CN116219532B - Guide cylinder for single crystal furnace, preparation method and single crystal furnace - Google Patents
Guide cylinder for single crystal furnace, preparation method and single crystal furnace Download PDFInfo
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- CN116219532B CN116219532B CN202310507657.6A CN202310507657A CN116219532B CN 116219532 B CN116219532 B CN 116219532B CN 202310507657 A CN202310507657 A CN 202310507657A CN 116219532 B CN116219532 B CN 116219532B
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- 239000013078 crystal Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 258
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 257
- 238000011049 filling Methods 0.000 claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 claims abstract description 16
- 230000000903 blocking effect Effects 0.000 claims description 36
- 230000002787 reinforcement Effects 0.000 claims description 33
- 229910000831 Steel Inorganic materials 0.000 claims description 29
- 239000010959 steel Substances 0.000 claims description 29
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 claims description 28
- 230000002829 reductive effect Effects 0.000 claims description 24
- 230000001965 increasing effect Effects 0.000 claims description 12
- 238000009417 prefabrication Methods 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 238000005524 ceramic coating Methods 0.000 claims description 5
- 238000009966 trimming Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 abstract description 22
- 230000003014 reinforcing effect Effects 0.000 abstract description 22
- 238000010298 pulverizing process Methods 0.000 abstract description 19
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 201
- 238000000034 method Methods 0.000 description 37
- 238000009413 insulation Methods 0.000 description 25
- 230000000694 effects Effects 0.000 description 18
- 230000008569 process Effects 0.000 description 17
- 230000004888 barrier function Effects 0.000 description 15
- 239000000843 powder Substances 0.000 description 14
- 238000009826 distribution Methods 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 230000009286 beneficial effect Effects 0.000 description 11
- 238000005192 partition Methods 0.000 description 10
- 239000000945 filler Substances 0.000 description 9
- 229910052581 Si3N4 Inorganic materials 0.000 description 6
- 230000002349 favourable effect Effects 0.000 description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 239000003351 stiffener Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
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- 238000004804 winding Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
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- 239000004744 fabric Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the field of monocrystalline silicon production, and particularly relates to a guide cylinder for a monocrystalline furnace, a preparation method and the monocrystalline furnace, wherein the guide cylinder comprises an outer guide cylinder with a first straight cylinder section and a first conical cylinder section from top to bottom and an inner guide cylinder with a second straight cylinder section and a second conical cylinder section from top to bottom, and the vertical height of the second straight cylinder section is smaller than that of the first straight cylinder section; the carbon felt filling area comprises a temperature gradient enhancement area positioned between the second straight cylinder section and the outer guide cylinder and an inclined low temperature gradient area positioned between the second conical cylinder section and the outer guide cylinder; the carbon felt filling area is filled with a high-density carbon felt layer and a low-density carbon felt layer which is vertically arranged around the high-density carbon felt layer, the temperature gradient reinforcing area is filled with a horizontal high-density carbon felt layer and a vertical high-density carbon felt layer, and the inclined low-temperature gradient area is filled with an inclined high-density carbon felt layer. The invention can effectively inhibit the influence of carbon felt pulverization, improve the influence of nonuniform arrangement of the heat preservation layer, inhibit crystal pulling broken lines, improve crystal quality and improve production efficiency.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon production, and particularly relates to a guide cylinder for a monocrystalline furnace, a preparation method and the monocrystalline furnace.
Background
Monocrystalline silicon is an important material for preparing solar cells in the photovoltaic industry, and is usually prepared by adopting a Czochralski method, specifically, a massive silicon material is placed in a crucible, the silicon material is heated to a melting point to be melted, and under the protection of inert gas, a seed crystal is used as a seeding rod for drawing the monocrystalline silicon rod.
The guide cylinder is generally adopted to guide inert gas, so that the gas is stably circulated, and meanwhile, soft felt is filled in the guide cylinder for heat preservation, so that stable crystallization can be ensured. CN211227431U relates to a novel guide cylinder, comprising an outer guide cylinder and a water-cooled jacket which are sequentially arranged from outside to inside, wherein a thermal insulation material is filled between the outer guide cylinder and the water-cooled jacket; the heat insulating material comprises one or more of soft felt, carbon-carbon composite material, polyurethane material, phenolic resin material, glass wool and aerogel felt.
The ideal heat-insulating layer arrangement is compact, uniform and void-free arrangement. However, the arrangement of the actual heat-insulating layer is easy to be uneven, tight extrusion arrangement among some soft adhesive layers is easy to occur, larger gaps exist among some soft adhesive layers, heat insulation properties of the heat-insulating layer in the guide cylinder in the radial direction and the axial direction are difficult to keep consistent, temperature distribution regularity of a thermal field is poor, crystal breakage is caused, crystal quality is affected, in addition, tiny gaps are inevitably generated due to the connection positions of components in the using process of the device, oxygen permeated into the working environment is easy to enter, pulverization of carbon felt and the like is caused, and heat-insulating effect is affected.
Disclosure of Invention
The invention aims to overcome the defects of broken crystal line and influence on crystal quality caused by pulverization of carbon felt and uneven arrangement of an insulating layer in the process of preparing monocrystalline silicon by a Czochralski method in the prior art, and provides a guide cylinder for a monocrystalline furnace, a preparation method and the monocrystalline furnace.
In order to achieve the above object, in a first aspect, the present invention provides a draft tube for a single crystal furnace, comprising:
the outer guide cylinder comprises a first straight cylinder section and a first cone cylinder section from top to bottom, and the first cone cylinder section is gradually reduced from top to bottom;
the inner guide cylinder comprises a second straight cylinder section and a second conical cylinder section from top to bottom, the second conical cylinder section is gradually reduced from top to bottom, the bottom of the second conical cylinder section is connected with the bottom of the first conical cylinder section, and the vertical height of the second straight cylinder section is smaller than that of the first straight cylinder section;
the carbon felt filling area comprises a temperature gradient enhancement area and an inclined low temperature gradient area, the temperature gradient enhancement area and the inclined low temperature gradient area are positioned in a cavity area between the outer guide cylinder and the inner guide cylinder, the temperature gradient enhancement area is positioned in a cavity area between the second straight cylinder section and the outer guide cylinder, and the inclined low temperature gradient area is positioned in a cavity area between the second cone section and the outer guide cylinder;
The high-density carbon felt layer is filled in the carbon felt filling area, the low-density carbon felt layer is vertically arranged around the high-density carbon felt layer, the high-density carbon felt layer is horizontally arranged and vertically arranged in the temperature gradient reinforcing area, the high-density carbon felt layer is obliquely arranged in the oblique low-temperature gradient area, and the oblique direction of the high-density carbon felt layer is the same as the oblique direction of the second cone section.
In some preferred embodiments, the temperature gradient enhancement region is filled with 2-8 high-density carbon felt layers horizontally arranged at intervals along the vertical direction.
In some preferred embodiments, the high density carbon felt layer is provided horizontally, vertically and obliquely at a density of 0.17g/cm 3 -0.24g/cm 3 The density of the low-density carbon felt layer is 0.08g/cm 3 -0.16g/cm 3 。
In some preferred embodiments, the surface of the vertically disposed high density carbon felt layer and/or the obliquely disposed high density carbon felt layer is coated with a ceramic coating;
in some preferred embodiments, tungsten-molybdenum steel sheet layers are obliquely arranged on two sides of the high-density carbon felt layer which is vertically arranged, and the horizontal distance from the upper part of the tungsten-molybdenum steel sheet layer to the high-density carbon felt layer which is vertically arranged is smaller than the horizontal distance from the lower part of the tungsten-molybdenum steel sheet layer to the high-density carbon felt layer which is vertically arranged.
