CN109097824A - Monocrystalline silicon growing combined type silica crucible and preparation method thereof - Google Patents
Monocrystalline silicon growing combined type silica crucible and preparation method thereof Download PDFInfo
- Publication number
- CN109097824A CN109097824A CN201710471258.3A CN201710471258A CN109097824A CN 109097824 A CN109097824 A CN 109097824A CN 201710471258 A CN201710471258 A CN 201710471258A CN 109097824 A CN109097824 A CN 109097824A
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- Prior art keywords
- crucible
- carbon fiber
- quartzy
- hole
- sintering tube
- Prior art date
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 286
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 110
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 169
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 157
- 239000004917 carbon fiber Substances 0.000 claims abstract description 157
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 157
- 235000013312 flour Nutrition 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 60
- 239000013078 crystal Substances 0.000 claims abstract description 35
- 239000004744 fabric Substances 0.000 claims abstract description 13
- 238000003723 Smelting Methods 0.000 claims abstract description 10
- 238000004080 punching Methods 0.000 claims description 78
- 239000007788 liquid Substances 0.000 claims description 58
- 239000010453 quartz Substances 0.000 claims description 58
- 238000000034 method Methods 0.000 claims description 21
- 229910002114 biscuit porcelain Inorganic materials 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 7
- 239000006004 Quartz sand Substances 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000010891 electric arc Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052571 earthenware Inorganic materials 0.000 claims description 3
- 230000002459 sustained effect Effects 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims 1
- 235000021050 feed intake Nutrition 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000001360 synchronised effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 56
- 238000004519 manufacturing process Methods 0.000 description 18
- 238000010586 diagram Methods 0.000 description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 11
- 239000002356 single layer Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 125000004122 cyclic group Chemical group 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000011265 semifinished product Substances 0.000 description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- 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
- C30B15/002—Continuous growth
-
- 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
Abstract
The present invention relates to a kind of monocrystalline silicon growing combined type silica crucibles and preparation method thereof.The combined type silica crucible includes the outer crucible body of crucible and crucible inner cylinder, and the outer crucible body of crucible includes outer cylindrical portion and crucible bottom, and crucible inner cylinder is constituted by carbon fiber sintering tube and around the quartzy agglomerated material that carbon fiber sintering tube is arranged.The quartzy agglomerated material is integral piece made of the silica flour being covered in carbon fiber sintering tube is sintered.The carbon fiber sintering tube is the tubular fabric for made of being woven and being sintered as carbon fiber up and down.In use, crucible inner cylinder is placed in the inside of the outer crucible body of crucible, and crucible body outside crucible is divided into crystal growth area and two regions inside and outside the smelting material area that feeds intake.The configuration of the present invention is simple separates impurity, can be realized feed intake, material, crystal growth and separation impurity is synchronous carries out and high temperature continuous working period is long.
Description
Technical field
The present invention relates to monocrystalline silicon manufacturing technology fields, and in particular to a kind of monocrystalline silicon growing combined type silica crucible and
Preparation method.
Background technique
Monocrystalline silicon is mainly used for photovoltaic power generation, photovoltaic power generation be the clean energy in current renewable energy, using too
Luminous energy is transformed into electric energy by sunlight irradiation, is the clean energy resource that the current whole world is generally acknowledged and greatly developed, industry development prospect is very
It is good, but due to monocrystalline silicon growing when requires liquid level steady and temperature plateau, to process conditions require harsh and energy consumption is high,
Cost is very high, hinder to a certain extent photovoltaic power generation widely popularize and universalness, therefore meeting monocrystalline silicon growing item
While part, reducing energy consumption and production costs is current urgent problem.Monocrystalline silicon growing is that photovoltaic produces with silica crucible
The Primary Component that monocrystalline silicon is produced in industry, be it is a kind of so that polysilicon raw materials is melted the container to form silicon melt, need to protect for a long time
The high temperature at 1420 DEG C ~ 1500 DEG C is held, and the defect of usually quartz ware is exactly when temperature reaches 1300 DEG C or more, quartz is just
It can soften, intensity is gradually reduced, the effect of container can not be individually undertaken, it is therefore desirable to physical deformation is small when silica crucible high temperature,
It is the critical issue to reduce energy consumption and production costs.
Currently, reducing there are mainly two types of the methods that silica crucible high-temperature physics deform both at home and abroad, first method is to pass
A kind of silicon carbide that phase transition will not occur under molten silicon treatment temperature or silicon nitride etc. are selected on the basis of system single layer crucible
Material makes crucible base, so that crucible base is not had Plastic phase, and then guarantee that specific times and its physics can be used in crucible
Integrality is without any significant deterioration.Second is that an internal layer earthenware is arranged that is, in former single layer crucible using the double-deck silica crucible
Crucible, the material of inside and outside crucible are silicon carbide, silicon nitride or zirconium oxide, and inner crucible bottom is equipped with through-hole, and with former single layer
Dry crucible shares same crucible bottom, and the interlayer between inner crucible and former single layer crucible is charging, material region, table in inner crucible
Face limited area is crystal growth zone, and two regions are separated by inner crucible, and inner crucible bottom is equipped with through-hole and can protect
Liquid level is steady when silicon liquid after card fusing flows into crystal growth zone from bottom, may be implemented to feed intake, material, crystal pulling can be with
It carries out simultaneously, continuous crystal-pulling may be implemented, shorten the working time of silica crucible at high temperature, and then the physics for reducing crucible becomes
Shape.
Chinese patent literature CN101370968A(application number 200780003063.0) disclose a kind of processing molten silicon
Crucible, the document belong to the first above-mentioned single layer crucible, which includes the silicon carbide that weight content is 65% or more, weight
The silicon oxide or silicon nitride that content is 12% ~ 30%, wherein silicon oxide or silicon nitride is coated in the inner surface of silicon carbide layer, for limiting
Determine crucible internal capacity.This kind of single layer crucible may be reused repeatedly, and physical deformation is small, but required silicon carbide or nitridation
Silicon raw material is expensive, and crucible cost of manufacture is high.In addition, when growing monocrystalline silicon using single layer crucible crystal growth need to be being carried out
Polycrystalline silicon raw material is filled to maximum limiting value by preceding elder generation, and temperature is then risen to 1500 DEG C or so progress materials, and material is completely melt
Afterwards, simultaneously then equilibrium temperature carries out crystal growth at 1420 DEG C or so for cooling, i.e., feed intake when growing monocrystalline silicon with single layer crucible/
Material/crystal growth three process must be separated and be carried out, and otherwise can be interfered with each other, be influenced the stationarity of liquid level and temperature, lead
Cause crystal can not normal growth, cannot get qualified monocrystal.Therefore, when carrying out crystal growth using single layer crucible, Zhi Nengshi
Blowing out again after a furnace is pulled, and the single layer crucible more renewed re-starts/material/crystal growth the process that feeds intake.Crystal growth
When 1500 DEG C or so in furnace of high temperature need to be reduced and stablize at 1420 DEG C or so, blowing out need 1420 DEG C or so in furnace
High temperature drops to 100 DEG C hereinafter, whole process loses a large amount of energy consumption, and wastes a large amount of time, has seriously affected list
The production capacity of brilliant furnace.
Chinese patent literature CN202246997U(application number 201120350790.8) disclose a kind of double crucible, this article
Offer and belong to above-mentioned second of double crucible, although realize feed intake, material, crystal pulling at the same carry out and can continuous crystal-pulling, avoid
Descent of temperature when crystal growth, but crucible material therefor higher cost.
