the service life will inevitably be greatly reduced. In addition, in the process of using the Czochralski method to manufacture single crystal silicon in a single crystal furnace, due to the different expansion coefficients of the graphite, carbon-carbon or ceramic crucible and the wrapped quartz crucible, it may also cause cracking problems in the graphite, carbon-carbon or ceramic crucible. After a certain degree of cracking and inner wall corrosion, the graphite, carbon-carbon or ceramic crucible will be scrapped. As the diameter of the crystals of single crystal silicon grows thicker and thicker, the diameter of the corresponding single crystal furnace is also getting larger and larger, and the reliability requirements for the thermal field are also getting higher and higher. Correspondingly, the wall thickness and weight of the graphite, carbon-carbon or ceramic crucibles increase, and the heater is required to increase the power and increase the heating temperature to meet the requirements of the hot melting temperature of the silicon liquid in the quartz crucible, which leads to increased energy consumption and increased manufacturing costs of graphite, carbon-carbon or ceramic crucibles. For this reason, patent No. 200910118210.X discloses a hollow mesh quartz crucible holder, which is added with a binder, high-temperature carbonization, and vapor deposition processing steps. It is directly sleeved on the outside of the quartz crucible and holds the quartz crucible, but it still does not solve the problem that the corresponding crucible holder body is easily corroded. Once corroded, the holder can be scrapped as a whole, and the cost of use is still very high.
发明内容Summary of the invention
本发明提供了一种组合式坩埚及利用该坩埚的单晶炉，解决了以上问题。The present invention provides a combined crucible and a single crystal furnace using the crucible, which solves the above problems.
为解决上述技术问题，本发明是通过以下技术方案实现的：To solve the above technical problems, the present invention is achieved through the following technical solutions:
本发明的一种组合式坩埚，包括套设于石英坩埚外部的内坩埚以及用于对内坩埚进行兜覆的网状坩埚，所述内坩埚采用石墨坩埚、碳碳坩埚或陶瓷坩埚；A combined crucible of the present invention comprises an inner crucible sleeved on the outside of a quartz crucible and a mesh crucible for covering the inner crucible, wherein the inner crucible is a graphite crucible, a carbon-carbon crucible or a ceramic crucible;
进一步地，网状坩埚与内坩埚之间采用网兜限位结构或通过石墨胶相粘接。Furthermore, the mesh crucible and the inner crucible are bonded together by a mesh bag limiting structure or by graphite glue.
进一步地，所述网兜限位结构包括利用设置于内坩埚外表面的凸起挂住网状坩埚或利用设置于内坩埚外表面的台阶结构卡接住网状坩埚；所述台阶结构的深度为1-10mm；所述凸起的厚度为1-10mm。Furthermore, the net bag limiting structure includes using a protrusion arranged on the outer surface of the inner crucible to hang the mesh crucible or using a step structure arranged on the outer surface of the inner crucible to clamp the mesh crucible; the depth of the step structure is 1-10mm; the thickness of the protrusion is 1-10mm.
进一步地，所述内坩埚采用整体式坩埚或分体式坩埚，所述分体式坩埚包括多瓣式坩埚。Furthermore, the inner crucible is a one-piece crucible or a split crucible, and the split crucible includes a multi-petal crucible.
进一步地，所述网状坩埚是由一根或多根碳纤维绳编织形成的对内坩埚进行兜覆的中空网状体，其内表面与内坩埚外表面相贴合。Furthermore, the mesh crucible is a hollow mesh body formed by weaving one or more carbon fiber ropes to cover the inner crucible, and the inner surface of the mesh crucible is in contact with the outer surface of the inner crucible.
进一步地，所述网状坩埚具体为碗状或直筒状，底部设有开口或由碳纤维绳编织覆盖，所述网状坩埚的顶部为开口。Furthermore, the mesh crucible is specifically bowl-shaped or straight-cylindrical, with an opening at the bottom or covered by woven carbon fiber ropes, and the top of the mesh crucible is an opening.
进一步地，所述网状坩埚的碳纤维绳表面包覆或填充有沉积碳层或硬化物质层。Furthermore, the surface of the carbon fiber rope of the mesh crucible is coated or filled with a deposited carbon layer or a hardened material layer.
进一步地，陶瓷坩埚的材料包括氮化硼、碳化硅、碳化钨、氧化锆、氧化铝、氮化铝、二硼化钛、碳化鉿中任意一种或多种混合。Furthermore, the material of the ceramic crucible includes any one or more of boron nitride, silicon carbide, tungsten carbide, zirconium oxide, aluminum oxide, aluminum nitride, titanium diboride, and tungsten carbide.
一种单晶炉，包括上述的组合式坩埚。A single crystal furnace comprises the above-mentioned combined crucible.
一种拉晶方法，采用所述单晶炉进行拉晶的方法。A crystal pulling method, which uses the single crystal furnace to pull crystals.