In some preferred embodiments, the high density carbon felt layer is disposed at an angle of 5-25 ° to the vertical.
In some preferred embodiments, the bottom of the guide cylinder is provided with a supporting structure, the supporting structure comprises a first supporting disk and a second supporting disk, the first supporting disk is obliquely arranged, the second supporting disk is horizontally arranged, the upper part of the first supporting disk is connected with the bottom of the inner guide cylinder, the outer part of the second supporting disk is connected with the bottom of the outer guide cylinder, and the inner part of the second supporting disk 702 is connected with the lower part of the first supporting disk;
the carbon felt filling area further comprises a high-density blocking area, the high-density blocking area is positioned in a cavity area between the first supporting disc and the second supporting disc and a cavity area between the first supporting disc and the outer guide cylinder, and the filling density of the high-density blocking area is 0.3g/cm 3 -0.5g/cm 3 。
More preferably, a reinforcement is arranged between the inclined low temperature gradient region and the high-density blocking region, the reinforcement comprises a first reinforcement part and a second reinforcement part which are integrally formed from top to bottom, the first reinforcement part is vertically arranged, and the first reinforcement part passes through an interface between the inclined low temperature gradient region and the high-density blocking region; the second reinforcing part is obliquely arranged, and the oblique direction of the second reinforcing part is the same as the oblique direction of the first supporting disc; the reinforcement is a tungsten molybdenum steel reinforcement.
In a second aspect, the present invention provides a method for preparing the guide cylinder according to the first aspect, which includes the following steps:
assembling the outer guide cylinder and the inner guide cylinder to form a shell of the guide cylinder, extracting the outline of a cavity area between the outer guide cylinder and the inner guide cylinder,
prefabricating a high-density carbon felt layer and a low-density carbon felt layer into a cylindrical prefabrication body, wherein prefabrication comprises arranging the positions and the directions of the high-density carbon felt layer and the low-density carbon felt layer according to the outline of the cavity area and the positions and the directions of the high-density carbon felt layer and the low-density carbon felt layer in the first aspect;
trimming the cylindrical preform into a filling body according to the outline of the cavity area, wherein the shape of the filling body is the same as that of the cavity area;
and assembling the filling body, the outer guide cylinder and the inner guide cylinder into the guide cylinder.
In a third aspect, the invention provides a single crystal furnace, which comprises the guide cylinder in the first aspect or the guide cylinder prepared by the preparation method in the second aspect; the crucible is positioned below the guide cylinder, the crucible is provided with a silicon melt containing part, and the inner diameter of the crucible is larger than the outer diameter of the first cylinder section of the outer guide cylinder.
According to the invention, the high-density carbon felt layers which are horizontally arranged and vertically arranged are filled in the temperature gradient enhancement region, the high-density carbon felt layers which are obliquely arranged are filled in the oblique low-temperature gradient region, and the oblique direction of the high-density carbon felt layers which are obliquely arranged is the same as the oblique direction of the second cone section, so that on one hand, the influence of carbon felt pulverization on the heat insulation performance can be restrained, on the other hand, the influence of uneven arrangement of the heat insulation layer can be improved, and a stable temperature gradient is established, so that the problem of crystal pulling disconnection is reduced, the crystal quality is improved, and in addition, the temperature gradient along the crystal pulling direction can be moderately increased, and the production efficiency is improved.
The high-density carbon felt layer horizontally arranged in the temperature gradient enhancement zone can cover gaps among the vertically arranged low-density carbon felt layers, and can block external air flow, so that pulverization of the carbon felt is inhibited, and the heat preservation effect is improved; in addition, the high-density carbon felt layer horizontally arranged can divide the temperature gradient enhancement area into more than 2 sections in the vertical direction, a plurality of temperature partitions with gradually reduced temperature are formed from bottom to top, the temperature of each temperature partition is kept approximately the same due to the blocking effect, stable temperature gradients can be formed, on one hand, the crystal pulling broken line is restrained, the crystal quality is improved, on the other hand, the temperature gradients along the crystal pulling direction are moderately increased, and the pulling speed can be properly improved, so that the production efficiency is improved; further, the high-density carbon felt layer horizontally arranged can block the pulverized powder at the upper part, so that the accumulation of the pulverized powder of the carbon felt to the lower part can be restrained, and further the heat conduction and insulation performance of the lower part is deteriorated.
The high-density carbon felt layer arranged vertically is filled in the temperature gradient enhancement region, and the high-density carbon felt layer arranged horizontally is matched, so that the high-density carbon felt layer can play a role of a framework, the carbon felt in the temperature gradient enhancement region is supported, the deformation resistance is improved, the pulverization of the carbon felt is reduced, and the heat preservation effect is improved; the temperature transmission from inside to outside in the radial direction can be adjusted, the temperature distribution is adjusted, the breakage of the crystal pulling is restrained, and the crystal quality is improved.
The high-density carbon felt layer is filled in the inclined low-temperature gradient zone, so that temperature transmission from inside to outside can be adjusted, temperature distribution can be adjusted, crystal breakage can be restrained, crystal quality can be improved, heat conduction direction can be adjusted, heat conduction perpendicular to the direction of the inclined high-density carbon felt layer can be formed, moderate temperature gradient can be formed in the contraction section of the guide cylinder, production efficiency can be improved on the premise that crystal cooling defects are avoided, in addition, the deposition position of pulverized powder can be controlled, and the influence on heat preservation performance of the whole zone is reduced.
According to the preparation method of the guide cylinder, the high-density carbon felt layer and the low-density carbon felt layer are prefabricated into the cylindrical prefabricated body, the cylindrical prefabricated body is trimmed into the filling body according to the outline of the cavity area, the filling body, the inner guide cylinder and the outer guide cylinder are assembled into the guide cylinder, the heat preservation layer has good bending strength, the inner guide cylinder and the outer guide cylinder can be mutually supported, deformation is reduced, the centering precision of a thermal field is improved, the shape of the filling body is matched with the cavity area between the inner guide cylinder and the outer guide cylinder, the temperature field at the lower end of the guide cylinder is stabilized, and crystal breakage is restrained and the crystal quality is improved.
The single crystal furnace provided by the invention can adjust the temperature distribution of the thermal field, thereby inhibiting the breakage of crystal pulling and improving the crystal quality, inhibiting the pulverization of carbon felt and the like, reducing the influence of the pulverization on the heat preservation effect, moderately increasing the temperature gradient along the crystal pulling direction and improving the production efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic sectional view of a single crystal furnace according to an embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view of an embodiment of a guide shell of the present invention.
FIG. 3 is a schematic cross-sectional view of one embodiment of the interface region of the sloped low temperature gradient zone 302 and the high density barrier zone 303 of the guide cylinder of the present invention.
Fig. 4 is a schematic first cross-sectional view of the packing in the interface region of the sloped low temperature gradient zone 302 and the high density barrier zone 303 of the draft tube of the present invention.
Fig. 5 is a schematic view of a second cross-sectional configuration of the packing in the interface region of the sloped low temperature gradient zone 302 and the high density barrier zone 303 of the draft tube of the present invention.
Description of the reference numerals
1-an outer guide cylinder; 101-a first barrel section; 102-a first cone section; 2-an inner guide shell; 201-a second straight barrel section; 202-a second cone section; 3-carbon felt filled region; 301-a temperature gradient enhancement zone; 302-a sloped low temperature gradient zone; 303-a high dense barrier region; 4-a high density carbon felt layer; 5-a low density carbon felt layer; 6-tungsten-molybdenum steel sheet layers; 7-a support structure; 701-a first support plate; 702-a second support plate; 8-a stiffener; 801-a first reinforcement; 802-a second reinforcement; 9-crucible.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventor of the invention researches and discovers that the heat insulation layer in the current single crystal furnace guide cylinder has poor temperature distribution regularity of a thermal field due to uneven arrangement of a soft adhesive layer, so that the broken line of crystal pulling is easily caused, the crystal quality is easily influenced, and meanwhile, the carbon felt is easily pulverized, so that the heat insulation effect is influenced.
