CN104131337B - The crucible with exhausting impurity function of application and polycrystalline silicon purifying or casting ingot method in polycrystalline silicon purifying or ingot casting link - Google Patents
The crucible with exhausting impurity function of application and polycrystalline silicon purifying or casting ingot method in polycrystalline silicon purifying or ingot casting link Download PDFInfo
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- CN104131337B CN104131337B CN201410339742.7A CN201410339742A CN104131337B CN 104131337 B CN104131337 B CN 104131337B CN 201410339742 A CN201410339742 A CN 201410339742A CN 104131337 B CN104131337 B CN 104131337B
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- crucible
- crucible body
- liquid
- spout hole
- polycrystalline silicon
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 37
- 239000012535 impurity Substances 0.000 title claims abstract description 25
- 238000005266 casting Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims description 12
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000002210 silicon-based material Substances 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 229920005591 polysilicon Polymers 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000012790 confirmation Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000007689 inspection Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000001223 reverse osmosis Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
In polycrystalline silicon purifying or ingot casting link, the crucible with exhausting impurity function of application, including the crucible body of column, is provided with spout hole on the sidewall of crucible body, and the bottom being positioned at spout hole in the outside of crucible body is provided with collecting tank；The base of the spout hole height H=H away from crucible body inside bottom surfaceLiquid+ (HGu-HLiquid) 20%, wherein HLiquidFor the liquid level in crucible body, H during polysilicon liquidGuHeight after crystallizing in crucible body for polysilicon.Step is as follows: loading polycrystalline silicon material in crucible body, shove charge carries out vacuum and takes out in advance；The entrance first stage heats and is completely melt；Long crystalline substance；Annealing, eliminates crystal internal stress；Cooling, cools to 400 DEG C with the furnace, comes out of the stove；Come out of the stove and be cooled to room temperature；Take out silicon ingot and collect spilling silicon material.By the impurity enriched district of top layer in running, remove under liquid condition, reduce the reverse osmosis of silicon ingot molding rear impurity enrichment region, improve silicon ingot overall utilization rate.
Description
Technical field
The present invention relates to crucible used in a kind of polycrystalline silicon purifying or ingot casting link and utilize this crucible to polycrystalline silicon purifying or the method for ingot casting.
Background technology
The device used during polycrystalline silicon ingot casting at present includes crucible, crucible mostly is rectangular shape, the casing i.e. having four sides and a bottom surface to surround, and is loaded by polycrystalline silicon material in crucible, it is subsequently placed on the graphite base of furnace body inside, in body of heater, is positioned at crucible periphery is provided with program control heater.Polycrystalline silicon material forms liquid after being heated, then crystallization forms ingot casting.Polysilicon top silicon material when liquid is impurity compact district, and silicon ingot can spread to bottom concentration range from top area with high mercury at coagulation forming rear impurity, thus affects utilization rate of silicon ingot.Usual method is after silicon ingot molding, with the cutting equipment of specialty, top height impurity range is excised, have the drawback that 1, after silicon ingot coagulation forming due to impurity diffusion, impurity range increase in time and expand, the height of excision is consequently increased, and utilization rate decreases；2, need the equipment excision impurity high concentration region, top of specialty, increase production run cost；3, also there is the method removing liquid top impurity present stage, but the transformation amount of equipment is very much not easily achieved.
Summary of the invention
It is an object of the invention to provide a kind of simple in construction, the liquid-state silicon material of top impurity close quarters can be discharged during the long crystalline substance of polysilicon, do not produce after ingot casting high density impurity range, without cutting, reduce cost, carry crucible used in high-quality polycrystalline silicon purifying or ingot casting link and utilize this crucible to polycrystalline silicon purifying or the method for ingot casting, overcome the deficiencies in the prior art.
In the polycrystalline silicon purifying of the present invention or ingot casting link, the crucible with exhausting impurity function of application, including the crucible body of column, is provided with spout hole on the sidewall of crucible body, and the bottom being positioned at spout hole in the outside of crucible body is provided with collecting tank；The base of the described spout hole height H=H away from crucible body inside bottom surfaceLiquid+ (HGu-HLiquid) 20%, wherein said HLiquidFor the liquid level in crucible body, H during polysilicon liquidGuHeight after crystallizing in crucible body for polysilicon.
Described crucible body is quadrangular shape, and described spout hole and collecting tank are distributed on each side of crucible body, and spout hole is circular hole.