本发明相对于现有技术包括有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
(1)本技术方案将坩埚分为内坩埚和网状坩埚两层式结构，采用在包裹石英坩埚的石墨、碳碳或陶瓷坩埚外部套设网状坩埚，该网状坩埚是由碳纤维绳编织形成的对石墨、碳碳或陶瓷坩埚进行兜覆的中空网状体，其内表面与石墨、碳碳或陶瓷坩埚的外壁相贴合；该网状坩埚能够时刻保持石墨、碳碳或陶瓷坩埚的结构稳定性，使选择比现有壁厚更薄的石墨、碳碳或陶瓷坩埚成为可能，薄壁石墨、碳碳或陶瓷坩埚和包裹其的外网状坩埚形成的组合坩埚的强度与原厚壁单层 石墨、碳碳或陶瓷坩埚相比没有下降；(1) The technical solution divides the crucible into a two-layer structure of an inner crucible and a mesh crucible, and adopts a mesh crucible that is sleeved on the outside of a graphite, carbon-carbon or ceramic crucible that wraps a quartz crucible. The mesh crucible is a hollow mesh body formed by weaving carbon fiber ropes to cover the graphite, carbon-carbon or ceramic crucible, and its inner surface fits the outer wall of the graphite, carbon-carbon or ceramic crucible; the mesh crucible can always maintain the structural stability of the graphite, carbon-carbon or ceramic crucible, making it possible to select a graphite, carbon-carbon or ceramic crucible with a thinner wall thickness than the existing one. The strength of the combined crucible formed by the thin-walled graphite, carbon-carbon or ceramic crucible and the outer mesh crucible wrapping it is comparable to that of the original thick-walled single-layer There is no decrease compared to graphite, carbon-carbon or ceramic crucibles;
(2)本技术方案采用内坩埚和网状坩埚两层式结构，在内坩埚被腐蚀导致内径变大或者由于热膨胀导致龟裂后，只需对内坩埚进行更换，网状坩埚可重复使用，相对于原厚壁单层石墨、碳碳或陶瓷坩埚，更换成本更低；(2) The technical solution adopts a two-layer structure of an inner crucible and a mesh crucible. When the inner crucible is corroded and the inner diameter becomes larger or cracks due to thermal expansion, only the inner crucible needs to be replaced, and the mesh crucible can be reused. Compared with the original thick-walled single-layer graphite, carbon-carbon or ceramic crucible, the replacement cost is lower;
(3)本技术方案采用内坩埚和网状坩埚两层式结构其内坩埚相对于原有的厚壁单层坩埚壁厚降低，且网状坩埚是镂空形式，总体热传导效率变高，加热和冷却时间大大缩短，不仅对于加热器所需的功率要求更低，还可以提升拉晶效率；(3) The technical solution adopts a two-layer structure of an inner crucible and a mesh crucible. The inner crucible has a thinner wall than the original thick-walled single-layer crucible, and the mesh crucible is hollow. The overall heat conduction efficiency is improved, and the heating and cooling time is greatly shortened. Not only is the power requirement for the heater lower, but the crystal pulling efficiency can also be improved.
(4)本技术方案采用网状坩埚能够使石墨、碳碳或陶瓷坩埚需要更换时便于脱离；(4) The mesh crucible used in this technical solution can facilitate the detachment of graphite, carbon-carbon or ceramic crucibles when they need to be replaced;
(5)本技术方案采用网状坩埚对内坩埚进行兜覆支撑的组合结构，当内坩埚可采用分体式坩埚结构时，如三瓣式或多瓣式坩埚，不仅可以有效降低热膨胀带来的影响，且具有良好的整体保持效果。(5) The technical solution adopts a combined structure in which a mesh crucible is used to cover and support the inner crucible. When the inner crucible can adopt a split crucible structure, such as a three-petal or multi-petal crucible, it can not only effectively reduce the impact of thermal expansion, but also has a good overall retention effect.
(6)本技术方案的内坩埚和网状坩埚组成的两层式结构，两层之间采用网兜限位结构或通过石墨胶相粘接，其中网兜限位结构具体包括设置于内坩埚外表面的凸起挂住网状坩埚或利用设置于内坩埚外表面的台阶结构卡接住网状坩埚，凸起和台阶结构样式简单，能够使网状坩埚很好的与内坩埚相结合，安装拆卸简单便捷。(6) The two-layer structure composed of the inner crucible and the mesh crucible of the technical solution is a mesh bag limiting structure or bonding the two layers by graphite glue, wherein the mesh bag limiting structure specifically includes a protrusion arranged on the outer surface of the inner crucible to hang the mesh crucible or a step structure arranged on the outer surface of the inner crucible to clamp the mesh crucible. The protrusion and step structure are simple in style, which can make the mesh crucible well combined with the inner crucible, and the installation and disassembly are simple and convenient.
当然，实施本发明的任一产品并不一定需要同时达到以上所述的所有优点。Of course, any product implementing the present invention does not necessarily need to achieve all of the above-mentioned advantages at the same time.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for describing the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
图1为本发明具体实施例1的一种组合式坩埚的结构示意图；FIG1 is a schematic structural diagram of a combined crucible according to a specific embodiment 1 of the present invention;
图2为图1中网状坩埚的结构示意图；FIG2 is a schematic structural diagram of the mesh crucible in FIG1 ;
图3为图1中材质为石墨、碳碳或陶瓷坩埚的内坩埚结构示意图；FIG3 is a schematic diagram of the structure of an inner crucible in FIG1 made of graphite, carbon-carbon or ceramic crucible;
图4为具体实施例2的组合式坩埚的结构示意图；FIG4 is a schematic structural diagram of a combined crucible according to a specific embodiment 2;
图5为图4中内坩埚的结构示意图； FIG5 is a schematic structural diagram of the inner crucible in FIG4 ;
图6为具体实施例3的组合式坩埚的结构示意图；FIG6 is a schematic structural diagram of a combined crucible according to a specific embodiment 3;
图7为图6中对应的带有台阶结构的内坩埚的结构示意图；FIG7 is a schematic structural diagram of an inner crucible with a step structure corresponding to FIG6 ;
图8为具体实施例4的网状坩埚的结构示意图；FIG8 is a schematic structural diagram of a mesh crucible according to a specific embodiment 4;
图9为具体实施例5的网状坩埚的结构示意图；FIG9 is a schematic structural diagram of a mesh crucible of specific embodiment 5;
图10为具体实施例6的网状坩埚的结构示意图；FIG10 is a schematic structural diagram of a mesh crucible of specific embodiment 6;
图11为具体实施例7的三瓣式石墨、碳碳或陶瓷坩埚的结构示意图；FIG11 is a schematic diagram of the structure of a three-petal graphite, carbon-carbon or ceramic crucible of specific embodiment 7;
图12为应用图11中三瓣式石墨、碳碳或陶瓷坩埚的组合式坩埚的结构示意图；FIG12 is a schematic diagram of the structure of a combined crucible using the three-petal graphite, carbon-carbon or ceramic crucible in FIG11;
图13为碳纤维绳的编织方式示意图之一；FIG13 is a schematic diagram of one of the braiding methods of the carbon fiber rope;
图14为碳纤维绳的编织方式示意图之二；FIG14 is a second schematic diagram of the braiding method of the carbon fiber rope;
图15为碳纤维绳的编织方式示意图之三；FIG15 is a third schematic diagram of the braiding method of the carbon fiber rope;
图16为碳纤维绳的编织方式示意图之四；FIG16 is a fourth schematic diagram of the braiding method of the carbon fiber rope;
图17为碳纤维绳的编织方式示意图之五；FIG17 is a fifth schematic diagram of the braiding method of the carbon fiber rope;
图18为另一种碳纤维绳的编织方式示意图；FIG18 is a schematic diagram of another braiding method of a carbon fiber rope;
图19为本发明的组合式坩埚安装于单晶炉内的结构示意图；FIG19 is a schematic diagram of the structure of the combined crucible of the present invention installed in a single crystal furnace;
图20为现有的单晶炉内的结构示意图；FIG20 is a schematic diagram of the structure of an existing single crystal furnace;
附图中，各标号所代表的部件列表如下：
1-内坩埚，101-凸起，102-台阶式限位环，2-网状坩埚，A-台阶结构。In the accompanying drawings, the components represented by the reference numerals are listed as follows:
1-inner crucible, 101-protrusion, 102-stepped limiting ring, 2-mesh crucible, A-step structure.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
在本发明的描述中，需要理解的是，术语“间隙”、“内表面”、“外表面”、“顶部”、“底部”等指示方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的组件或元件必须具有特定的方位，以特定的方位构造和操作，因此不能理解为对本发明的限制。In the description of the present invention, it is necessary to understand that the terms "gap", "inner surface", "outer surface", "top", "bottom" and the like indicating orientation or positional relationship are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the components or elements referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore should not be understood as limiting the present invention.