Chinese patent literature CN102660768A (application number 201210166266.4) discloses a kind of monocrystaline silicon stove use
The preparation process of carbon/carbon composite material crucible, the production method that the document specifically discloses three-dimensional carbon fiber crucible green body, i.e., with
The polyacrylonitrile-based carbon fibre of T-700 is raw material, is separately woven into net tire and charcoal cloth, and be allowed to be combined into felt by needle thorn,
Felt is fastened on the mold of crucible shape, covers one layer of charcoal cloth thereon, then cover one layer of net tire, is so folded and places and lead to
It crosses needle thorn and is allowed to compound, obtain the three-dimensional crucible preform of the standard that density is 0.45g/cm3.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide it is a kind of cost is relatively low and use in production capacity it is higher, high
Temperature is persistently longer using the time and guarantees monocrystalline silicon growing combined type silica crucible and preparation method thereof of crystal high-quality.
Realizing the technical solution for providing a kind of combined type silica crucible in the object of the invention is: monocrystalline silicon of the invention is raw
Long to use combined type silica crucible, crucible body outside the crucible including opening upwards, the outer crucible body of crucible is the sintering integrated part of quartz.Monocrystalline silicon
Growth combined type silica crucible further includes crucible inner cylinder.
The outer crucible body of crucible includes outer cylindrical portion and crucible bottom；The top and crucible bottom of outer cylindrical portion are connected with each other.
Crucible inner cylinder is cylinder up and down, by carbon fiber sintering tube and around the quartz of carbon fiber sintering tube setting
Agglomerated material is constituted；The carbon fiber sintering tube is the tubular sinter made of being woven and be sintered as carbon fiber up and down；
The side wall of carbon fiber sintering tube is equipped at least two liquid flow hole and multiple quartzy holes in dispersed distribution.Quartzy agglomerated material
To be covered on the quartzy integral piece being linked together made of being sintered in carbon fiber sintering tube as silica flour, the quartz integral piece
It is not placed only on the interior outside of crucible inner cylinder and the surface of downside, is further filled in each quartzy hole, but also be covered on
On the hole wall of each liquid flow hole.The quartz that covers on the hole wall of each liquid flow hole of its carbon fiber sintering tube of crucible inner cylinder is burnt
The position for tying material, forms the material through hole through its side wall of crucible inner cylinder, and the material passes through hole number
It is identical as the quantity of liquid flow hole.In use, crucible inner cylinder is placed on the inner sidewall of the crucible bottom of the outer crucible body of crucible, and in crucible
The lateral wall of cylinder and the inner sidewall spacing distance of outer cylindrical portion, so that crucible body outside crucible is divided into two regions.
Further, the carbon fiber sintering tube of crucible inner cylinder is cylindric sinter.Crucible inner cylinder is cylinder；Carbon
The aperture of each liquid flow hole of fiber sintering cylinder is 20 to 60mm, and is located at the 15mm to 40mm high of carbon fiber sintering tube bottom
Place.Material through hole is Chong Die with the central axis of liquid flow hole.The quartzy hole of carbon fiber sintering tube is uniformly arranged, and gets out of the way the liquid
Discharge orifice.Further, the aperture in the quartzy hole of carbon fiber sintering tube is 20 ± 10mm, and quartzy being uniformly arranged for hole refers to stone
English hole by between the upper and lower every on 40mm ± 10mm and sustained height between left and right every 40mm ± 10mm in the way of be arranged.
Further, the quartzy integral piece of crucible inner cylinder is divided into quartzy internal layer, quartz according to the difference of location
Quartz in outer layer, quartzy bottom and hole；Quartz refers to the quartz riddled in each quartzy hole and is covered on each liquid in hole
Quartz on the hole wall of discharge orifice.
Further, the outer diameter of quartzy internal layer is the internal diameter of carbon fiber sintering tube, and the internal diameter of quartzy internal layer is earthenware
The internal diameter of crucible inner cylinder；The internal diameter of quartzy outer layer is the outer diameter of carbon fiber sintering tube, and the outer diameter of quartzy outer layer is in crucible
The outer diameter of cylinder；The internal diameter of quartzy bottom is the internal diameter of crucible inner cylinder, and the outer diameter of quartzy bottom is crucible inner cylinder
Outer diameter.The thickness of carbon fiber sintering tube, quartzy internal layer and quartzy outer layer three is identical.The outer surface of quartzy internal layer and carbon fiber are burnt
The inner surface of knot cylinder connects, and the inner surface of quartzy outer layer connects with the outer surface of carbon fiber sintering tube.The upper surface of quartzy bottom
Connect respectively with the lower surface homogeneity of the lower surface of quartzy internal layer, quartzy outer layer, and connects with the lower surface of carbon fiber sintering tube.
The quartzy inner and outer ends end face relative to the side wall inside table with the outer surface of quartzy internal layer and quartzy outer layer respectively in hole
Face homogeneity connects.
Further again, the crucible bottom of the outer crucible body of crucible further includes the supporting part being arranged on inner sidewall, the carrying
Portion is located at the top sides of crucible bottom along the inner sidewall of lower section, thus the part of the inner sidewall of crucible bottom being located above supporting part
The as top of the inner sidewall of crucible bottom, the part of the inner sidewall of crucible bottom being located at below supporting part are the inside of crucible bottom
The lower part of wall, that is to say, the inner sidewall of crucible bottom be divided into according to order from top to bottom the top of inner sidewall, supporting part and
The lower part of inner sidewall.The bottom surface of crucible inner cylinder can be with the supporting part close contact of crucible body outside crucible when use.Again more
Further, the outer cylindrical portion of the outer crucible body of crucible is cylindrical shape, the spherical shape of the inner and outer surfaces of crucible bottom, and the position of the centre of sphere
The full-size of the same position being arranged on the central axis of outer cylindrical portion, the surrounding of crucible bottom is outer no more than outer cylindrical portion
Diameter.
It is further again, the outer crucible body of crucible be 99.999% by purity quartz sand powder through sintering integrated molding,
And the homogeneity integral piece that outer cylindrical portion therein and crucible bottom are connected together.Outer cylindrical portion with a thickness of 15mm to 60mm,
Crucible bottom with a thickness of 15mm to 60mm, the thickness of outer cylindrical portion is not more than the thickness of crucible bottom.
The method for preparing monocrystalline silicon growing combined type silica crucible as described above, comprising the following steps:
1. the preparation of the outer crucible body of crucible: the first step rotates prefabricated punching block with 60 to 80 revs/min of speed, then
Silica flour is poured into punching block, silica flour is equably scraped mould inner wall with scraper plate in punching block rotation process.Since mold turns
Dynamic, silica flour, which can be attached to due to the effect of centrifugal force on mould inner wall, forms quartzy bisque.
Second step, the structure for controlling quartzy bisque with scraper plate are identical with the structure of crucible body outside preset crucible；When in punching block
When the thickness of the quartzy bisque of wall attachment reaches 15mm to 60mm green body is shaped substantially, to obtain outer pan body blank.
Either, the shape for controlling quartzy bisque with scraper plate is identical with the shape of crucible body outside default crucible for second step.Work as steel
The quartzy powder layer thickness of mould inner wall attachment shapes green body substantially when reaching 15mm, then with scraper plate green body pot bottom
The top sides of inner sidewall scrape supporting part along lower section.
Third step, will with outer pan body blank punching block be pushed into high temperature furnace, with the external crucible chaeta base of electric arc heating mode into
Row heat-agglomerating, sintering temperature are not less than 1750 DEG C ± 2 DEG C.It sinters post-tensioning to go out punching block and stop operating, outer pan body at this time
Blank has become crucible outer pan body；It is cooled to after room temperature to take out and sinters the outer crucible body of crucible in punching block, so far the outer crucible of crucible
Body completes.
2. the preparation of carbon fiber sintering tube: after being woven into cylindraceous fabric by carbon fiber, then being sintered, burn under vacuum conditions
Junction temperature is not less than 2800 DEG C, passes through mechanical punching and finishing on the cylindraceous fabric after natural cooling, then after sintering, and
Obtain the carbon fiber sintering tube with liquid flow hole and quartzy hole.