In this regard, in a first aspect, the present invention provides a draft tube for a single crystal furnace, comprising:
the outer guide cylinder 1 comprises a first straight cylinder section 101 and a first cone cylinder section 102 from top to bottom, wherein the first cone cylinder section 102 tapers from top to bottom;
the inner guide cylinder 2 comprises a second straight cylinder section 201 and a second conical cylinder section 202 from top to bottom, the second conical cylinder section 202 tapers from top to bottom, the bottom of the second conical cylinder section 202 is connected with the bottom of the first conical cylinder section 102, and the vertical height of the second straight cylinder section 201 is smaller than that of the first straight cylinder section 101;
a carbon felt filling region 3, wherein the carbon felt filling region 3 comprises a temperature gradient enhancement region 301 and an inclined low temperature gradient region 302, the temperature gradient enhancement region 301 and the inclined low temperature gradient region 302 are positioned in a cavity region between the outer guide cylinder 1 and the inner guide cylinder 2, the temperature gradient enhancement region 301 is positioned in a cavity region between the second straight cylinder section 201 and the outer guide cylinder 1, and the inclined low temperature gradient region 302 is positioned in a cavity region between the second cone section 202 and the outer guide cylinder 1;
wherein, the carbon felt filling area 3 is filled with a high-density carbon felt layer 4 and a low-density carbon felt layer 5 filled around the high-density carbon felt layer 4, the low-density carbon felt layer 5 is vertically arranged, the temperature gradient enhancing area 301 is filled with the high-density carbon felt layer 4 horizontally arranged and vertically arranged, the inclined low-temperature gradient area 302 is filled with the high-density carbon felt layer 4 obliquely arranged, and the inclined direction of the high-density carbon felt layer 4 obliquely arranged is the same as the inclined direction of the second cone section 202.
According to the invention, the outer guide cylinder and the inner guide cylinder comprise a straight cylinder section and a conical cylinder section from top to bottom, the vertical height of the straight cylinder section of the inner guide cylinder is smaller than that of the straight cylinder section of the outer guide cylinder, the bottoms of the conical cylinder sections of the inner guide cylinder and the outer guide cylinder are connected, a temperature gradient enhancement area is arranged in a cavity area between the straight cylinder section of the inner guide cylinder and the outer guide cylinder, and an inclined low temperature gradient area is arranged in the cavity area between the conical cylinder section of the inner guide cylinder and the outer guide cylinder, so that the influence of uneven arrangement of a heat preservation layer can be improved, the temperature distribution can be adjusted, the broken line phenomenon of crystal is reduced, the influence of carbon felt pulverization on heat preservation performance can be restrained, in addition, the temperature gradient along the crystal pulling direction can be moderately increased, and the production efficiency is improved.
Specifically, in the cavity area between the straight barrel section of the inner guide barrel and the outer guide barrel, the high-density carbon felt layers arranged horizontally are filled, on one hand, gaps or uneven lamination are inevitably formed between the carbon felt layers in the laying process of the vertical multi-layer low-density carbon felt (mainly soft felt) in the prior art, the gaps lead to the entering of external air flow, and further lead to the pulverization of the carbon felt, the heat preservation effect is affected, the service life is shortened, the gaps between the vertical low-density carbon felt layers can be covered by the high-density carbon felt layers arranged horizontally, the external air flow is blocked, the pulverization of the carbon felt is restrained, the heat preservation effect is improved, and the service life is prolonged; further, in the use process of the carbon felt, along with the extension of the use time, the pulverized powder of the carbon felt is continuously accumulated towards the lower part, so that the lower heat conduction and insulation performance is deteriorated, the service life is reduced, the horizontally arranged high-density carbon felt layer can play a role in blocking the carbonized powder at the upper part of the heat insulation layer of the guide cylinder, the accumulation of the carbonized powder towards the lower part is restrained, is reduced in the deterioration of the lower heat insulation performance, on the other hand, a cavity area between a straight cylinder section of the inner guide cylinder and an outer guide cylinder can be divided into more than two sections in the vertical direction, a plurality of temperature partitions are formed, wherein the temperature of each temperature partition is kept approximately the same due to the blocking effect, the temperature distribution can be adjusted, the broken line is restrained, the crystal quality is improved, in addition, the higher the temperature of the temperature partition which is closer to the silicon melt in the crucible is gradually reduced from bottom to top is formed, and the temperature partition which is far away from the silicon melt in the crucible is separated from the lower, the lower in temperature partition is not obtained in the lower heat supplement or is obtained in the heat supplement from the lower part, the temperature partition which is moderately increased in the temperature gradient along the pulling direction is approximately, the temperature gradient of the silicon melt in the crucible is far away from the crucible is suitable for the temperature partition, the temperature in the crucible is suitable for the production, the temperature partition is lower, and the temperature is suitable for the temperature change is higher, and the temperature condition is suitable for the temperature is higher.
In the cavity district between the straight section of inner draft tube and outer draft tube, pack vertical high density carbon felt layer, on the one hand can cooperate with the high density carbon felt layer that the level set up, play the skeleton effect, realize the support to the carbon felt in temperature gradient enhancement district, improve anti deformability, reduce carbon felt pulverization, improve the heat preservation effect, improve life-span, on the other hand, can adjust the inside-out temperature transmission of radial direction, adjust temperature distribution, thereby restrain the crystal pulling broken string and improve crystal quality.
The vertical height of the straight section of the inner guide cylinder is smaller than that of the straight section of the outer guide cylinder, the high-density carbon felt layer which is obliquely arranged is filled in a cavity area between the taper section of the inner guide cylinder and the outer guide cylinder in cooperation with the high-density carbon felt layer which is obliquely arranged, the oblique direction of the high-density carbon felt layer which is obliquely arranged is identical with that of the taper section of the inner guide cylinder, on one hand, the deposition position of powdered powder can be controlled, the influence of the powdered powder on the heat insulation performance of the whole area of the heat insulation layer is reduced, on the other hand, the temperature transmission from inside to outside can be adjusted, the temperature distribution is adjusted, the broken line of crystal pulling is restrained, the crystal quality is improved, further, the specific shape of the cavity area is combined, the heat conduction direction can be adjusted, the heat conduction perpendicular to the direction of the high-density carbon felt layer which is obliquely arranged is formed, and the production efficiency is improved on the premise that the crystal cooling defect is avoided. In addition, the high-density carbon felt layer which is obliquely arranged is filled, so that the carbon felt filled in the oblique low-temperature gradient area can be supported, the deformation resistance is improved, the pulverization of the carbon felt is reduced, and the heat preservation effect is improved.
In the present invention, the temperature gradient increasing region means that the region has a moderately increased temperature gradient in the pulling direction, and the inclined low temperature gradient region means that the region has heat conduction in a direction perpendicular to the high density carbon felt layer which is obliquely disposed, in which a moderately increased temperature gradient is formed.
The high-density carbon felt layer and the low-density carbon felt layer are high and low in relative density, the vertically arranged carbon felt layer comprises a carbon felt layer with lower density and a carbon felt layer with higher density, and the densities of the horizontally arranged carbon felt layer and the obliquely arranged carbon felt layer are high relative to those of the vertically arranged carbon felt layer with lower density.