如图20所示，为现有的采用石墨、碳碳或陶瓷坩埚的单晶炉的内部结构示 意图，由图中可以看到其采用的是壁厚较厚且质量较重的单层整体式的石墨、碳碳或陶瓷坩埚包裹于石英坩埚外部，因为石墨、碳碳或陶瓷坩埚与石英坩埚之间热膨胀系数不一致，会导致石墨、碳碳或陶瓷坩埚的龟裂，加之长期使用过程中，一氧化硅对石墨、碳碳或陶瓷坩埚与石英坩埚接触面的腐蚀，会导致整个石墨、碳碳或陶瓷坩埚内表面的进一步腐蚀，内径扩大，直至报废，使用成本高；另外，由于石墨、碳碳或陶瓷坩埚厚度大，对石英坩埚内的硅进行加热需要使用较高的热量，导致对加热器的功率要求较高，能耗成本高。As shown in FIG. 20 , the internal structure of a single crystal furnace using a graphite, carbon-carbon or ceramic crucible is shown. As can be seen from the figure, a single-layer integral graphite, carbon-carbon or ceramic crucible with thicker walls and heavier mass is used to wrap the outside of the quartz crucible. Because the thermal expansion coefficients of the graphite, carbon-carbon or ceramic crucible and the quartz crucible are inconsistent, the graphite, carbon-carbon or ceramic crucible will crack. In addition, during long-term use, the corrosion of the contact surface between the graphite, carbon-carbon or ceramic crucible and the quartz crucible by silicon monoxide will cause further corrosion of the inner surface of the entire graphite, carbon-carbon or ceramic crucible, and the inner diameter will expand until it is scrapped, with high cost of use. In addition, due to the large thickness of the graphite, carbon-carbon or ceramic crucible, a higher amount of heat is required to heat the silicon in the quartz crucible, resulting in a higher power requirement for the heater and high energy consumption cost.
请参阅图1-18所示，本发明的一种组合式坩埚，包括套设于石英坩埚外部的内坩埚1以及用于对内坩埚1进行兜覆的网状坩埚2，内坩埚1采用石墨坩埚、碳碳坩埚或陶瓷坩埚；上述网状坩埚2与内坩埚1之间采用网兜限位结构或通过石墨胶相粘接；网兜限位结构包括利用设置于内坩埚1外表面的凸起101挂住网状坩埚2或利用设置于内坩埚1外表面的台阶结构A卡接住网状坩埚2；Please refer to FIG. 1-18 , a combined crucible of the present invention comprises an inner crucible 1 sleeved on the outside of a quartz crucible and a mesh crucible 2 for covering the inner crucible 1, wherein the inner crucible 1 is made of graphite crucible, carbon-carbon crucible or ceramic crucible; a mesh bag limiting structure is used between the mesh crucible 2 and the inner crucible 1 or the mesh crucible 2 is bonded with graphite glue; the mesh bag limiting structure comprises a protrusion 101 provided on the outer surface of the inner crucible 1 to hang the mesh crucible 2 or a step structure A provided on the outer surface of the inner crucible 1 to clamp the mesh crucible 2;
内坩埚1采用整体式坩埚或分体式坩埚，分体式坩埚包括多瓣式坩埚；本技术方案中的内坩埚1无需采用壁厚较厚的石墨、碳碳或陶瓷坩埚，相对于现有的石墨、碳碳或陶瓷坩埚的壁厚为20mm，本技术方案中的内坩埚1的厚度可采用5mm、8mm或10mm，在具体厚度上大大减小，并带来重量及制造成本的降低。The inner crucible 1 adopts an integral crucible or a split crucible, and the split crucible includes a multi-petal crucible. The inner crucible 1 in the present technical solution does not need to adopt a graphite, carbon-carbon or ceramic crucible with a thicker wall thickness. Compared with the existing graphite, carbon-carbon or ceramic crucibles with a wall thickness of 20 mm, the thickness of the inner crucible 1 in the present technical solution can be 5 mm, 8 mm or 10 mm, which greatly reduces the specific thickness and brings about a reduction in weight and manufacturing cost.