3. the preparation of crucible inner cylinder: the first step, make the prefabricated punching block for being used to prepare crucible inner cylinder with 60 to 80 turns/
The speed of minute is rotated, and silica flour is subsequently poured into.Punching block rotates so that silica flour is attached to mold by centrifugal action
On inner wall, the pressure that the silica flour being attached on die inside wall carries out uniformity is scraped with scraper plate again in the rotation of punching block, from
And form the silica flour outer layer of 5mm to 30mm thickness.Prefabricated carbon fiber sintering tube is put into prefabricated be used for upside down
In the punching block for preparing crucible inner cylinder, even if also the bottom of carbon fiber sintering tube is upward, and make the outer of carbon fiber sintering tube
Surface and the inner surface of silica flour outer layer are affixed.After placing carbon fiber sintering tube, continue to add quartz into the punching block of rotation
Powder, then with scraper plate silica flour is equably scraped on the inner surface and bottom surface of carbon fiber sintering tube, and scrape carbon fiber
In the quartzy hole of sintering tube and liquid flow hole.Punching block rotates so that silica flour is attached to the interior of carbon fiber sintering tube by centrifugal action
On wall, while part silica flour passes through the liquid flow hole of carbon fiber sintering tube under the influence of centrifugal force and quartzy hole and is filled in carbon
Gap between the outer surface of fiber sintering cylinder and the inner surface of silica flour outer layer；When the inside and outside and bottom of carbon fiber sintering tube
The quartzy bisque of 5mm to 30mm thickness, and outer surface and silica flour outer layer of the silica flour full of carbon fiber sintering tube are adhered in surface
Inner surface between gap and carbon fiber sintering tube each quartzy hole and liquid flow hole after, then inner cylinder base is formd in punching block
Body；Then the punching block of the rotation by this with the inner cylinder green body is pushed into high temperature furnace.
The carbon fiber sintering tube prepared either, is placed in prefabricated be used to prepare first with upside down by the first step
On the inner sidewall of the dome shape bottom of the punching block of crucible inner cylinder, even if also the bottom of carbon fiber sintering tube is upward, and make
The inner surface interval 5mm of the outer surface of carbon fiber sintering tube and prefabricated punching block is to 30mm distance；Then make prefabricated punching block with 60
It is rotated to 80 revs/min of speed, then pours into silica flour；In punching block rotation process, silica flour is scraped to carbon fiber with scraper plate
On the inner sidewall for tieing up sintering tube；Punching block rotates so that the silica flour on the inner sidewall of carbon fiber sintering tube is passed through by centrifugal action
Quartzy hole and liquid flow hole and the region being filled between the outer surface of carbon fiber sintering tube and prefabricated punching block inner surface.To stone
Region and carbon fiber sintering tube of the English powder filling completely between the outer surface and prefabricated punching block inner surface of carbon fiber sintering tube
Behind each quartz hole and liquid flow hole, then silica flour was poured into, and scraped silica flour to the inner sidewall of carbon fiber sintering tube with scraper plate
In bottom surface, after the inner sidewall of carbon fiber sintering tube and the quartzy bisque of bottom surface attachment 5mm to 30mm thickness, then pre-
Inner cylinder green body is formd in punching block processed；Then the punching block of the rotation with the inner cylinder green body is pushed into high temperature furnace.
Second step carries out heat-agglomerating to the silica flour for forming inner cylinder green body with electric arc heating mode, and sintering temperature is
1750℃±2℃；Post-tensioning is sintered to go out punching block and stop operating, it is to be cooled to obtaining composite body after room temperature.
Third step is taken out the composite body prepared and is cut in height to the bottom of composite body, cutting
Size and position are corresponding with the size of carbon fiber sintering tube, and 2 to 5mm thick quartzy bottoms are left after cutting, and compound
Green body bottom surface and top surface are annular plane.
4th step is got and liquid flow hole at each position of the setting liquid flow hole apart from carbon fiber sintering tube bottom of green body
With coaxial line and aperture is 80% to the 90% material through hole hole in liquid flow hole aperture, and crucible inner cylinder is so far made.
It is further again, the preparation step of monocrystalline silicon growing combined type silica crucible further include: 4. will prepare
Crucible outer barrel is placed in the outer crucible body of crucible, and the bottom that will be close to the crucible inner cylinder of material through hole is placed in crucible outer pan body
Crucible bottom inner sidewall on or be placed on the top sides of crucible bottom along the supporting part on the inner sidewall of lower section, and finally make
At monocrystalline silicon growing combined type silica crucible.
The present invention has the effect of positive: (1) the outer crucible body of crucible of the invention can be divided into setting supporting part and be not provided with
Supporting part two ways.So of the invention in use, when the bottom of crucible inner cylinder is placed in outside crucible in crucible body, just
There is the bottom by crucible inner cylinder to be placed directly on the inner sidewall of the crucible bottom of crucible body outside crucible and be placed in holding for crucible body outside crucible
Two ways on load portion.Both front and back mode makes crucible inner cylinder up and down that crucible body outside crucible is divided into crystal life
Two regions inside and outside long area and the smelting material area that feeds intake.Since the certain eminence in side passes through crucible inner cylinder equipped with material on its bottom
Hole, and the upper edge of the side wall of the supporting part of the outer crucible body of crucible is set according to the lower end of the material through hole lower than crucible inner cylinder
Set, outside the bottom of crucible inner cylinder and crucible between the crucible bottom of crucible body in close contact state (due to see below), from
And the impurity that can prevent the single crystal silicon materials for entering the smelting material area that feeds intake from generating in material enters crystal growth area, may be implemented
Feed intake, material, crystal growth and impurity separation it is synchronous progress, to save a large amount of electricity charge and labour cost, and significantly
Improve the production capacity of crystal quality and crystal growth.In use, since crucible inner cylinder will be subjected to 1400 DEG C or so of high temperature,
At this temperature, the quartz of the pot bottom of the outer crucible body of quartz and crucible of crucible inner cylinder bottom is softened, so, even if
Between the two or there is gap, close contact between the two has also been formed at this time.(2) when crucible body setting carrying outside crucible
When portion, supporting part also acts as limitation crucible inner cylinder and is displaced in the horizontal direction, to protect in addition to playing the role of carrying
Demonstrate,prove the stabilization of mutual close contact relationship.(3) Strength Changes very little of the carbon fiber sintering tube at 2500 DEG C or more, therefore by
The crucible inner cylinder that carbon fiber sintering tube is combined with quartz avoids pure quartz ware at 1300 DEG C or more because softening, deforming
Lead to not the effect for serving as quartz container, and the crucible inner cylinder physical efficiency equipped with carbon fiber sintering tube of the invention is at 1600 DEG C
The intensity remained intact below, and it is able to maintain the original advantage of quartz ware.(4) single set monocrystalline silicon growing group of the invention
The working time of box-like silica crucible at high temperature is up to 720 hours to 1000 hours, and each production cycle is extended to
7 to 10 times of prior art, the service life of combined type silica crucible are accordingly then 7 to 10 times that common crucible uses the time.
Therefore, the production capacity of single set monocrystalline silicon growing combined type silica crucible is much higher than common crucible, and crucible consumption is also significantly
It reduces.(5) combined type silica crucible of the invention can long time continuous working, and can realize the smelting material area that feeds intake during the work time
Domain temperature is 1500 DEG C or so, while the temperature of crystal growth zone is 1420 DEG C or so, is avoided because frequently replacing crucible, adjustment
Material temperature and crystal pulling temperature, and in-furnace temperature is raised and lowered repeatedly, and then save a large amount of electric energy.(6) in each production week
After phase, the quartz of the carbon fiber sintering tube periphery of crucible inner cylinder can be broken into pieces remove, obtain carbon fiber sintering tube
It can continue on for manufacturing crucible inner cylinder and reusing, so that the manufacturing cost of combined type silica crucible of the invention
It is greatly reduced.
Detailed description of the invention
Fig. 1 is the stereoscopic schematic diagram of monocrystalline silicon growing combined type silica crucible of the invention.