In the present invention, the inclination direction of the high-density carbon felt layer 4 which is obliquely arranged is the same as the inclination direction of the second cone section 202, and the inclination direction is the same direction, and the inclination angle is not included.
In some preferred embodiments, the high density carbon felt layer 4 is arranged horizontally, vertically and obliquely with a density of 0.17g/cm 3 -0.24g/cm 3 The density of the low density carbon felt layer 5 was 0.08g/cm 3 -0.16g/cm 3 . The heat preservation effect of the low-density carbon felt layer is better exerted, and the effects of adjusting the temperature distribution of the high-density carbon felt layer, moderately increasing the temperature gradient in the crystal pulling direction, blocking the pulverized powder, supporting the temperature gradient enhancement region and the inclined low-temperature gradient region are better exerted.
In the present invention, the densities of the high-density carbon felt layers 4 which are horizontally arranged, vertically arranged and obliquely arranged may be the same or different, and the average thicknesses thereof may be the same or different, so long as the effects of suppressing pulverization of the carbon felt, adjusting the temperature distribution, suppressing breakage of crystal pulling and improving the crystal quality can be achieved.
In some preferred embodiments, the temperature gradient reinforcement areas 301 are filled with 2 to 8 high-density carbon felt layers 4 arranged horizontally at intervals along the vertical direction. Specifically, the number of the elements may be, for example, 2, 3, 4, 5, 6, 7, or 8. The number of the high-density carbon felt layers 4 arranged horizontally is at least 2, which is more beneficial to blocking external air flow, inhibiting pulverization of carbon felt and inhibiting accumulation of carbonized powder to the lower part, and the temperature gradient enhancement area is divided into 3-9 sections in the vertical direction by adopting 2-8 high-density carbon felt layers arranged horizontally, so that the temperature distribution is more beneficial to adjusting, the requirement of the Czochralski method for producing single crystals on the temperature gradient is more met, the pulling speed can be properly improved, and the production efficiency is more beneficial to improving.
In some preferred embodiments, the temperature gradient reinforcement areas 301 are filled with 1 to 3 high-density carbon felt layers 4 arranged vertically at intervals along the horizontal direction. Specifically, the number of the components may be 1, 2 or 3. The high-density carbon felt layers with 1-3 vertical settings divide the temperature gradient enhancement zone into 2-4 sections in the radial direction, so that the high-density carbon felt layers which are horizontally arranged are more beneficial to being matched, the temperature gradient enhancement zone is supported, the pulverization of carbon felt is reduced, the heat preservation effect is improved, the radial temperature distribution is more beneficial to being adjusted, the broken line of crystal pulling is restrained, and the crystal quality is improved.
In some preferred embodiments, the included angle between the high-density carbon felt layer 4 and the vertical direction is 5-25 degrees, and the height of the straight barrel section of the inner guide barrel is smaller than that of the straight barrel section of the outer guide barrel in combination with the structure of the guide barrel, the cone section of the outer guide barrel is connected with the bottom of the cone section of the inner guide barrel, the included angle is larger than 5 degrees, the heat conduction direction is more favorably adjusted, the heat conduction perpendicular to the direction of the high-density carbon felt layer is formed, the moderate temperature gradient is more favorably formed in the shrinkage section of the guide barrel, the production efficiency is more favorably improved, the included angle is smaller than 25 degrees, the temperature gradient is more favorably controlled, and the risk of broken crystal pulling is reduced.
In the present invention, the connection mode of the high-density carbon felt layer 4 vertically arranged and the high-density carbon felt layer 4 horizontally arranged has a wide optional range, and can play a role of a skeleton as long as the connection modes can be mutually matched, so that the carbon felt in the temperature gradient enhancement region is supported, the deformation resistance is improved, and in some preferred embodiments, the connection mode comprises at least one of the following connection modes, the connection modes are connected in an integrally formed mode, the connection modes are not connected at intervals, and the connection modes are connected together through extrusion.
In some preferred embodiments, the low-density carbon felt layer 5 is filled in the temperature gradient enhancing region 301 and the inclined low-temperature gradient region 302, that is, the low-density carbon felt layer 5 is uninterrupted at the interface of the temperature gradient enhancing region 301 and the inclined low-temperature gradient region 302, which is beneficial to enhancing the strength and the heat preservation effect of the heat preservation layer.
In some preferred embodiments, the surface of the high-density carbon felt layer 4 disposed vertically and/or the high-density carbon felt layer 4 disposed obliquely is coated with a ceramic coating; optionally, tungsten-molybdenum steel sheet layers 6 are obliquely arranged on two sides of the high-density carbon felt layer 4 which is vertically arranged, and the horizontal distance from the upper part of the tungsten-molybdenum steel sheet layer 6 to the high-density carbon felt layer 4 which is vertically arranged is smaller than the horizontal distance from the lower part of the tungsten-molybdenum steel sheet layer 6 to the high-density carbon felt layer 4 which is vertically arranged. Through the surface coating ceramic coating at the high density carbon felt layer of vertical setting and the high density carbon felt layer 4 of slope setting, because ceramic coating heat conductivity is limited, more be favorable to delaying the transmission of temperature, improve thermal insulation performance, more be favorable to restraining the crystal pulling broken wire and improve crystal quality. Preferably, the ceramic layer is selected from one or more of alumina, silicon nitride, silicon carbide, zirconia. Through set up tungsten molybdenum steel sheet layer in the slope of the both sides on the high density carbon felt layer of vertical setting, wherein tungsten molybdenum steel sheet layer's upper portion is less than tungsten molybdenum steel sheet layer's lower part to vertical setting to the horizontal distance on high density carbon felt layer 4, more do benefit to the layering of the low density carbon felt layer that reduces vertical setting, improve the holistic stability of carbon felt packing body, improve life.
In some preferred embodiments, the bottom of the guide cylinder is provided with a supporting structure 7, the supporting structure 7 comprises a first supporting disc 701 and a second supporting disc 702, the first supporting disc 701 is obliquely arranged, the second supporting disc 702 is horizontally arranged, the upper part of the first supporting disc 701 is connected with the bottom of the inner guide cylinder 2, the outer part of the second supporting disc 702 is connected with the bottom of the outer guide cylinder 1, and the inner part of the second supporting disc 702 is connected with the lower part of the first supporting disc 701;
the carbon felt filled region 3 further comprises a highly dense barrier region 303, the highly dense barrier region 303 being located between the first support plate 701 and the second support plate 702 and the first cavity regionThe high density barrier region 303 fills the cavity region between the support plate 701 and the outer guide shell 1 with a density of 0.3g/cm 3 -0.5g/cm 3 。
The cavity area between the first support disk and the second support disk and the cavity area between the first support disk and the outer guide cylinder are nearest to the silicon melt and the seed crystal, and have great influence on the crystal pulling process and the crystal quality by 0.3g/cm 3 -0.5g/cm 3 Is more favorable for improving the strength of the carbon felt at the position, is more favorable for effectively blocking the pulverized powder of the upper carbon felt, is more favorable for reducing the risk of the pulverized powder of the carbon felt falling into a crucible, improves the crystal pulling quality, and is also more favorable for improving the crystal pulling quality by ultra-high densification (0.3 g/cm) 3 -0.5g/cm 3 ) The heat conduction performance of the area is greatly increased, although the heat insulation capability of the carbon felt is reduced, the heat conduction is mainly realized by the heat radiation and heat convection mode due to the extremely thin part, namely the heat conduction at the part is weakened, the mode of relying on the heat radiation and the heat convection is changed, the temperature fluctuation of the initial position of the crystal pulling entering the guide cylinder can be further reduced, the breakage rate is further reduced, and the pulling speed and the production efficiency are further improved.