网状坩埚2是由一根或多根碳纤维绳编织形成的对内坩埚1进行兜覆的中空网状体，其内表面与内坩埚1外表面相贴合。网状坩埚2具体为碗状或直筒状，底部设有开口或由碳纤维绳编织覆盖，网状坩埚2的顶部为开口；作为一种具体实施例，网状坩埚2的碳纤维绳表面可进行包覆或填充有沉积碳层或硬化物质层；硬化物质层具体包括碳化硅、氮化硅或者其它的陶瓷材料；网状坩埚2的厚度大于等于1mm，优选5-18mm；内坩埚1为石墨、碳碳或陶瓷坩埚，其厚度大于等于1mm，优选5-10mm；采用陶瓷坩埚时，陶瓷坩埚的材料包括氮化硼、碳化硅、碳化钨、氧化锆、氧化铝、氮化铝、二硼化钛、碳化鉿中任意一种或多种混合；The mesh crucible 2 is a hollow mesh body formed by weaving one or more carbon fiber ropes to cover the inner crucible 1, and its inner surface is in contact with the outer surface of the inner crucible 1. The mesh crucible 2 is specifically bowl-shaped or straight-cylindrical, with an opening at the bottom or covered by woven carbon fiber ropes, and the top of the mesh crucible 2 is an opening; as a specific embodiment, the surface of the carbon fiber rope of the mesh crucible 2 can be coated or filled with a deposited carbon layer or a hardened material layer; the hardened material layer specifically includes silicon carbide, silicon nitride or other ceramic materials; the thickness of the mesh crucible 2 is greater than or equal to 1mm, preferably 5-18mm; the inner crucible 1 is a graphite, carbon-carbon or ceramic crucible, and its thickness is greater than or equal to 1mm, preferably 5-10mm; when a ceramic crucible is used, the material of the ceramic crucible includes any one or more of boron nitride, silicon carbide, tungsten carbide, zirconium oxide, aluminum oxide, aluminum nitride, titanium diboride, and arsenic carbide;
网状坩埚2使用的一根或多根碳纤维绳编织形成，其中，其网状坩埚2的具体结构形式如图2以及图8-10所示，包括如图2所示的带有上封边、下封边及中部中空网形成的坩埚型网状结构，该结构中底部可设置为开口孔或编织绳进行兜底；如图8所示的仅带有中部中空网以及底部为下封边的碗状结构，此时结构中底部可设置为开口孔或编织绳进行兜底；如图9所示，为仅带有中部中空网底 部为开口的碗状结构；如图10所示，为仅带有中部中空网的直筒型结构；The mesh crucible 2 is formed by weaving one or more carbon fiber ropes, wherein the specific structural form of the mesh crucible 2 is shown in FIG. 2 and FIG. 8-10, including a crucible-type mesh structure with an upper edge seal, a lower edge seal and a middle hollow net as shown in FIG. 2, in which the bottom can be set as an open hole or a braided rope for bottoming; a bowl-shaped structure with only a middle hollow net and a bottom with a lower edge seal as shown in FIG. 8, in which case the bottom can be set as an open hole or a braided rope for bottoming; as shown in FIG. 9, a bowl-shaped structure with only a middle hollow net bottom The first part is an open bowl-shaped structure; as shown in FIG10 , it is a straight cylindrical structure with only a hollow net in the middle;
本技术方案的组合式坩埚，采用网状坩埚2包裹于内坩埚1的外表面的形式，相对于同尺寸和厚度的普通石墨坩埚或碳碳坩埚的六个使用周期，一个周期为400小时，多增加2个使用周期，大大提高了坩埚的使用期限并节省了成本。相对于普通同等15mm厚度且尺寸为36寸的整体式石墨坩埚，本技术方案中采用13mm厚度的石墨内坩埚1以及2mm厚度的网状坩埚2，本技术方案的内坩埚1由拉晶前的内径为951mm，在拉晶结束后，膨胀为953mm，而普通的整体式的石墨内坩埚1由拉晶前的内径为951mm，在拉晶结束后，膨胀为954mm，本技术方案的坩埚结构膨胀度更小；The combined crucible of the present technical solution adopts the form of a mesh crucible 2 wrapped around the outer surface of the inner crucible 1. Compared with the six use cycles of ordinary graphite crucibles or carbon-carbon crucibles of the same size and thickness, one cycle is 400 hours, which adds 2 more use cycles, greatly improving the service life of the crucible and saving costs. Compared with the ordinary monolithic graphite crucible of the same thickness of 15mm and size of 36 inches, the present technical solution adopts a 13mm thick graphite inner crucible 1 and a 2mm thick mesh crucible 2. The inner diameter of the inner crucible 1 of the present technical solution is 951mm before crystal pulling, and expands to 953mm after the crystal pulling is completed, while the inner diameter of the ordinary monolithic graphite inner crucible 1 is 951mm before crystal pulling, and expands to 954mm after the crystal pulling is completed. The crucible structure of the present technical solution has a smaller expansion degree;
并且，对应的网状坩埚2中一根或多根碳纤维绳的编织的方式具体如图13-18所示，具体的包括：如图13所示，碳纤维绳的每一根均包含多根碳纤维纱线，绳子的中心为平行于绳子轴心的碳纤维纱线，平行于轴心的碳纤维纱线外面包覆碳纤维编织管；封边部和下封边部为环形体，由一根或多根所述碳纤维绳编织而成，上封边部和下封边部的编织方法和中环部的编织方法不同，上封边部和下封边部的编织密度比中环部的编织密度大；中环部的网状体由一根或多根碳纤维绳沿相对于所述中心轴倾斜第一角度的第一方向对齐；由一根或多根碳纤维绳沿相对于所述中心轴倾斜第二角度的第二方向对齐；第二角度与所述第一角度相同，并且其中第一方向与第二方向相对于所述中心轴对称。此实施例的编织方式我们称之为交叉编织方式；又如图13-18所示，为对应的上封边以及下封边的编织的各种编织方式，通过一根或多跟碳纤维绳编织形成。又如图18所示，为另一种编织方式，编织形成网状坩埚2为仅带有中部为直筒状结构，中环部包括多数根轴向条，一根或多根所述碳纤维绳绕所述轴向条螺旋编织，轴向条与所述碳纤维绳螺旋编织方向的夹角为大于70度小于90度。此实施例的编织方式我们称之为螺旋编织方式。螺旋编织时，中环部包括多数根轴向条的支撑，可以没有封边部。In addition, the braiding method of one or more carbon fiber ropes in the corresponding mesh crucible 2 is specifically shown in Figures 13-18, specifically including: as shown in Figure 13, each of the carbon fiber ropes contains multiple carbon fiber yarns, the center of the rope is a carbon fiber yarn parallel to the axis of the rope, and the carbon fiber yarn parallel to the axis is coated with a carbon fiber braided tube; the edge sealing part and the lower edge sealing part are annular bodies, woven from one or more of the carbon fiber ropes, the braiding method of the upper edge sealing part and the lower edge sealing part is different from the braiding method of the middle ring part, and the braiding density of the upper edge sealing part and the lower edge sealing part is greater than the braiding density of the middle ring part; the mesh body of the middle ring part is aligned along a first direction inclined at a first angle relative to the central axis by one or more carbon fiber ropes; aligned along a second direction inclined at a second angle relative to the central axis by one or more carbon fiber ropes; the second angle is the same as the first angle, and the first direction and the second direction are symmetrical relative to the central axis. The braiding method of this embodiment is called a cross braiding method; as shown in Figures 13-18, it is various braiding methods for braiding the corresponding upper and lower edge sealing parts, which are braided by one or more carbon fiber ropes. As shown in FIG. 18, another weaving method is used to weave the mesh crucible 2 with only a straight cylindrical structure in the middle, the middle ring portion includes a plurality of axial bars, one or more carbon fiber ropes are spirally woven around the axial bars, and the angle between the axial bars and the spiral weaving direction of the carbon fiber rope is greater than 70 degrees and less than 90 degrees. The weaving method of this embodiment is called a spiral weaving method. When spirally weaving, the middle ring portion includes the support of a plurality of axial bars, and there may be no edge sealing portion.