Fig. 2 is the schematic top plan view of Fig. 1.
Fig. 3 is the A-A schematic cross-sectional view of Fig. 2.
Fig. 4 is the partial enlargement diagram in Fig. 3 at D.
Fig. 5 is the stereoscopic schematic diagram of the crucible inner cylinder in Fig. 1.
Fig. 6 is the main view of Fig. 5.
Fig. 7-1 is the B-B schematic cross-sectional view of Fig. 6.
Fig. 7-2 is the partial enlargement diagram in Fig. 7-1 at E.
Fig. 8-1 is a kind of schematic diagram of the carbon fiber sintering tube namely carbon fiber sintering tube of the invention in Fig. 6.
Fig. 8-2 is the D-D schematic cross-sectional view of Fig. 8-1.
Fig. 8-3 is the partial enlargement diagram in Fig. 8-2 at G.
Fig. 9 is a kind of stereoscopic schematic diagram of the crucible outer pan body in Fig. 1.
Figure 10 is the schematic top plan view of Fig. 9.
Figure 11 is the C1-C1 schematic cross-sectional view of Figure 10.
Figure 12 is the partial enlargement diagram in Figure 11 at F1.
Figure 13 is another structural schematic diagram of the outer crucible body of crucible of the invention, and institute's apparent direction is to overlook.
Figure 14 is the C2-C2 schematic cross-sectional view of Figure 13.
Figure 15 is the partial enlargement diagram in Figure 14 at F2.
Figure 16 is another structural schematic diagram of the outer crucible body of crucible of the invention, and institute's apparent direction is to overlook.
Figure 17 is the C3-C3 schematic cross-sectional view of Figure 16.
Figure 18 is the partial enlargement diagram in Figure 17 at F3.
Figure 19 is the 4th kind of structural schematic diagram of the outer crucible body of crucible of the invention, and institute's apparent direction is to overlook.
Figure 20 is the C4-C4 schematic cross-sectional view of Figure 19.
Label in above-mentioned attached drawing is as follows:
The outer crucible body 1 of crucible, outer cylindrical portion 11, crucible bottom 12, supporting part 13, cyclic annular engaging portion 13-1, side wall 13-2, crucible inner cylinder
2, carbon fiber sintering tube 21, liquid flow hole 21-1, liquid flow hole 21-2, quartzy internal layer 22, quartzy outer layer 23, quartz top 24, Kong Zhong
Quartz 25, material through hole 26.
Specific embodiment
(embodiment 1, combined type silica crucible and preparation method thereof)
See that Fig. 1 to Fig. 3, the monocrystalline silicon growing combined type silica crucible of the present embodiment include crucible body 1 and crucible inner cylinder outside crucible
Body 2.
See that Fig. 9 to Figure 12, the outer crucible body 1 of crucible and crucible inner cylinder 2 are integrated, wherein the outer crucible body 1 of crucible is opening
The upward sintering integrated part of quartz.The outer crucible body 1 of crucible includes outer cylindrical portion 11 interconnected and crucible bottom 12, the top of crucible bottom 12
Inner sidewall below portion edge is equipped with supporting part 13, and the part for being located at 13 top of supporting part of the inner sidewall of crucible bottom 12 is
The part for being located at 13 lower section of supporting part on the top of the inner sidewall of crucible bottom 12, the inner sidewall of crucible bottom 12 is crucible bottom 12
The lower part of inner sidewall.Supporting part 13 have ring-type engaging portion 13-1 and be located at ring-type engaging portion 13-1 top and with cyclic annular engaging portion
Side wall 13-2 of the 13-1 outer side edges along vertical connection.The internal diameter of outer cylindrical portion 11 is 820mm, outer diameter 850mm, is highly 280mm.
Crucible bottom 12 is dome shape, and the radius of a ball of inner sidewall is 838mm, and the radius of a ball of lateral wall is 853mm.
See that Fig. 3 to Fig. 7-2, crucible inner cylinder 2 are cylinder up and down, and by carbon fiber sintering tube 21 and surrounds carbon
The quartzy agglomerated material that fiber sintering cylinder 21 is arranged is constituted.The quartzy agglomerated material is to be covered in carbon fiber sintering tube 21
Silica flour be sintered made of integral piece namely crucible inner cylinder 2 interior outside and upper and lower side surface be quartz sintering material
Material.In the present embodiment, crucible inner cylinder 2 is cylindrical shape, and outer diameter 750mm, internal diameter 720mm are highly 260mm.
See Fig. 8-1 to Fig. 8-3, carbon fiber sintering tube 21 is the cylindrical object warp being coiled by the fabric that carbon fiber is woven into
Tubular sinter up and down made of high temperature is sintered under the state or vacuum state for being full of nitrogen is crossed, and carbon fiber is burnt
The side wall for tying cylinder 21 is equipped with liquid flow hole 21-1 and quartz hole 21-2.
See that Fig. 8-1, the liquid flow hole 21-1 of carbon fiber sintering tube 21 there are 6 and be evenly distributed on the bottom of carbon fiber sintering tube 21
Right above portion at 30mm, the diameter of liquid flow hole 21-1 is 36mm.Quartzy hole 21-2 is uniformly arranged, and the plan of establishment is: in carbon fiber
It ties up and the quartzy hole 21-2 in one aperture 10mm is set every 30mm on the sustained height of the barrel of sintering tube 21, to form one group
Quartzy hole 21-2, and one group of quartz hole 21-2 is respectively set every 30mm at various height.Also, in setting liquid flow hole 21-1
Position at no longer be arranged quartz hole 21-2.
The preparation method of above-mentioned carbon fiber sintering tube 21 has following steps:
1. preparing carbon fiber sintering tube semi-finished product: the fabric being woven by carbon fiber is closely wound into 4 to 5 millimeters thicks around model
Cylindrical shape up and down, after cylindrical object is removed from the mold, using 2800 DEG C of high temperature be full of nitrogen shape
Cylindric sinter made of being sintered under state or vacuum state up and down；After natural cooling to get arrive carbon fiber sintering tube
Semi-finished product.
2. after punching and modify by mechanical means on cylindric carbon fiber sintering tube semi-finished product again, and being had
The carbon fiber sintering tube 21 of liquid flow hole 21-1 and quartz hole 21-2.The outer diameter of carbon fiber sintering tube 21 is 740mm, and internal diameter is
730mm is highly 260mm.
Above-mentioned carbon fiber sintering tube semi-finished product can also obtain as follows: according to Chinese patent literature
CN102660768A(the step of application No. is the preparation processes of carbon/carbon composite material crucible disclosed in 201210166266.4)
(1) quasi- three-dimensional crucible preform (see specification [0022] section), that is, carbon fiber sintering tube semi-finished product are obtained.This is prefabricated
The preparation method of carbon fiber sintering tube semi-finished product is: the first, " using the polyacrylonitrile-based carbon fibre of T-700 as raw material, compiling respectively
It is made into net tire and charcoal cloth, and is allowed to be combined into felt by needle thorn, felt is fastened on the mold of crucible shape, is covered thereon
One layer of charcoal cloth, then cover one layer of net tire, be so folded placement and be allowed to compound by needle thorn, obtaining density is 0.45 g/cm3's
Quasi- three-dimensional crucible preform ".The second, it is sintered under the state or vacuum state for being full of nitrogen using 2800 DEG C of high temperature.Third,
Natural cooling.
See Fig. 4 and Fig. 7-1, the quartzy agglomerated material around the setting of carbon fiber sintering tube of crucible inner cylinder 2 includes quartz
Quartz 25 namely the quartzy internal layer 22, quartzy outer layer 23, quartzy bottom in internal layer 22, quartzy outer layer 23, quartzy bottom 24 and hole
Quartz 25 is integral piece made of being sintered as quartz sand in portion 24 and hole.