Further, by filling the carbon felt filling region between the second cone section 202 of the inner guide cylinder 2 and the outer guide cylinder 1 with the high-density carbon felt layer 4 which is obliquely arranged, the powdered carbon felt can be obliquely conveyed downwards to the upper part of the bottom high-density blocking region 303, and the effect of the bottom high-density blocking region 303 can be enhanced by the deposition, so that the effects of long service time, no influence on the use, maintenance or enhancement are achieved, and the service life is prolonged.
In the invention, the high-density blocking area 303 means that the filling density of the carbon felt in the area is high, which is more beneficial to blocking the pulverized powder of the carbon felt at the upper part and reducing the risk of the pulverized powder of the carbon felt falling into a crucible.
In some preferred embodiments, the surface of the carbon felt filler in the highly dense barrier region 303 is coated with a reflective coating, which is more beneficial to increase local reflection, reduce temperature fluctuations of the crystal ingot, and reduce the risk of crystal pull wire breakage. Preferably, the reflective coating is at least one of a silicon carbide coating, a high temperature resistant nanomaterial, a carbon-carbon composite material or a carbon cloth reflective material.
In some preferred embodiments, a reinforcement member 8 is disposed between the sloped low temperature gradient zone 302 and the high density blocking zone 303, the reinforcement member 8 includes a first reinforcement portion 801 and a second reinforcement portion 802 integrally formed from top to bottom, the first reinforcement portion 801 is disposed vertically, and the first reinforcement portion 801 passes through an interface between the sloped low temperature gradient zone 302 and the high density blocking zone 303; the second reinforcing portion 802 is obliquely arranged, and the oblique direction of the second reinforcing portion 802 is the same as the oblique direction of the first supporting plate 701; preferably, the stiffener 8 is a tungsten molybdenum steel stiffener. Through setting up the reinforcement that first enhancement portion and the second enhancement portion integrated into one piece that the slope set up of vertical setting are connected, can further strengthen the joint strength in high dense blocking area and slant low temperature gradient district, improve the life-span, further increase the intensity in high dense blocking area simultaneously.
In a second aspect, the present invention provides a method for preparing the guide cylinder according to the first aspect, including the following steps:
assembling the outer guide cylinder 1 and the inner guide cylinder 2 to form a guide cylinder shell, extracting the outline of a cavity area between the outer guide cylinder 1 and the inner guide cylinder 2,
Prefabricating the high-density carbon felt layer 4 and the low-density carbon felt layer 5 into a cylindrical prefabrication body, wherein the prefabrication comprises the steps of setting the positions and the directions of the high-density carbon felt layer 4 and the low-density carbon felt layer 5 according to the outline of the cavity area and the positions and the directions of the high-density carbon felt layer 4 and the low-density carbon felt layer 5 in the first aspect;
trimming the cylindrical preform into a filling body according to the outline of the cavity area, wherein the shape of the filling body is the same as that of the cavity area;
and assembling the filling body, the outer guide cylinder 1 and the inner guide cylinder 2 into the guide cylinder.
According to the invention, the cylindrical prefabricated body is prepared according to the outline of the cavity area and the positions and directions of the high-density carbon felt layer 4 and the low-density carbon felt layer 5 in the first aspect, then the cylindrical prefabricated body is trimmed into a filling body according to the outline of the cavity area, and then the filling body, the outer guide cylinder and the inner guide cylinder are assembled into the guide cylinder, so that the bending strength of the heat insulation layer in the guide cylinder can be further improved, the outer guide cylinder and the inner guide cylinder are mutually supported, the deformation is reduced, the centering precision of a thermal field is further improved, the heat insulation performance of the heat insulation layer in the circumferential direction is further ensured due to the fact that the shape of the filling body is the same as that of the cavity area between the outer guide cylinder and the inner guide cylinder, the axisymmetry and the stability of the thermal field are improved, the crystal quality is further ensured, and in addition, the filling body is prefabricated in advance, the disassembly and assembly and disassembly are convenient, the labor hour and the labor intensity of workers are saved, and the high-strength work and positioning correction of staff in the winding process of the carbon felt are avoided.
The narrow and small carbon felt filling area of draft tube bottom, the liquid level of silicon melt in the crucible is nearer, and is great to crystal pulling stability influence, and the temperature fluctuation in this region can greatly increased crystal pulling broken wire risk, and direct winding carbon felt hardly twines evenly, forms two kinds of compound heat conduction modes of air convection and carbon felt heat conduction in this position region, and twines in the position of draft tube bottom circumference round and arrange, and the clearance of carbon felt after twining each other is inhomogeneous, probably influences the stability of this position temperature, causes crystal pulling in-process broken wire. In particular, in the invention, the cylindrical prefabricated body is trimmed into the filling body according to the outline of the cavity area, and the filling body, the outer guide cylinder and the inner guide cylinder are directly assembled into the guide cylinder, so that the heat insulation layer in a narrow area at the bottom of the guide cylinder is tightly attached to the wall of the guide cylinder, the consistency of temperature gradient is further ensured, the heat insulation performance and strength of the bottom position of the guide cylinder are ensured, the crystal pulling stability is improved, and the service life of the guide cylinder is prolonged.
In the present invention, by filling the high-density carbon felt layer 4 horizontally and vertically disposed in the temperature gradient enhancing region 301 between the second cone section 202 of the inner cylinder 2 and the outer cylinder 1, the overall deformation resistance of the preform and the filler can be improved in the process of prefabricating the high-density carbon felt layer 4 and the low-density carbon felt layer 5 into a cylindrical preform, trimming the cylindrical preform into a filler, and assembling the filler into a cylinder.
In some preferred embodiments, the high-density carbon felt layer 4, the low-density carbon felt layer 5, and the tungsten-molybdenum steel sheet layer 6 are preformed into a cylindrical preform, the prefabrication including positioning and orienting the high-density carbon felt layer 4, the low-density carbon felt layer 5, and the tungsten-molybdenum steel sheet layer 6 in accordance with the outline of the cavity region and the positioning and orientation of the first aspect.
In some preferred embodiments, the outer guide shell 1, the inner guide shell 2 and the support structure 7 are assembled to form the outer shell of the guide shell, and the overall outline of the cavity area between the outer guide shell 1 and the inner guide shell 2, the cavity area between the first support disc 701 and the second support disc 702, and the cavity area between the first support disc 701 and the outer guide shell 1 is extracted; prefabricating the filling bodies of the high-density carbon felt layer 4, the low-density carbon felt layer 5 and the high-density barrier region 303 into cylindrical filling bodies, wherein the prefabrication comprises arranging the positions and the directions of the filling bodies of the high-density carbon felt layer 4, the low-density carbon felt layer 5 and the high-density barrier region 303 according to the overall outline of the cavity region and the arranging positions and the directions of the first aspect; and assembling the filling body, the outer guide cylinder 1, the inner guide cylinder 2 and the supporting structure 7 into the guide cylinder.
More preferably, the high-density carbon felt layer 4, the low-density carbon felt layer 5, the filler of the high-density barrier region 303, and the reinforcing member 8 are prefabricated into a cylindrical filler, the prefabrication including arranging the positions and orientations of the high-density carbon felt layer 4, the low-density carbon felt layer 5, the filler of the high-density barrier region 303, and the reinforcing member 8 in accordance with the overall outline of the cavity region and the arrangement positions and orientations of the first aspect.