网状坩埚2具体是将30k根碳纤维束加捻成碳纤维绳，预浸树脂后再编织成条状织物作为碳纤维绳，该树脂具体为环氧树脂，本具体实施例中环氧树脂的质量为碳纤维束或碳纤维绳与树脂总质量的6％；然后按照上述编织方法和造型编织成网状，获得如上述编织造型的碳纤维网状体，然后将获得的碳纤维网状体经 过模具辅助固化形成碳纤维网状预制体，其中固化定形条件为：固化温度为200℃，时间为6h，升温速率为8℃/min；模具采用本领域常见的石墨模具，该模具与内坩埚造型一致；去除模具后，然后进行气相沉积，将获得的碳纤维网状预制体放入沉积炉中，在1000℃温度下，通入三氯甲基硅烷，并以氢气为载气和稀释气体，三氯甲基硅烷与氢气流量比为1∶3；沉积25h获得所需的网状坩埚2；通过将网状坩埚2与内坩埚1相组合的方式使得整体的组合式坩埚相对于现有的单独的内坩埚在使用时，具有更优的结构强度，不易因热膨胀而产生龟裂。The mesh crucible 2 is specifically made by twisting 30k carbon fiber bundles into a carbon fiber rope, pre-impregnating the carbon fiber rope with resin, and then weaving it into a strip fabric as a carbon fiber rope. The resin is specifically epoxy resin. In this specific embodiment, the mass of the epoxy resin is 6% of the total mass of the carbon fiber bundle or the carbon fiber rope and the resin; then weaving it into a mesh according to the above-mentioned weaving method and shape to obtain a carbon fiber mesh body as the above-mentioned weaving shape, and then the obtained carbon fiber mesh body is A carbon fiber mesh preform is formed by die-assisted curing, wherein the curing and shaping conditions are: a curing temperature of 200°C, a time of 6 hours, and a heating rate of 8°C/min; the mold adopts a common graphite mold in the field, and the mold is consistent with the shape of the inner crucible; after removing the mold, vapor deposition is then carried out, and the obtained carbon fiber mesh preform is placed in a deposition furnace, and trichloromethylsilane is introduced at a temperature of 1000°C, and hydrogen is used as a carrier gas and a dilution gas, and the flow ratio of trichloromethylsilane to hydrogen is 1:3; the desired mesh crucible 2 is obtained by deposition for 25 hours; by combining the mesh crucible 2 with the inner crucible 1, the overall combined crucible has better structural strength than the existing single inner crucible when in use, and is not prone to cracking due to thermal expansion.
作为构成碳纤维绳的碳纤维，可以使用沥青基碳纤维、PAN基碳纤维、黏胶基碳纤维等。构成碳纤维绳的碳纤维可以为相同材料或不同材料。与现有技术的坩埚相比，本申请的网状坩埚2采用碳纤维复合材料的碳纤维绳编织，不需要制作胚体，网状坩埚2的形状不受胚体的限制，可以灵活设计，由于原料规格统一，可以批量生产，提高纤维绳生产效率，缩短网状坩埚制造工时，所以成本较低，交货周期短，易于供应。As the carbon fiber constituting the carbon fiber rope, asphalt-based carbon fiber, PAN-based carbon fiber, viscose-based carbon fiber, etc. can be used. The carbon fibers constituting the carbon fiber rope can be the same material or different materials. Compared with the crucible in the prior art, the mesh crucible 2 of the present application is woven with a carbon fiber rope made of a carbon fiber composite material, and does not need to make an embryo. The shape of the mesh crucible 2 is not limited by the embryo and can be flexibly designed. Due to the uniform specifications of the raw materials, it can be mass-produced, improve the production efficiency of the fiber rope, and shorten the manufacturing time of the mesh crucible, so the cost is low, the delivery cycle is short, and it is easy to supply.
如图19所示，一种单晶炉，包括带有上述技术特征的组合式坩埚，安装于单晶炉的内炉腔内；As shown in FIG19 , a single crystal furnace includes a combined crucible with the above technical features, which is installed in the inner furnace cavity of the single crystal furnace;
一种拉晶方法，其具体是使用该组合式坩埚的拉晶方法。The invention discloses a crystal pulling method, in particular a crystal pulling method using the combined crucible.