In the crucible inner cylinder 2, quartzy internal layer 22, carbon fiber sintering tube 21 and quartzy outer layer 23 are according to from inside to outside
Order set gradually, the outer surface of quartzy internal layer 22 connects with the inner surface of carbon fiber sintering tube 21, quartzy outer layer 23 it is interior
Surface connects with the outer surface of carbon fiber sintering tube 21；Quartzy bottom is located at quartzy internal layer 22, carbon fiber sintering tube 21 and quartz
The lower section of outer layer 23, and the upper surface of quartzy bottom is same with the lower surface of the lower surface of quartzy internal layer 22, quartzy outer layer 23 respectively
Matter connects and (refers to that identical material is connected as one), while also connecting with the lower surface of carbon fiber sintering tube 21.Quartz 25 in hole
Refer to the quartz riddled in each quartz hole 21-2 and the quartz being covered on the hole wall of each liquid flow hole (21-1), wherein
Fill and be full of quartz 25 in the hole in each quartz hole 21-2 of carbon fiber sintering tube 21.In hole everywhere quartz 25 respectively with
Quartzy internal layer 22, carbon fiber sintering tube 21 and quartzy outer layer 23 connect, and in hole everywhere quartz 25 and quartzy internal layer 22 and
Connecting for quartzy outer layer 23 is that homogeneity connects.
Still see Fig. 4 and Fig. 7-1, the carbon fiber sintering tube 21 of crucible inner cylinder 2 is the middle layer of crucible inner cylinder 2.Quartz
The internal diameter of internal layer 22 is the internal diameter of crucible inner cylinder 2, and the outer diameter of quartzy internal layer 22 is the internal diameter of carbon fiber sintering tube 21.Stone
The internal diameter of English outer layer 23 is the outer diameter of carbon fiber sintering tube 21, and the outer diameter of quartzy outer layer 23 is the outer diameter of crucible inner cylinder 2.
The internal diameter of quartzy bottom 24 is also the internal diameter of crucible inner cylinder 2, and the outer diameter of quartzy bottom 24 is the outer of crucible inner cylinder 2
Diameter.The thickness (referring to radical length) of carbon fiber sintering tube 21, quartzy internal layer 22 and 23 three of quartzy outer layer is identical, is 5mm；Stone
The thickness of English bottom 24 is also 5mm.
See Fig. 5 and Fig. 6,6 material through holes 26 of crucible inner cylinder 2 are that the diameter surrounded by quartzy agglomerated material is
The round through hole of 30mm, material through hole 26 are Chong Die with the central axis of liquid flow hole 21-1.
See that Fig. 9 to Figure 12, the outer crucible body 1 of crucible are the sintering integrated part of quartz.The outer cylindrical portion 11 of the outer crucible body 1 of crucible be top and
The straight cylinder of bottom perforation, the spherical shape of the inner and outer surfaces of crucible bottom 12, and the position of the centre of sphere is respectively positioned in outer cylindrical portion 11
Same position on central axis.Outer diameter of the full-size of the surrounding of crucible bottom 12 no more than outer cylindrical portion 11.Crucible bottom 12
Thickness, the thickness of outer cylindrical portion 11 it is identical, and be 15mm.The bottom surface of outer cylindrical portion 11 and the top surface of crucible bottom 12 are complete
Connect entirely.Supporting part 13 is located at the inner surface of crucible bottom 12.The shape of the cyclic annular engaging portion 13-1 of supporting part 13 is that level is set
The annular plane set, the side wall 13-2 of supporting part 13 are cylindrical.Inner side edge edge and the crucible bottom of cyclic annular engaging portion 13-1
Connect in the middle part of 12 side wall, the top edge of side wall 13-2 connects with the top of the inner sidewall of crucible bottom 12.The outer crucible body 1 of crucible
It is by quartz sand powder through the sintering integrated homogeneity integral piece formed and outer cylindrical portion therein 11 and crucible bottom 12 link together
(referring to that identical material is connected as one).
Fig. 3, Figure 11 and Figure 12 are seen, outside crucible in the outer diameter and crucible of the cyclic annular engaging portion 13-1 of the supporting part 13 of crucible body 1
The outer diameter of cylinder 2 is identical, and the internal diameter of cyclic annular engaging portion 13-1 is identical as the internal diameter of crucible inner cylinder 2.In use, by the crucible
Inner cylinder 2 is placed on the supporting part 13 of the outer crucible body 1 of crucible, and the bottom of crucible inner cylinder 2 and supporting part 13 is mutual closed sets
It sets；And the inner sidewall spacing distance of the lateral wall of the crucible inner cylinder 2 and outer cylindrical portion 11, so that crucible body 1 outside crucible be divided
At two regions inside and outside crystal growth area and the smelting material area that feeds intake.
Prepare the method for monocrystalline silicon growing combined type silica crucible the following steps are included:
1. the preparation of the outer crucible body 1 of crucible: the first step rotates prefabricated punching block with 70 revs/min of speed, is subsequently poured into
The silica flour (also have and claim quartz sand) that the purity of 500 mesh screens is 99.999% is crossed, uses scraper plate quartz in punching block rotation process
Powder equably scrapes on mould inner wall.Due to mold rotation, silica flour can be attached on mould inner wall due to the effect of centrifugal force
Form quartzy bisque.
Second step, the shape for controlling quartzy bisque with scraper plate are identical with the shape of crucible body 1 outside default crucible.When punching block inner wall
When the quartzy powder layer thickness of attachment reaches 15mm green body is shaped substantially, to obtain outer pan body blank.
Either, the shape for controlling quartzy bisque with scraper plate is identical with the shape of crucible body 1 outside default crucible for second step.Work as steel
The quartzy powder layer thickness of mould inner wall attachment shapes green body substantially when reaching 15mm, then with scraper plate green body pot bottom
The top sides of inner sidewall scrape supporting part 13 along lower section.
Third step, will with outer crucible chaeta base punching block be pushed into high temperature furnace, with the external crucible chaeta base of electric arc heating mode into
Row heat-agglomerating, sintering temperature are 1750 DEG C.Post-tensioning is sintered to go out punching block and stop operating, outer pan body blank at this time at
For crucible outer pan body 1.After naturally cool to crucible body 1 outside the crucible sintered in taking-up punching block after room temperature, so far outside silica crucible
Crucible body 1 completes.
2. the preparation of carbon fiber sintering tube 21: after being woven into cylindraceous fabric by carbon fiber, then it is sintered under vacuum conditions,
Sintering temperature is 2800 DEG C, by mechanical punching and finishing on the cylindraceous fabric after natural cooling, then after sintering, and is obtained
To the carbon fiber sintering tube 21 with liquid flow hole 21-1 He quartz hole 21-2.
3. the preparation of crucible inner cylinder 2: the first step makes the prefabricated punching block for being used to prepare crucible inner cylinder with 70 revs/min
The speed of clock is rotated, and the silica flour (also have and claim quartz sand) that the purity of 500 mesh screens is 99.999% was subsequently poured into.
Punching block rotates so that silica flour is attached on the inner wall of mold by centrifugal action, again will attachment with scraper plate in the rotation of punching block
The pressure that silica flour on die inside wall carries out uniformity is scraped, to form the silica flour outer layer of 5mm thickness.Again by aforementioned preparation
Good carbon fiber sintering tube 21 with upside down be put into it is prefabricated be used to prepare in the punching block of crucible inner cylinder, even if also carbon fiber
The bottom of sintering tube 21 upward, and is affixed the outer surface of carbon fiber sintering tube 21 and the inner surface of silica flour outer layer.