In some preferred embodiments, after the profile of the cavity area between the outer guide cylinder 1 and the inner guide cylinder 2 is extracted, the profile of the cavity area is optimized, and small-size or small-area edges with complex shapes and negligible edges with small areas are sheared or removed, so that the processing and forming of the filling body are facilitated, partial fracture of the filling body in the process of assembling the guide cylinder is avoided, the heat insulation of the heat insulation layer at the partial position is not uniform, preferably, the profile pattern of the filling body in fig. 4 is optimized to the profile pattern of the filling body in fig. 5, and gaps between the filling body at the lowest part of the guide cylinder and the inner guide cylinder wall or between the first support disc 701 and the second support disc 702 are consistent through the optimized profile, so that a gap cavity structure in the radial direction is formed, and uniform heat insulation and heat insulation blocking are facilitated.
In a third aspect, the invention provides a single crystal furnace, which comprises the guide cylinder in the first aspect or the guide cylinder prepared by the preparation method in the second aspect; a crucible 9, the crucible 9 is located below the guide cylinder, the crucible 9 is provided with a silicon melt containing part, and the inner diameter of the crucible 9 is larger than the outer diameter of the first cylinder section 101 of the outer guide cylinder 1.
The following describes the technical solution in the embodiment of the present invention in detail with reference to the drawings in the embodiment of the present invention.
Example 1
1-3, including crucible 9 and the draft tube that is located crucible 9 top, silicon melt holding portion has in the crucible 9, the internal diameter of crucible 9 is greater than the external diameter of the first section 101 of outer draft tube 1, the draft tube includes outer draft tube 1 and interior draft tube 2, the top of interior draft tube 2 and outer draft tube 1 is provided with the connecting portion that is connected with the single crystal growing furnace, be used for fixing the draft tube in the single crystal growing furnace, outer draft tube 1 top-down includes first section 101 and first section 102, first section 102 top-down tapers, interior draft tube 2 top-down includes second section 201 and second section 202, second section 202 tapers from top to bottom, the inclination angle of first section 102 is 45 with respect to first section 101, the inclination angle of second section 202 is 20 with respect to second section 201. The bottom of the guide cylinder is provided with a supporting structure 7, the supporting structure 7 comprises a first supporting disk 701 and a second supporting disk 702, the first supporting disk 701 is obliquely arranged, the second supporting disk 702 is horizontally arranged, the upper part of the first supporting disk 701 is connected with the bottom of the second cone section 202 of the inner guide cylinder 2, the outer part of the second supporting disk 702 is connected with the bottom of the first cone section 102 of the outer guide cylinder 1, and the inner part of the second supporting disk 702 is connected with the lower part of the first supporting disk 701;
A temperature gradient enhancement zone 301 is arranged between the second straight cylinder section 201 and the outer guide cylinder 1, an inclined low temperature gradient zone 302 is arranged between the second conical cylinder section 202 and the outer guide cylinder 1, and a high-density blocking zone 303 is arranged between the first support plate 701 and the second support plate 702 and between the first support plate 701 and the outer guide cylinder 1;
and, the temperature gradient reinforcement zone 301 is filled with 3 high-density carbon felt layers 4 arranged horizontally at intervals along the vertical direction, the density of the high-density carbon felt layers 4 arranged horizontally is 0.23g/cm 3 The temperature gradient reinforcement zone 301 is filled with 1 vertically disposed high density carbon felt layer 4, the vertically disposed high density carbon felt layer 4 extends from the uppermost horizontally disposed high density carbon felt layer 4 to the lowermost horizontally disposed high density carbon felt layer 4, the vertically disposed high density carbon felt layer 4 forms an "I" with the horizontally disposed high density carbon felt layer 4, and the density of the vertically disposed high density carbon felt layer 4 is 0.23g/cm 3 The surface of the high-density carbon felt layer is coated with a silicon nitride coating, the vertically arranged high-density carbon felt layer 4 and the horizontally arranged high-density carbon felt layer 4 are connected in an integrated mode, and tungsten-molybdenum steel sheet layers 6 are obliquely arranged on two sides of the vertically arranged high-density carbon felt layer 4;
and, the inclined low temperature gradient zone 302 is filled with 3 high density carbon felt layers 4 arranged in an inclined way at intervals, the density of the high density carbon felt layers 4 arranged in an inclined way is 0.23g/cm 3 The surface of the inner guide cylinder is coated with a silicon nitride coating, and the inclined direction of the high-density carbon felt layer 4 which is obliquely arranged is the same as the inclined direction of the cone section of the inner guide cylinder, and the included angle between the high-density carbon felt layer and the vertical direction is 18 degrees;
and, except for the high-density carbon felt layer 4, the temperature gradient reinforcing region 301 and the inclined low-temperature gradient region 302 are integrally filled with a vertically arranged low-density carbon felt layer 5, the low-density carbon felt layer 5 is uninterrupted at the interface of the temperature gradient reinforcing region 301 and the inclined low-temperature gradient region 302, and the density of the low-density carbon felt layer 5 is 0.14g/cm 3 ；
And the carbon felt packing density of the high density barrier region 303 was 0.45g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The outer surface of the high-density blocking area 303 is coated with a high-temperature-resistant nanomaterial reflective coating, a tungsten-molybdenum steel reinforcing piece 8 is arranged between the inclined low-temperature gradient area 302 and the high-density blocking area 303, the tungsten-molybdenum steel reinforcing piece 8 comprises a first reinforcing portion 801 and a second reinforcing portion 802 which are integrally formed from top to bottom, the first reinforcing portion 801 is vertically arranged, and the first reinforcing portion 801 penetrates through the inclined low-temperature gradientThe interface between the region 302 and the high density blocking region 303 is such that the ratio of the heights of the first reinforcing portion 801 located in the inclined low temperature gradient region 302 to the first reinforcing portion 801 located in the high density blocking region 303 is 5:1, the second reinforcing portion 802 is inclined, and the inclination direction of the second reinforcing portion 802 is the same as that of the first support plate 701.
The preparation method of the single crystal furnace comprises the following steps: assembling the outer guide cylinder 1, the inner guide cylinder 2 and the supporting structure 7 to form a shell of the guide cylinder, and extracting the whole outline of a cavity area between the outer guide cylinder 1 and the inner guide cylinder 2, a cavity area between the first supporting disk 701 and the second supporting disk 702 and a cavity area between the first supporting disk 701 and the outer guide cylinder 1;
prefabricating the high-density carbon felt layer 4, the low-density carbon felt layer 5, the filling body of the high-density blocking area 303, the tungsten-molybdenum steel reinforcing member 8 and the tungsten-molybdenum steel sheet layer 6 into a cylindrical prefabrication body, wherein prefabrication comprises arranging the positions and the directions of the high-density carbon felt layer 4, the low-density carbon felt layer 5, the filling body of the high-density blocking area 303, the tungsten-molybdenum steel reinforcing member 8 and the tungsten-molybdenum steel sheet layer 6 according to the whole outline of the cavity area and the arrangement positions and the directions;
according to the overall outline of the cavity area, the cylindrical preform is trimmed into a filling body, and the shape of the filling body is the same as the overall shape of the cavity area;
the filling body, the outer guide cylinder 1, the inner guide cylinder 2 and the supporting structure 7 are assembled into the guide cylinder.
The method for preparing monocrystalline silicon by using the single crystal furnace is a Czochralski method.
Example 2
The procedure is as in example 1, except that the surface of the carbon felt filler in the high density barrier region 303 is not coated with a high temperature resistant nanomaterial reflective coating.
Example 3
The procedure of example 1 was followed except that no tungsten molybdenum steel reinforcement 8 was provided between the sloped low temperature gradient zone 302 and the high density barrier zone 303.