具体实施例1：Specific embodiment 1:
如图1-3所示，该组合式坩埚的网状坩埚2具体采用带有上封边和下封边以及中部网状编织部的网状坩埚2结构，上封边和下封边具体如上述编织方式中的任意一种；并且该具体实施例中的内坩埚1具体采用整体式石墨、碳碳或陶瓷坩埚，其高度与网状坩埚2的高度一致；As shown in FIGS. 1-3 , the mesh crucible 2 of the combined crucible specifically adopts a mesh crucible 2 structure with an upper sealing edge, a lower sealing edge and a middle mesh woven portion, and the upper sealing edge and the lower sealing edge are specifically any one of the above-mentioned weaving methods; and the inner crucible 1 in the specific embodiment specifically adopts a monolithic graphite, carbon-carbon or ceramic crucible, and its height is consistent with the height of the mesh crucible 2;
并且，对应的本具体实施例中，内坩埚1外表面设置有网兜限位结构，该网兜限位结构具体采用环绕设置于内坩埚1外面表面上方的凸起101对网状坩埚2进行限位悬挂，使内坩埚1外周侧面的凸起101与网状坩埚2上部的网兜孔相对应实现悬挂，凸起101的数量非限制，本具体实施例中采用环绕布置且与单排网兜孔数量及位置相对应，或与单排网兜孔间隙对应布置，本具体实施例中凸起101的形状为三角形，采用每50mm间距设置一个凸起101，当然圆形、四边形或其它多边形同样能够产生相同的技术效果，应当也属于本技术方案的保护范围；凸出后对网状坩埚2进行吊挂限位；凸起101的厚度为5mm，本具体实施例中 仅列举了一个厚度数据，而采用1-10mm中任意厚度均能够达到相同的技术效果，能够将网状坩埚2很好的与内坩埚1上进行牢固的固定结合，应当均属于本技术方案的保护范围。In addition, in the corresponding specific embodiment of the present invention, a mesh bag limiting structure is provided on the outer surface of the inner crucible 1. The mesh bag limiting structure specifically adopts a protrusion 101 arranged around the upper surface of the outer surface of the inner crucible 1 to limit and suspend the mesh crucible 2, so that the protrusions 101 on the outer peripheral side of the inner crucible 1 correspond to the mesh bag holes on the upper part of the mesh crucible 2 to achieve suspension. The number of protrusions 101 is not limited. In the present specific embodiment, a surrounding arrangement is adopted and corresponds to the number and position of a single row of mesh bag holes, or is arranged corresponding to the gap between the single row of mesh bag holes. In the present specific embodiment, the shape of the protrusion 101 is a triangle, and a protrusion 101 is arranged at a spacing of 50 mm. Of course, a circle, a quadrilateral or other polygon can also produce the same technical effect, and should also belong to the protection scope of the present technical solution; after protruding, the mesh crucible 2 is suspended and limited; the thickness of the protrusion 101 is 5 mm, in the present specific embodiment Only one thickness data is listed, and any thickness in the range of 1-10 mm can achieve the same technical effect, and the mesh crucible 2 can be well and firmly fixed to the inner crucible 1, which should all fall within the protection scope of the present technical solution.
具体实施例2：Specific embodiment 2:
如图4-5所示，本具体实施例相对于具体实施例1的区别在于，本具体实施例的内坩埚1外表面设置的网兜限位结构具体采用台阶结构A，该台阶结构A具体为内坩埚1的外表面由上至下依次间距环绕布置台阶式限位环102，台阶式限位环102的直径由上至下依次减小，使网状坩埚2上部等直径的网兜结构能够卡接夹持于台阶结构A上；本具体实施例中，台阶式限位环102设置四道，最上层的台阶式限位环102的外直径相对于内坩埚1长10mm，最底层的台阶式限位环102的外直径相对于内坩埚1长4mm，由最上层至最下层依次按照2mm的直径依次递减；在拉晶结束后，对应的台阶限位环102并没有损坏或脱落。As shown in Figures 4-5, the difference between this specific embodiment and specific embodiment 1 is that the mesh bag limiting structure arranged on the outer surface of the inner crucible 1 of this specific embodiment specifically adopts a step structure A, and the step structure A is specifically that the outer surface of the inner crucible 1 is arranged with step-type limiting rings 102 in sequence from top to bottom, and the diameter of the step-type limiting rings 102 decreases from top to bottom, so that the mesh bag structure of the same diameter on the upper part of the mesh crucible 2 can be clamped on the step structure A; in this specific embodiment, four step-type limiting rings 102 are arranged, the outer diameter of the topmost step-type limiting ring 102 is 10mm longer than the inner crucible 1, and the outer diameter of the bottommost step-type limiting ring 102 is 4mm longer than the inner crucible 1, and the diameter decreases from the top to the bottom by 2mm; after the crystal pulling is completed, the corresponding step limiting rings 102 are not damaged or fall off.
具体实施例3：Specific embodiment 3:
如图6-7所示，本具体实施例中的内坩埚1外表面设置的网兜限位结构具体采用如图7中A位置所显示的台阶结构A，该台阶结构A具体为内坩埚1外表面上设置有单层台阶，如图7所示，台阶的深度为5mm，即台阶结构A的在拉晶前的外直径相对于内坩埚1由拉晶前的内径为955mm小10mm，即为945mm，本具体实施例中台阶结构A位于内坩埚1外表面上部的3/4高度的位置，本具体实施例中仅列举了一个深度数据，而采用1-10mm中任意深度，以及位于内坩埚1外表面其它位置的高度也能够达到相同的技术效果，能够将网状坩埚2很好的与内坩埚1上进行牢固的固定结合，因此其它能够产生相同技术效果的尺寸和数据应当均属于本技术方案的保护范围，应当均属于本技术方案的保护范围，将网状坩埚2直接套设于台台阶结构A上，本具体实施例中的网状坩埚2具体采用如图10所示的网状坩埚；在拉晶结束后，对应的台阶结构A并没有损坏或脱离。As shown in FIGS. 6-7, the net bag limiting structure provided on the outer surface of the inner crucible 1 in this specific embodiment specifically adopts the step structure A shown in the position A in FIG. 7. The step structure A is specifically a single-layer step provided on the outer surface of the inner crucible 1. As shown in FIG. 7, the depth of the step is 5 mm, that is, the outer diameter of the step structure A before crystal pulling is 955 mm less than the inner diameter of the inner crucible 1 before crystal pulling by 10 mm, that is, 945 mm. In this specific embodiment, the step structure A is located at a height of 3/4 of the upper part of the outer surface of the inner crucible 1. In this specific embodiment, only one depth data is listed, and The same technical effect can be achieved by using any depth of 1-10 mm, as well as heights at other positions on the outer surface of the inner crucible 1, and the mesh crucible 2 can be firmly fixed to the inner crucible 1. Therefore, other dimensions and data that can produce the same technical effect should all belong to the protection scope of the present technical solution. The mesh crucible 2 is directly mounted on the step structure A. The mesh crucible 2 in this specific embodiment specifically adopts the mesh crucible shown in Figure 10; after the crystal pulling is completed, the corresponding step structure A is not damaged or detached.