After placing carbon fiber sintering tube 21, continue the purity that 1500 mesh screens were added into the punching block of rotation as 99.999% stone
Ying Fen, then with scraper plate silica flour is equably scraped on the inner surface and bottom surface of carbon fiber sintering tube 21, and scrape carbon
In the quartzy hole 21-2 and liquid flow hole 21-1 of fiber sintering cylinder 21；Punching block rotates so that silica flour is attached to carbon by centrifugal action
On the inner wall of fiber sintering cylinder 21, while part silica flour passes through the liquid flow hole of carbon fiber sintering tube 21 under the influence of centrifugal force
21-1 and quartz hole 21-2 and the gap being filled between the outer surface of carbon fiber sintering tube 21 and the inner surface of silica flour outer layer.
When the inside and outside and bottom surface of carbon fiber sintering tube 21 adheres to the quartzy bisque of 5mm thickness, and silica flour is sintered full of carbon fiber
Cylinder 21 outer surface and silica flour outer layer inner surface between gap and carbon fiber sintering tube 21 each quartz hole 21-2 and respectively
After liquid flow hole 21-1, then inner cylinder green body is formd in punching block.Then the punching block by the rotation with the inner cylinder green body pushes away
Enter high temperature furnace.
The carbon fiber sintering tube 21 prepared either, is placed in upside down prefabricated is used to make first by the first step
On the inner sidewall of the dome shape bottom of the punching block of standby crucible inner cylinder, even if also the bottom of carbon fiber sintering tube 21 is upward,
And make the outer surface of carbon fiber sintering tube 21 and the inner surface interval 5mm distance of prefabricated punching block.Then make prefabricated punching block with 70
Rev/min speed rotated, then poured into 500 mesh screens purity be 99.999% silica flour.Punching block rotation process
In, silica flour is scraped to the inner sidewall of carbon fiber sintering tube with scraper plate.Punching block rotates the inner sidewall so that carbon fiber sintering tube
On silica flour by centrifugal action pass through quartz hole 21-2 and liquid flow hole 21-1 and the outside for being filled in carbon fiber sintering tube 21
Region between surface and prefabricated punching block inner surface.To silica flour fill the outer surface of full carbon fiber sintering tube 21 with it is prefabricated
After each quartz hole 21-2 and liquid flow hole 21-1 in region and carbon fiber sintering tube 21 between punching block inner surface, then pour into
The purity for crossing 1500 mesh screens is 99.999% silica flour, and is scraped silica flour to the inner sidewall of carbon fiber sintering tube with scraper plate
In bottom surface, after the inner sidewall of carbon fiber sintering tube and the quartzy bisque of bottom surface attachment 5mm thickness, then in pre-manufactured steel
Inner cylinder green body is formd in mould.Then the punching block of the rotation with the inner cylinder green body is pushed into high temperature furnace.
Second step carries out heat-agglomerating to the silica flour for forming inner cylinder green body with electric arc heating mode, and sintering temperature is
1750℃.It sinters post-tensioning to go out punching block and stop operating, composite body is obtained after naturally cooling to room temperature.
Third step is taken out the composite body prepared and is cut in height to the bottom of composite body, cutting
Size and position are corresponding with the size of carbon fiber sintering tube 21, and the quartzy bottom 24 of 5mm thickness is left after cutting, and multiple
It closes green body bottom surface and top surface is annular plane.
4th step, in each portion of the setting liquid flow hole 21-1 apart from 21 bottom 30mm of carbon fiber sintering tube of composite body
Position, got with spark has the through-hole that coaxial line and aperture are 30mm to get to 6 equally distributed holes with liquid flow hole 21-1
Diameter is the material through hole 26 of the perforation of 30mm, and crucible inner cylinder 2 is so far made.
4. 3. crucible inner cylinder 2 that step obtains is placed in outside 1. crucible that step obtains in crucible body 1, and it will be close to material
The bottom of the crucible inner cylinder 2 of through hole 26 is placed on the cyclic annular engaging portion 13-1 of supporting part 13, and the two is on upper and lower contact surface
Mutual contact is formed in closed mode, to form monocrystalline silicon growing combined type silica crucible.Wherein, crucible inner cylinder
Area defined is the crystal of combined type silica crucible between the inner cavity of body 2 and the inner wall of the crucible bottom 12 of the outer crucible body 1 of crucible
Vitellarium, and the outer cylindrical portion of the inner wall of the crucible bottom 12 of the outer crucible body 1 of the outer wall of crucible inner cylinder 2, crucible and the outer crucible body 1 of crucible
Area defined is the smelting material area that feeds intake of combined type silica crucible between 11 inner wall.
(Production Example)
When the combined type silica crucible obtained by embodiment 1 prepares monocrystalline silicon, first combined type silica crucible is placed in single crystal growing furnace,
Original from manually putting into from 150 to 180 kilograms of solid silicons (purity 99.9999%) to the smelting material area that feeds intake of combined type silica crucible
Material.Then according to the conventional vacuum pumping method of single crystal growing furnace, to carrying out vacuumize process in the burner hearth of single crystal growing furnace, and it is filled with nitrogen.
Then the temperature of the smelting material area that feeds intake of heating single crystal growing furnace and control combination formula silica crucible is 1500 DEG C.Again by automatic charging device
By setting speed to smelting material area continuous dosing, the melt liquid level to crystal growth zone reaches setting height time control combinations body vitellarium
The temperature in domain is 1420 DEG C, and will be inserted into bath surface by mounted seed crystal in advance, while rotating seed crystal, then invert Combined stone
English crucible is sequentially completed seeding, shouldering, turns shoulder, isometrical and ending process, that is, is drawn into monocrystal rod (monocrystalline obtained by this Production Example
Stick diameter is 210mm, length 4m).Seed crystal is replaced after the completion of ending process and is repeated seeding, shouldering, is turned shoulder, isometrical and ending
Process draws another monocrystal rod.Automatic charging speed is suitable with pulling rate during crystal pulling, melt liquid level and liquid level
Held stationary, the lateral wall and crucible of crucible inner cylinder 2 of the impurity autodeposition below material through hole 26 in silicon raw material
In region between the inner sidewall of outer pan body 1.
The unexpected monocrystalline silicon institute's power consumption for having the technical effect that (1) draws 1 kilogram of this Production Example is 15 degree, and
For the monocrystalline silicon institute power consumption for using conventional method to draw 1 kilogram then for 35 degree, the economize on electricity of this Production Example is up to 57.1%, namely is consumed
Electricity is the 42.8% of conventional method.(2) since drawn monocrystalline silicon can be carried out continuously, so that every single crystal growing furnace (also referred to as monocrystalline
Silicon furnace) production capacity be greatly improved, from originally monthly draw 1.5 to 1.8 tons of monocrystalline silicon be increased to and can monthly draw
Make 4 to 4.5 tons of monocrystalline silicon.(3) due to reducing the number of more exchange device and using automatic charging device, the monocrystalline of every 3 people
Silicon monthly output can achieve 32 tons, and than original 10 tons of monthly output, efficiency improves 300%.(4) cost of equipment is greatly reduced,
Equipment investment only has original 1/7 to 1/10.
(embodiment 2)
See Figure 13 to Figure 15, the rest part of the present embodiment is same as Example 1, the difference is that:
The supporting part 13 of the outer crucible body 1 of crucible has ring-type engaging portion 13-1 and is located at below ring-type engaging portion 13-1 and ties with ring-type
Side wall 13-2 of the conjunction portion 13-1 inner side edge along vertical connection.
The shape of the cyclic annular engaging portion 13-1 of the supporting part 13 of the outer crucible body 1 of crucible is horizontally disposed annular plane,
Outer side edges with the inner sidewall on the top of crucible bottom 12 along connecting, and the side wall 13-2 of supporting part 13 is cylindrical, and side wall 13-2
Lower section edge connect with the lower part of the inner sidewall of crucible bottom 12.