Example 4
The procedure is as in example 1, except that the bottom of the second cone section 202 and the bottom of the first cone section 102 are not connected by the support structure 7, that no high density blocking area 303 is provided, and that the bottom of the second cone section 202 and the bottom of the first cone section 102 are directly connected.
Example 5
The procedure of example 1 was followed, except that the temperature gradient enhancement zone was provided with 9 horizontally disposed high density carbon felt layers 4.
Example 6
The process was conducted as in example 1 except that the high-density carbon felt layer was horizontally disposed at a density of 0.168g/cm 3 The density of the vertically arranged high-density carbon felt layer is 0.168g/cm 3 The density of the high-density carbon felt layer which is obliquely arranged is 0.168g/cm 3 The density of the low-density carbon felt layer is 0.162g/cm 3 。
Example 7
The procedure is as in example 1, except that the high-density carbon felt layer 4 is disposed at an angle of 30 ° to the vertical.
Example 8
The procedure of example 1 was followed, except that the surface of the vertically disposed high density carbon felt layer 4 was not coated with a silicon nitride coating.
Example 9
The procedure of example 1 was followed, except that the surface of the high-density carbon felt layer 4, which was disposed obliquely, was not coated with a silicon nitride coating.
Example 10
The procedure of example 1 was followed, except that no tungsten-molybdenum steel sheet layer was provided on both sides of the vertically disposed high density carbon felt 4.
Comparative example 1
The procedure of example 1 was followed, except that the temperature gradient enhancement zone 301 was not filled with the horizontally disposed high density carbon felt layer 4.
Comparative example 2
The procedure of example 1 was followed except that the temperature gradient enhancement zone 301 was not filled with a vertically disposed high density carbon felt layer 4.
Comparative example 3
The procedure of example 1 was followed except that the sloped low temperature gradient zone 302 was not filled with the sloped high density carbon felt layer 4.
Test case
In the crystal pulling process, when the process enters an equal diameter stage after shoulder turning, the equal diameter power refers to the power value required by the equal diameter process, is stable power required to be maintained when the growth diameters of crystals are equal (diameter deviation is +/-0.5 mm) in the drawing growth process, and can be directly read from the feedback value of a power supply cabinet.
The periphery of the crystal bar which is perfectly normal is provided with 4 evenly distributed ridgelines which are parallel to the central line of the crystal bar, in the crystal pulling process, when the 4 ridgelines disappear, the ridgelines are called broken ridges or broken lines, after the ridgelines disappear, the CCD image recognition automatically detects the ridgelines disappear, namely the ridgelines are broken lines are abnormal, and the wire breaking rate of a single crystal furnace refers to the number of times/days of the broken lines.
The total breaking rate is the sum of the shouldering breaking rate and the equal-diameter breaking rate (the sum of the breaking rate of the shouldering process and the breaking rate of the equal-diameter process), the total breaking rate is more than 500 breaking rate, the equal-diameter length is more than 500mm, the equal-diameter length is less than or equal to 500mm, and the shouldering breaking rate is the breaking rate of the disappearance of 4 edge lines in the shouldering process.
The diameter control means that the single crystal furnace is provided with a CCD phase formation detection function, the diameter is automatically detected to be in a constant range (within +/-0.5 of deviation) through image processing and PID regulation, and when the deviation is large, the heating power is automatically regulated to maintain the relative stability of the diameter.
The single furnace per unit calculation method is the total available crystallization (normal ingot with high oxygen content, unqualified resistivity, etc. available for slicing) weight/day.
The results of measurements of the breakage rate, yield, pulverization of carbon felt, strength of heat-insulating layer and stability of the seed crystal production of examples 1 to 10 and comparative examples 1 to 3 are shown in Table 1.
TABLE 1
By comparing examples 1-10 with comparative examples 1-3, it can be seen that example 1 has the smallest isodiametric power, the lowest total breakage, and only 17% isodiametric breakage and shoulderingThe wire breakage rate is also lowest, the control effect on the diameter of the crystal bar is best, the deviation is +/-0.5 mm, the unit yield is best, the unit yield is 197 kg/day, the carbon felt is not pulverized at all, and the strength and the stability of the heat insulation layer are good. The surface of the carbon felt filler in the high-density blocking region 303 is coated with a high-temperature-resistant nanomaterial reflective coating, which is more beneficial to reducing the risk of breakage of the crystal pulling. No tungsten-molybdenum steel reinforcement 8 is arranged between the inclined low temperature gradient zone 302 and the high density blocking zone 303, which is more beneficial to controlling pulverization of carbon felt and improving strength and stability of the heat preservation layer. Connect the bottom of second cone section 202 and the bottom of first cone section 102 through bearing structure 7 to set up high dense blocking area 303, more do benefit to the reduction and pull out the line risk, improve the productivity ratio, improve the intensity and the stability of heat preservation. 2-8 high-density carbon felt layers 4 horizontally arranged are filled in the temperature gradient enhancement region 301 at intervals along the vertical direction, so that the risk of broken lines in crystal pulling is reduced, and the yield is improved. By making the density of the high-density carbon felt layer 4 0.17g/cm 3 -0.24g/cm 3 The density of the low density carbon felt layer 5 was 0.08g/cm 3 -0.16g/cm 3 The method is more beneficial to reducing the risk of crystal pulling and wire breakage, controlling the diameter, improving the yield, inhibiting the pulverization of the carbon felt and improving the strength and the stability of the heat preservation. The inclined angle between the high-density carbon felt layer 4 and the vertical direction is 5-25 degrees, so that the risk of broken wires in crystal pulling is reduced. The silicon nitride coating is coated on the surfaces of the high-density carbon felt layer 4 which is vertically arranged and the high-density carbon felt layer 4 which is obliquely arranged, so that the risk of broken wires in pulling is reduced. Through set up tungsten molybdenum steel sheet layer in the both sides of the high density carbon felt 4 of vertical setting, more do benefit to the reduction and pull out broken line risk, restrain the carbon felt and powdered, improve the intensity and the stability of heat preservation. The high-density carbon felt layer 4 arranged at the non-filling level of the temperature gradient enhancement zone 301 increases the isodiametric power, increases the risk of crystal pulling and wire breakage, is unfavorable for controlling the diameter, greatly reduces the unit yield, the carbon felt is easy to pulverize, reduces the strength and stability of the heat insulation layer, and the high-density carbon felt layer 4 arranged vertically is not filled in the temperature gradient enhancement zone 301, increases the isodiametric power, increases the risk of crystal pulling and wire breakage, is unfavorable for controlling the diameter, greatly reduces the unit yield, the carbon felt is easy to pulverize, reduces the strength and stability of the heat insulation layer, and is suitable for being used in the inclined low-temperature gradient zone 3 02 do not set up high density carbon felt layer 4, can increase the constant diameter power, increase and draw the broken string risk, be unfavorable for controlling the diameter, reduce the unit yield by a wide margin, reduce the intensity and the stability of heat preservation.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. A draft tube for a single crystal furnace, comprising:
the outer guide cylinder (1), wherein the outer guide cylinder (1) comprises a first straight cylinder section (101) and a first conical cylinder section (102) from top to bottom, and the first conical cylinder section (102) is gradually reduced from top to bottom;
the inner guide cylinder (2) comprises a second straight cylinder section (201) and a second conical cylinder section (202) from top to bottom, the second conical cylinder section (202) is gradually reduced from top to bottom, the bottom of the second conical cylinder section (202) is connected with the bottom of the first conical cylinder section (102), and the vertical height of the second straight cylinder section (201) is smaller than that of the first straight cylinder section (101);
A carbon felt filling region (3), wherein the carbon felt filling region (3) comprises a temperature gradient enhancement region (301) and an inclined low temperature gradient region (302), the temperature gradient enhancement region (301) and the inclined low temperature gradient region (302) are positioned in a cavity region between the outer guide cylinder (1) and the inner guide cylinder (2), the temperature gradient enhancement region (301) is positioned in a cavity region between the second straight cylinder section (201) and the outer guide cylinder (1), and the inclined low temperature gradient region (302) is positioned in a cavity region between the second taper cylinder section (202) and the outer guide cylinder (1);
the carbon felt filling area (3) is filled with a high-density carbon felt layer (4) and a low-density carbon felt layer (5) filled around the high-density carbon felt layer (4), the low-density carbon felt layer (5) is vertically arranged, the temperature gradient increasing area (301) is filled with the high-density carbon felt layer (4) horizontally arranged and vertically arranged, the inclined low-temperature gradient area (302) is filled with the high-density carbon felt layer (4) obliquely arranged, and the inclined direction of the high-density carbon felt layer (4) obliquely arranged is the same as the inclined direction of the second cone section (202);
The density of the high-density carbon felt layer (4) which is horizontally arranged, vertically arranged and obliquely arranged is 0.17g/cm 3 -0.24g/cm 3 The density of the low density carbon felt layer (5) is 0.08g/cm 3 -0.16g/cm 3 。
2. A draft tube according to claim 1 wherein the temperature gradient enhancement zone (301) is vertically spaced apart filled with 2-8 horizontally disposed layers (4) of high density carbon felt.