具体实施例4：Specific embodiment 4:
如图8所示，该具体实施例相对于具体实施例1的区别在于，网状坩埚2仅具有下封边以及中部网状编织部；并且本具体实施例中，内坩埚1采用石墨坩埚，网状坩埚2与内坩埚1之间采用的是网兜后涂覆石墨胶的方式实现粘接，本具体实施例中石墨胶的涂刷厚度为1mm，涂覆后能够使网状坩埚2很好的粘附 于内坩埚1的外表面不掉落；当然本具体实施例中的网状坩埚2也可采用如具体实施例1相对应的环绕设置于内坩埚1外面表面上方的凸起101对网状坩埚2进行限位吊挂的结构，或采用如具体实施例2相对应的在内坩埚1的外表面由上至下依次间距环绕布置台阶式限位环102的结构。As shown in FIG8 , the difference between this specific embodiment and the specific embodiment 1 is that the mesh crucible 2 has only a lower edge seal and a middle mesh woven portion; and in this specific embodiment, the inner crucible 1 is a graphite crucible, and the mesh crucible 2 and the inner crucible 1 are bonded by coating a graphite glue with a mesh bag. In this specific embodiment, the graphite glue is applied with a thickness of 1 mm, which enables the mesh crucible 2 to adhere well after coating. The outer surface of the inner crucible 1 does not fall; of course, the mesh crucible 2 in this specific embodiment can also adopt the structure of limiting and hanging the mesh crucible 2 by surrounding the protrusion 101 above the outer surface of the inner crucible 1 as in the specific embodiment 1, or adopt the structure of arranging stepped limiting rings 102 in sequence from top to bottom on the outer surface of the inner crucible 1 as in the specific embodiment 2.
具体实施例5：Specific embodiment 5:
如图9所示，该具体实施例相对于具体实施例4的区别在于，中部网状编织部为碗状结构且底部为开口，不带有下封边；As shown in FIG. 9 , the difference between this specific embodiment and specific embodiment 4 is that the middle mesh woven portion is a bowl-shaped structure with an open bottom and no lower edge sealing;
当然本具体实施例中的网状坩埚2也可采用如具体实施例1相对应的环绕设置于内坩埚1外面表面上方的凸起101对网状坩埚2进行限位吊挂的结构，或采用如具体实施例2相对应的在内坩埚1的外表面由上至下依次间距环绕布置台阶式限位环102的结构。Of course, the mesh crucible 2 in this specific embodiment may also adopt a structure in which the protrusions 101 arranged around the outer surface of the inner crucible 1 are used to limit and suspend the mesh crucible 2 as in the specific embodiment 1, or adopt a structure in which stepped limiting rings 102 are arranged around the outer surface of the inner crucible 1 in sequence from top to bottom as in the specific embodiment 2.
具体实施例6：Specific embodiment 6:
如图10所示，该具体实施例相对于具体实施例1的区别在于，中部网状编织部为直筒状结构；网状坩埚2采用环绕设置于内坩埚1外面表面上方的凸起101对网状坩埚2进行限位吊挂的结构，或采用如具体实施例2相对应的在内坩埚1的外表面由上至下依次间距环绕布置台阶式限位环102的结构。As shown in FIG10 , the difference between this specific embodiment and the specific embodiment 1 is that the middle mesh woven portion is a straight cylindrical structure; the mesh crucible 2 adopts a structure in which a protrusion 101 arranged around the outer surface of the inner crucible 1 is used to limit and suspend the mesh crucible 2, or adopts a structure in which stepped limiting rings 102 are arranged around the outer surface of the inner crucible 1 from top to bottom in sequence as in the specific embodiment 2.
具体实施例7：Specific embodiment 7:
如图11-12所示，本具体实施例相对于具体实施例1-6任一项的区别在于，内坩埚1采用分体式坩埚，具体为三瓣式坩埚，且该内坩埚1与网状坩埚2相接触的面上涂覆有石墨胶使形成整体；本具体实施例中仅列举了三瓣式的石墨、碳碳或陶瓷坩埚，当然多瓣式坩埚仍然属于本技术方案的保护范围。As shown in Figures 11-12, the difference between this specific embodiment and any one of specific embodiments 1-6 is that the inner crucible 1 adopts a split crucible, specifically a three-petal crucible, and the surface of the inner crucible 1 in contact with the mesh crucible 2 is coated with graphite glue to form a whole; this specific embodiment only lists three-petal graphite, carbon-carbon or ceramic crucibles, and of course multi-petal crucibles still fall within the protection scope of this technical solution.
本技术方案采用在包裹石英坩埚的石墨、碳碳或陶瓷坩埚外部套设网状坩埚，该网状坩埚是由碳纤维绳编织形成的对石墨、碳碳或陶瓷坩埚进行兜覆的中空网状体，内表面与石墨、碳碳或陶瓷坩埚的外壁相贴合。包裹石英坩埚的坩埚通过选用两层结构，不仅发挥了编织的网状结构能够时刻保持石墨、碳碳或陶瓷坩埚的结构稳定性的优点，还使选择比现有壁厚更薄的石墨、碳碳或陶瓷坩埚成为可能，薄壁石墨、碳碳或陶瓷坩埚和包裹其外的网状坩埚形成的组合坩埚的强度与原厚壁石墨、碳碳或陶瓷坩埚相比没有下降；在该石墨、碳碳或陶瓷坩埚被腐蚀导致内径变大或者由于热膨胀导致龟裂后，只需要对内坩埚进行更换，网状坩埚 可重复使用，相对于原厚壁石墨、碳碳或陶瓷坩埚，其更换成本更低；且由于石墨、碳碳或陶瓷坩埚厚度降低，且网状坩埚是镂空形式，总体热传导效率更高，加热和冷却时间大大缩短，不仅对于加热器所需的功率要求更低，还可以提升拉晶效率，采用网状坩埚能够使石墨、碳碳或陶瓷坩埚需要更换时便于脱离；采用网状坩埚对内坩埚进行兜覆支撑的组合结构，当内坩埚采用分体式坩埚结构时，如三瓣式或多瓣式坩埚，不仅可以有效降低热膨胀带来的影响，且具有良好的整体保持效果。The technical solution adopts a mesh crucible sleeved on the outside of the graphite, carbon-carbon or ceramic crucible that wraps the quartz crucible. The mesh crucible is a hollow mesh body formed by weaving carbon fiber ropes to cover the graphite, carbon-carbon or ceramic crucible, and the inner surface is in contact with the outer wall of the graphite, carbon-carbon or ceramic crucible. The crucible that wraps the quartz crucible adopts a two-layer structure, which not only takes advantage of the woven mesh structure to always maintain the structural stability of the graphite, carbon-carbon or ceramic crucible, but also makes it possible to choose a graphite, carbon-carbon or ceramic crucible with a thinner wall thickness than the existing one. The strength of the combined crucible formed by the thin-walled graphite, carbon-carbon or ceramic crucible and the mesh crucible that wraps it is not reduced compared with the original thick-walled graphite, carbon-carbon or ceramic crucible; after the graphite, carbon-carbon or ceramic crucible is corroded to increase its inner diameter or cracks due to thermal expansion, only the inner crucible needs to be replaced, and the mesh crucible can be replaced. It is reusable and has a lower replacement cost than the original thick-walled graphite, carbon-carbon or ceramic crucible. Since the thickness of the graphite, carbon-carbon or ceramic crucible is reduced and the mesh crucible is hollow, the overall heat conduction efficiency is higher and the heating and cooling time is greatly shortened, which not only reduces the power requirement for the heater but also improves the crystal pulling efficiency. The use of a mesh crucible can facilitate the detachment of the graphite, carbon-carbon or ceramic crucible when it needs to be replaced. The mesh crucible is used to cover and support the inner crucible. When the inner crucible adopts a split crucible structure, such as a three-petal or multi-petal crucible, it can not only effectively reduce the impact of thermal expansion, but also has a good overall retention effect.