(embodiment 3)
See Figure 16 to Figure 18, the rest part of the present embodiment is same as Example 1, the difference is that: the crucible of crucible outer pan body 1
The thickness on the top of bottom 12 and the thickness of outer barrel are identical as in embodiment 1, but being located at for pot bottom 12 carries
The thickness of the part of 13 top of portion is greater than the thickness of the part for being located at 13 lower section of supporting part of crucible bottom 12, the shape of supporting part 13
It is horizontally disposed annular plane, and the outer side edges of supporting part 13 are carried along connecting with the top of the inner sidewall of crucible bottom 12
The inner side edge edge in portion 13 connects with the lower part of the inner sidewall of crucible bottom 12.The crucible for being located at 13 top of supporting part of the outer crucible body 1 of crucible
The spherical radius of the inner sidewall of bottom 12 is 838mm, positioned at the spherical radius of the inner sidewall of the crucible bottom 12 of 13 lower section of supporting part
For 833mm.
(embodiment 4)
See Figure 19 to Figure 20, the rest part of the present embodiment is same as Example 1, the difference is that: crucible outer pan body 1 is by crucible
Bottom 12 and outer cylindrical portion 11 are constituted, and are not provided with supporting part 13.In use, the bottom of crucible inner cylinder 2 is placed in 12 inside of crucible bottom
On wall, and the central axis of crucible inner cylinder 2 and the central axis of crucible outer pan body 1 are coincided, crucible inner cylinder at this time
The lateral wall of body 2 and the inner sidewall spacing distance of outer cylindrical portion 11.In material, the bottom of crucible inner cylinder 2 can with outside crucible
The interior side-wall surface close contact of the crucible bottom 12 of crucible body 1；This is because crucible inner cylinder will be subjected to 1400 DEG C or so of high temperature,
At this temperature, quartzy softened, the institute of the pot bottom 12 of the outer crucible body 1 of quartz and crucible of the bottom of crucible inner cylinder 2
Close contact between the two to have also been formed at this time even if between the two or having gap.
Above embodiments are used for illustrative purposes only, rather than limitation of the present invention, the technology people in relation to technical field
Member without departing from the spirit and scope of the present invention, can also make various transformation and variation, during concrete application
It can also be transformed accordingly according to the inspiration of above-described embodiment, therefore all equivalent technical solutions should be included into this hair
Within bright scope of patent protection.
Claims (10)
1. a kind of monocrystalline silicon growing combined type silica crucible, crucible body (1) outside the crucible including opening upwards；The outer crucible body of crucible
It (1) is the sintering integrated part of quartz；It is characterized by also including crucible inner cylinder (2)；The outer crucible body (1) of the crucible includes outer cylinder
Portion (11) and crucible bottom (12)；The bottom of the outer cylindrical portion (11) and the top of crucible bottom (12) are connected with each other；
The crucible inner cylinder (2) is cylinder up and down, by carbon fiber sintering tube (21) and surrounds carbon fiber sintering tube
(21) the quartzy agglomerated material being arranged is constituted；The carbon fiber sintering tube (21) is upper and lower made of being woven and be sintered as carbon fiber
The tubular sinter of perforation；The side wall of carbon fiber sintering tube (21) is equipped at least two liquid flow hole (21-1) and multiple in dispersion
The quartzy hole (21-2) of shape distribution；The quartzy agglomerated material is to be covered on being passed through on carbon fiber sintering tube (21) by silica flour
The quartzy integral piece being linked together made of sintering, the quartz integral piece be not placed only in crucible inner cylinder (2) interior outside and
On the surface of downside, it is further filled in each quartzy hole (21-2), but also be covered on the hole wall of each liquid flow hole (21-1)；
The quartz that covers on the hole wall of each liquid flow hole (21-1) of its carbon fiber sintering tube (21) of the crucible inner cylinder (2) is burnt
The position for tying material, forms the material through hole (26) through its side wall of crucible inner cylinder (2), and the material passes through
Hole (26) quantity is identical as the quantity of liquid flow hole (21-1)；
In use, the crucible inner cylinder (2) is placed on the inner sidewall of the crucible bottom (12) of the outer crucible body (1) of crucible, and described
The lateral wall of crucible inner cylinder (2) and the inner sidewall spacing distance of outer cylindrical portion (11), so that crucible body (1) outside crucible is divided into crystal
Vitellarium and the smelting material area region Liang Ge that feeds intake.
2. monocrystalline silicon growing according to claim 1 combined type silica crucible, it is characterised in that: the crucible inner cylinder
(2) carbon fiber sintering tube (21) is cylindric sinter；Crucible inner cylinder (2) is cylinder；Carbon fiber sintering tube (21)
The aperture of each liquid flow hole (21-1) is 20 to 60mm, and is located at 15mm to the 40mm eminence of carbon fiber sintering tube (21) bottom；
The material through hole (26) is Chong Die with the central axis of liquid flow hole (21-1)；The quartzy hole (21-2) of carbon fiber sintering tube (21)
It is uniformly arranged, and gets out of the way the liquid flow hole (21-1).
3. monocrystalline silicon growing according to claim 2 combined type silica crucible, it is characterised in that: the carbon fiber is burnt
The aperture for tying the quartzy hole (21-2) of cylinder (21) is 20 ± 10mm, and quartzy being uniformly arranged for hole (21-2) refers to quartzy hole (21-
2) by between the upper and lower every on 40mm ± 10mm and sustained height between left and right every 40mm ± 10mm in the way of be arranged.
4. monocrystalline silicon growing according to claim 1 combined type silica crucible, it is characterised in that: the crucible inner cylinder
(2) quartzy integral piece is divided into quartzy internal layer (22), quartzy outer layer (23), quartzy bottom (24) according to the difference of location
With (25) quartzy in hole；In the hole quartzy (25) refer to the quartz riddled in each quartzy hole (21-2) and
The quartz being covered on the hole wall of each liquid flow hole (21-1).
5. monocrystalline silicon growing according to claim 4 combined type silica crucible, it is characterised in that: the quartz internal layer
(22) outer diameter is the internal diameter of carbon fiber sintering tube (21), and the internal diameter of quartzy internal layer (22) is the interior of crucible inner cylinder (2)
Diameter；The internal diameter of the quartz outer layer (23) is the outer diameter of carbon fiber sintering tube (21), and the outer diameter of quartzy outer layer (23) is earthenware
The outer diameter of crucible inner cylinder (2)；The internal diameter of quartzy bottom (24) is the internal diameter of crucible inner cylinder (2), quartzy bottom (24) it is outer
Diameter is the outer diameter of crucible inner cylinder (2)；The carbon fiber sintering tube (21), quartzy internal layer (22) and quartzy outer layer (23) three
Thickness it is identical；The outer surface of the quartz internal layer (22) connects with the inner surface of carbon fiber sintering tube (21)；Quartzy outer layer
(23) inner surface connects with the outer surface of carbon fiber sintering tube (21)；The upper surface of quartzy bottom (24) respectively with quartzy internal layer
(22) the lower surface homogeneity of lower surface, quartzy outer layer (23) connects, and connects with the lower surface of carbon fiber sintering tube (21)；Hole
The inner and outer ends relative to side wall of middle quartz (25) respectively with the outer surface of quartzy internal layer (22) and quartz outer layer (23)
Inner surface homogeneity connects.
6. monocrystalline silicon growing according to claim 5 combined type silica crucible, it is characterised in that: the outer crucible body (1) of crucible
Crucible bottom (12) further include the supporting part (13) being arranged on inner sidewall, the supporting part (13) is located at the top of crucible bottom (12)
On inner sidewall below portion edge, so that the part of the inner sidewall of crucible bottom (12) being located above supporting part (13) is crucible bottom
The part being located at below supporting part (13) on the top of the inner sidewall in portion (12), the inner sidewall of crucible bottom (12) is crucible bottom
(12) lower part of inner sidewall, that is to say, the inner sidewall of crucible bottom (12) is divided into inner sidewall according to order from top to bottom
Top, supporting part and inner sidewall lower part；
In use, the bottom surface of crucible inner cylinder (2) can be with supporting part (13) close contact of crucible body (1) outside crucible.