3. Guide shell according to claim 1, characterized in that the surface of the vertically arranged high-density carbon felt layer (4) and/or the obliquely arranged high-density carbon felt layer (4) is coated with a ceramic coating.
4. Guide cylinder according to claim 1, characterized in that tungsten-molybdenum steel sheet layers (6) are obliquely arranged on both sides of the high-density carbon felt layer (4) arranged vertically, and the horizontal distance from the upper part of the tungsten-molybdenum steel sheet layers (6) to the high-density carbon felt layer (4) arranged vertically is smaller than the horizontal distance from the lower part of the tungsten-molybdenum steel sheet layers (6) to the high-density carbon felt layer (4) arranged vertically.
5. A guide shell according to claim 1, characterized in that the high-density carbon felt layer (4) is arranged obliquely at an angle of 5-25 ° to the vertical.
6. A guide shell according to claim 1, characterized in that the bottom of the guide shell is provided with a supporting structure (7), the supporting structure (7) comprises a first supporting disc (701) and a second supporting disc (702), the first supporting disc (701) is arranged obliquely, the second supporting disc (702) is arranged horizontally, the upper part of the first supporting disc (701) is connected with the bottom of the inner guide shell (2), the outer part of the second supporting disc (702) is connected with the bottom of the outer guide shell (1), and the inner part of the second supporting disc (702) is connected with the lower part of the first supporting disc (701);
the carbon felt filling area (3) further comprises a high-density blocking area (303), the high-density blocking area (303) is positioned in a cavity area between the first supporting disc (701) and the second supporting disc (702) and a cavity area between the first supporting disc (701) and the outer guide cylinder (1), and the filling density of the carbon felt in the high-density blocking area (303) is 0.3g/cm 3 -0.5g/cm 3 。
7. The guide shell according to claim 6, wherein a reinforcement (8) is arranged between the inclined low temperature gradient zone (302) and the high-density blocking zone (303), the reinforcement (8) comprises a first reinforcement part (801) and a second reinforcement part (802) which are integrally formed from top to bottom, the first reinforcement part (801) is vertically arranged, and the first reinforcement part (801) passes through an interface between the inclined low temperature gradient zone (302) and the high-density blocking zone (303); the second reinforcement part (802) is obliquely arranged, and the oblique direction of the second reinforcement part (802) is the same as the oblique direction of the first support disc (701); the reinforcement (8) is a tungsten molybdenum steel reinforcement.
8. A method of making a guide shell according to any one of claims 1 to 7, comprising the steps of:
assembling an outer guide cylinder (1) and an inner guide cylinder (2) to form a shell of the guide cylinder, extracting the outline of a cavity area between the outer guide cylinder (1) and the inner guide cylinder (2),
prefabricating a high-density carbon felt layer (4) and a low-density carbon felt layer (5) into a cylindrical prefabrication body, said prefabrication comprising arranging the positions and directions of the high-density carbon felt layer (4) and the low-density carbon felt layer (5) according to the outline of the cavity area and the positions and directions of the high-density carbon felt layer (4) and the low-density carbon felt layer (5) according to any one of claims 1 to 7;
trimming the cylindrical preform into a filling body according to the outline of the cavity area, wherein the shape of the filling body is the same as that of the cavity area;
and assembling the filling body, the outer guide cylinder (1) and the inner guide cylinder (2) into the guide cylinder.
9. A single crystal growing furnace, comprising: a guide cylinder, wherein the guide cylinder is a guide cylinder according to any one of claims 1 to 7 or a guide cylinder prepared by the preparation method according to claim 8;
The crucible (9), crucible (9) are located the below of draft tube, crucible (9) have silicon melt holding portion, the internal diameter of crucible (9) is greater than the external diameter of outer draft tube (1) first section of cylinder (101).
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| KR20110095474A (en) * | 2010-02-19 | 2011-08-25 | 네오세미테크 주식회사 | Graphite cone restructure |
| CN102167325B (en) * | 2010-12-27 | 2012-07-25 | 湖南南方搏云新材料有限责任公司 | Carbon/carbon heat screen of polysilicon hydrogenation furnace and manufacture method thereof |
| CN202279867U (en) * | 2011-06-27 | 2012-06-20 | 湖南金博复合材料科技有限公司 | Carbon/carbon composite guide cylinder |
| CN102296355B (en) * | 2011-06-27 | 2013-12-11 | 湖南金博复合材料科技有限公司 | Guide shell made from carbon/carbon composite material and production method |
| CN202717873U (en) * | 2012-06-20 | 2013-02-06 | 陕西天宏硅材料有限责任公司 | Flow guide cylinder used for drawing large diameter semiconductor grade monocrystalline silicon rod |
| CN202954132U (en) * | 2012-12-04 | 2013-05-29 | 英利能源（中国）有限公司 | Guide cylinder for single crystal furnace |
| CN107244938B (en) * | 2017-02-23 | 2022-07-26 | 辽宁奥亿达新材料有限公司 | Manufacturing method of high-performance composite carbon fiber guide cylinder |
| CN210030952U (en) * | 2019-04-09 | 2020-02-07 | 浙江明峰电子科技有限公司 | Guiding device for monocrystalline silicon production |
| CN212840144U (en) * | 2020-08-24 | 2021-03-30 | 新疆晶科能源有限公司 | Heat insulation structure in draft tube |
| CN114197034B (en) * | 2020-09-02 | 2024-08-16 | 西安奕斯伟材料科技股份有限公司 | Combined sleeve of single crystal furnace and single crystal furnace |
| CN215560795U (en) * | 2021-05-13 | 2022-01-18 | 弘元新材料(包头)有限公司 | Guide cylinder for large-size monocrystalline silicon rod |
| CN217378090U (en) * | 2022-02-24 | 2022-09-06 | 西安维柯亿新能源科技有限公司 | Quartz guide cylinder for single crystal furnace |
| CN217709752U (en) * | 2022-05-10 | 2022-11-01 | 包头美科硅能源有限公司 | Draft tube for prolonging service life of graphite felt |
| CN115323479A (en) * | 2022-08-16 | 2022-11-11 | 晶澳太阳能有限公司 | Guide cylinder and preparation method thereof |
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