以上公开的本发明优选实施例只是用于帮助阐述本发明。优选实施例并没有详尽叙述所有的细节，也不限制该发明仅为所述的具体实施方式。显然，根据本说明书的内容，可作很多的修改和变化。本说明书选取并具体描述这些实施例，是为了更好地解释本发明的原理和实际应用，从而使所属技术领域技术人员能很好地理解和利用本发明。本发明仅受权利要求书及其全部范围和等效物的限制。 The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims (10)

  1. 一种组合式坩埚，其特征在于，包括套设于石英坩埚外部的内坩埚(1)以及用于对内坩埚(1)进行兜覆的网状坩埚(2)，所述内坩埚(1)采用石墨坩埚、碳碳坩埚或陶瓷坩埚。A combined crucible, characterized in that it comprises an inner crucible (1) sleeved on the outside of a quartz crucible and a mesh crucible (2) used to cover the inner crucible (1), wherein the inner crucible (1) is a graphite crucible, a carbon-carbon crucible or a ceramic crucible.
  2. 根据权利要求1所述的一种组合式坩埚，其特征在于，所述网状坩埚(2)与内坩埚(1)之间采用网兜限位结构或通过石墨胶相粘接。The combined crucible according to claim 1, characterized in that a mesh bag limiting structure is used between the mesh crucible (2) and the inner crucible (1) or they are bonded by graphite glue.
  3. 根据权利要求2所述的一种组合式坩埚，其特征在于，所述网兜限位结构包括利用设置于内坩埚(1)外表面的凸起(101)挂住网状坩埚(2)或利用设置于内坩埚(1)外表面的台阶结构(A)卡接住网状坩埚(2)；所述台阶结构(A)的深度为1-10mm；所述凸起(101)的厚度为1-10mm。A combined crucible according to claim 2, characterized in that the net bag limiting structure comprises using a protrusion (101) arranged on the outer surface of the inner crucible (1) to hang the mesh crucible (2) or using a step structure (A) arranged on the outer surface of the inner crucible (1) to clamp the mesh crucible (2); the depth of the step structure (A) is 1-10 mm; the thickness of the protrusion (101) is 1-10 mm.
  4. 据权利要求1所述的一种组合式坩埚，其特征在于，所述内坩埚(1)采用整体式坩埚或分体式坩埚，所述分体式坩埚包括多瓣式坩埚。A combined crucible according to claim 1, characterized in that the inner crucible (1) is a one-piece crucible or a split crucible, and the split crucible includes a multi-petal crucible.
  5. 根据权利要求1所述的一种组合式坩埚，其特征在于，所述网状坩埚(2)是由一根或多根碳纤维绳编织形成的对内坩埚(1)进行兜覆的中空网状体，其内表面与内坩埚(1)外表面相贴合。The combined crucible according to claim 1 is characterized in that the mesh crucible (2) is a hollow mesh body covering the inner crucible (1) formed by weaving one or more carbon fiber ropes, and its inner surface is in contact with the outer surface of the inner crucible (1).
  6. 根据权利要求5所述的一种组合式坩埚，其特征在于，所述网状坩埚(2)具体为碗状或直筒状，底部设有开口或由碳纤维绳编织覆盖，所述网状坩埚(2)的顶部为开口。The combined crucible according to claim 5 is characterized in that the mesh crucible (2) is specifically bowl-shaped or straight-cylindrical, with an opening at the bottom or covered by woven carbon fiber ropes, and the top of the mesh crucible (2) is open.
  7. 根据权利要求5所述的一种组合式坩埚，其特征在于，所述网状坩埚(2)的碳纤维绳表面包覆或填充有沉积碳层或硬化物质层。The combined crucible according to claim 5, characterized in that the surface of the carbon fiber rope of the mesh crucible (2) is coated or filled with a deposited carbon layer or a hardened material layer.
  8. 根据权利要求1所述的一种组合式坩埚，其特征在于，所述陶瓷坩埚的材料包括氮化硼、碳化硅、碳化钨、氧化锆、氧化铝、氮化铝、二硼化钛、碳化鉿中任意一种或多种混合。The combined crucible according to claim 1 is characterized in that the material of the ceramic crucible includes a mixture of any one or more of boron nitride, silicon carbide, tungsten carbide, zirconium oxide, aluminum oxide, aluminum nitride, titanium diboride, and arsenic carbide.
  9. 一种单晶炉，其特征在于：包括如权利要求1-8任一项所述的组合式坩埚。A single crystal furnace, characterized in that it comprises the combined crucible as described in any one of claims 1 to 8.
  10. 一种拉晶方法，其特征在于，采用权利要求9所述单晶炉进行拉晶的方法。 A crystal pulling method, characterized in that the single crystal furnace described in claim 9 is used to pull crystals.
PCT/CN2023/100949 2022-10-20 2023-06-19 Combined crucible and single crystal furnace using same WO2024082663A1 (en)

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