7. the combined type silica crucible of the monocrystalline silicon growing according to any one of claim 2 to 6, it is characterised in that: institute
The outer cylindrical portion (11) for stating the outer crucible body (1) of crucible is cylindrical shape, the spherical shape of inner and outer surfaces of the crucible bottom (12), and ball
The position of the heart is arranged at the same position on the central axis of outer cylindrical portion (11)；The full-size of the surrounding of crucible bottom (12) is equal
No more than the outer diameter of outer cylindrical portion (11).
8. monocrystalline silicon growing according to claim 7 combined type silica crucible, it is characterised in that: the outer crucible body of the crucible
(1) be 99.999% by purity quartz sand powder through sintering integrated molding, and outer cylindrical portion therein (11) and crucible bottom
(12) the homogeneity integral piece being connected together；Outer cylindrical portion (11) with a thickness of 15mm to 60mm, crucible bottom (12) with a thickness of
15mm to 60mm, the thickness of outer cylindrical portion (11) are not more than the thickness of crucible bottom (12).
9. the method for preparing the monocrystalline silicon growing combined type silica crucible as described in one of claim 1 to 8, including following step
It is rapid:
1. the preparation of the outer crucible body (1) of crucible: the first step rotates prefabricated punching block with 60 to 80 revs/min of speed, so
Silica flour is poured into punching block afterwards, silica flour is equably scraped mould inner wall with scraper plate in punching block rotation process；Due to mold
Rotation, silica flour, which can be attached to due to the effect of centrifugal force on mould inner wall, forms quartzy bisque；
Second step, the structure for controlling quartzy bisque with scraper plate are identical with the structure of crucible body (1) outside preset crucible；When punching block inner wall
When the thickness of the quartzy bisque of attachment reaches 15mm to 60mm green body is shaped substantially, to obtain outer pan body blank；
Either, the shape for controlling quartzy bisque with scraper plate is identical with the shape of crucible body (1) outside default crucible for second step；Work as punching block
When the quartzy powder layer thickness of inner wall attachment reaches 15mm to 60mm green body is shaped substantially, then with scraper plate in the bottom of a pan of green body
The top sides of the inner sidewall in portion scrape supporting part (13) along lower section；
Punching block with outer pan body blank is pushed into high temperature furnace, is added with the external crucible chaeta base of electric arc heating mode by third step
Thermal sintering, sintering temperature are not less than 1750 DEG C；Post-tensioning is sintered to go out punching block and stop operating, outer pan body blank at this time at
For crucible outer pan body (1)；It is cooled to after room temperature to take out and sinters the outer crucible body (1) of crucible in punching block, so far the outer crucible body (1) of crucible
It completes；
2. the preparation of carbon fiber sintering tube (21): after being woven into cylindraceous fabric by carbon fiber, then being sintered, burn under vacuum conditions
Junction temperature is not less than 2800 DEG C, passes through mechanical punching and finishing on the cylindraceous fabric after natural cooling, then after sintering, and
Obtain the carbon fiber sintering tube (21) with liquid flow hole (21-1) and quartzy hole (21-2)；
3. the preparation of crucible inner cylinder (2): the first step makes the prefabricated punching block for being used to prepare crucible inner cylinder (2) with 60 to 80
Rev/min speed rotated, be subsequently poured into silica flour；Punching block rotates so that silica flour is attached to mold by centrifugal action
Inner wall on, the pressure that the silica flour being attached on die inside wall carries out uniformity is scraped with scraper plate again in the rotation of punching block,
To form the silica flour outer layer of 5mm to 30mm thickness；Prefabricated carbon fiber sintering tube (21) is put into upside down prefabricated
Be used to prepare in the punching block of crucible inner cylinder, even if also the bottom of carbon fiber sintering tube (21) is upward, and make carbon fiber
The outer surface of sintering tube (21) and the inner surface of silica flour outer layer are affixed；After placing carbon fiber sintering tube (21), continue to turn
Silica flour is added in dynamic punching block, then silica flour is equably scraped with scraper plate inner surface and the bottom of carbon fiber sintering tube (21)
On surface, and scrape in the quartzy hole (21-2) and liquid flow hole (21-1) of carbon fiber sintering tube (21)；Punching block rotates so that stone
English powder is attached on the inner wall of carbon fiber sintering tube (21) by centrifugal action, while part silica flour is under the influence of centrifugal force
Across the liquid flow hole (21-1) of carbon fiber sintering tube (21) and quartzy hole (21-2) and it is filled in the outer of carbon fiber sintering tube (21)
Gap between surface and the inner surface of silica flour outer layer；When the inside and outside and bottom surface of carbon fiber sintering tube (21) is adhered to
The quartzy bisque of 5mm to 30mm thickness, and the interior table of outer surface and silica flour outer layer of the silica flour full of carbon fiber sintering tube (21)
After each quartzy hole (21-2) in gap and carbon fiber sintering tube (21) between face and liquid flow hole (21-1), then the shape in punching block
At inner cylinder green body；Then the punching block of the rotation with the inner cylinder green body is pushed into high temperature furnace；
The carbon fiber sintering tube (21) prepared either, is placed in prefabricated be used to prepare first with upside down by the first step
On the inner sidewall of the dome shape bottom of the punching block of crucible inner cylinder, even if also the bottom of carbon fiber sintering tube is upward, and make
The inner surface interval 5mm of the outer surface of carbon fiber sintering tube (21) and prefabricated punching block is to 30mm distance；Then make prefabricated punching block
It is rotated with 60 to 80 revs/min of speed, then pours into silica flour；In punching block rotation process, with scraper plate by silica flour scrape to
On the inner sidewall of carbon fiber sintering tube；Punching block rotates so that the silica flour on the inner sidewall of carbon fiber sintering tube passes through centrifugal action
Across quartzy hole (21-2) and liquid flow hole (21-1) and it is filled in the outer surface and prefabricated punching block of carbon fiber sintering tube (21)
Region between side surface；To silica flour fill full carbon fiber sintering tube (21) outer surface and prefabricated punching block inner surface it
Between region and carbon fiber sintering tube (21) each quartzy hole (21-2) and liquid flow hole (21-1) after, pour into silica flour again,
And silica flour is scraped to the inner sidewall and bottom surface of carbon fiber sintering tube with scraper plate, the inside to carbon fiber sintering tube (21)
After wall and the quartzy bisque of bottom surface attachment 5mm to 30mm thickness, then inner cylinder green body is formd in prefabricated punching block；Then will
The punching block of rotation with the inner cylinder green body is pushed into high temperature furnace；
Second step carries out heat-agglomerating to the silica flour for forming inner cylinder green body with electric arc heating mode, and sintering temperature is not low
In 1750 DEG C；Post-tensioning is sintered to go out punching block and stop operating, it is to be cooled to obtaining composite body after room temperature；
Third step is taken out the composite body prepared and is cut in height to the bottom of composite body, the size of cutting
It is corresponding with the size of carbon fiber sintering tube (21) with position, and 2 to 5mm thick quartzy bottoms are left after cutting, and compound
Green body bottom surface and top surface are annular plane；
4th step is beaten at each position of the setting liquid flow hole (21-1) apart from carbon fiber sintering tube (21) bottom of composite body
Out there is coaxial line with liquid flow hole (21-1) and aperture is 80% to the 90% material through hole (26) in the aperture liquid flow hole (21-1)
Crucible inner cylinder (2) are so far made in hole.
10. the monocrystalline silicon growing according to claim 9 preparation method of combined type silica crucible, it is characterised in that: also
Include the following steps:
4. the crucible outer barrel (2) prepared is placed in the outer crucible body (1) of crucible, and it will be close to the crucible of material through hole (26)
The bottom of inner cylinder (2) is placed on the inner sidewall of the crucible bottom (12) of crucible outer pan body (1) or is placed on crucible bottom (12)
Top sides are finally made monocrystalline silicon growing combined type silica crucible on the supporting part (13) on the inner sidewall of lower section.
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