The present invention utilizes aforesaid crucible to purify polysilicon or the method for ingot casting, and step is as follows:
(1), in crucible body, load polycrystalline silicon material, load the silicon material diameter loaded after silicon material reaches spout hole height and should be greater than overflow orifice diameter；
(2), shove charge carries out vacuum and takes out in advance；
(3), when vacuum values to programmed values, system carries out equipment self-inspection, clicks on and automatically run after no problem
Enter first stage heating；
, the heating period complete after Automatic Program enter the melting stage, after Programmable detection is completely melt to silicon material, alarm, manual confirmation be completely melt after entrance next stage；
, crystal growing stage, Automatic Program is run, until crystal occurs to silicon material top in Programmable detection, alarm, after the long crystalline substance in manual confirmation top, entrance next stage, discharges, from spout hole, the liquid-state silicon that impurity content is high during long crystalline substance in collecting tank；
, annealing stage, eliminate crystal internal stress；
, cooling stage, cool to 400 DEG C with the furnace, open furnace chamber and come out of the stove；
(8), come out of the stove and be cooled to room temperature；
(9), take out silicon ingot and collect spilling silicon material.
The present invention compared with prior art has the following technical effect that
1, the physical characteristic of polycrystalline silicon material itself is utilized, it is not necessary to additive does not has garbage to produce yet；
2, method is easily achieved, and existing orientation equipment need not be carried out large-scale redevelopment, only by crucible
Local is changed, and as processed spout hole and arranging collecting tank, i.e. can reach impurities removal purpose；By the impurity enriched district of top layer during long crystalline substance, removed by spout hole under liquid condition, reduce the reverse osmosis of silicon ingot molding rear impurity enrichment region, improve silicon ingot overall utilization rate；
3, the suitability is strong, it is adaptable to directional freeze method, as purified and ingot casting；
4, need not special technique coordinate, realize the most on a production line；
5, impurities removal silicon material recoverable, circulates melting again, reduces cost.
Accompanying drawing explanation
Fig. 1 is the schematic front view of crucible in the present invention；
Fig. 2 is the schematic perspective view of crucible in the present invention；
Fig. 3 is to load in the present invention in the crucible of polycrystalline silicon material is placed in body of heater to carry out casting fixed structural representation.
Detailed description of the invention
As shown in Figure 1, 2: the crucible with exhausting impurity function of application in polycrystalline silicon purifying of the present invention or ingot casting link, including the crucible body 2 of column, being machined with spout hole 7 on the sidewall of crucible body 2, the bottom being positioned at spout hole 7 in the outside of crucible body 2 is provided with collecting tank 8.The base of the spout hole 7 height H=H away from crucible body 2 inside bottom surfaceLiquid+ (HGu-HLiquid) 20%, wherein HLiquidFor the liquid level in crucible body, H during polysilicon liquidGuHeight after crystallizing in crucible body for polysilicon.
Crucible body 2 is quadrangular shape, and spout hole 7 and collecting tank 8 are distributed on each side of crucible body 2, and spout hole 7 is circular hole.
The present invention utilizes above-mentioned crucible to purify polysilicon or the method for ingot casting, and step is as follows:
(1), in crucible body, load polycrystalline silicon material, load the silicon material diameter loaded after silicon material reaches spout hole height and should be greater than overflow orifice diameter；
(2), shove charge carries out vacuum and takes out in advance, as shown in Figure 3: 3 is body of heater, and the lower inside at body of heater 3 is provided with graphite base 4, and crucible 2 is placed on graphite base 4, and being positioned at around crucible 2 in the inner side of body of heater 3 has the heater 1 connected with stored program controlled.
(3), when vacuum values to programmed values, system carries out equipment self-inspection, clicks on and automatically run after no problem
Enter first stage heating；
, the heating period complete after Automatic Program enter the melting stage, formed liquid-state silicon 5, after Programmable detection is completely melt to silicon material, alarm, manual confirmation be completely melt after entrance next stage；
, crystal growing stage, Automatic Program is run, until Programmable detection crystal occurs to silicon material top, alarm, manual confirmation top length is brilliant, enters next stage, discharge, from spout hole 7, the liquid-state silicon that impurity content is high during long crystalline substance in collecting tank 8 after forming solid-state silicon 6；
, annealing stage, eliminate crystal internal stress；
, cooling stage, cool to 400 DEG C with the furnace, open furnace chamber and come out of the stove；
(8), come out of the stove and be cooled to room temperature；
(9), take out silicon ingot and collect spilling silicon material.
Instantiation:
As shown in Figure 1, 2, 3: as a example by GT DSS450, ingot casting weight 450Kg, crucible size 840mm × 840mm × 420mm；ρLiquid=2.42g/cm3, ρGu=2.33 g/cm3。
Polysilicon liquid level H during liquid in crucibleLiquid=VLiquid/SThe end=M/ρLiquid/ SThe end=263mm
Polysilicon casts fixed height H after crucible intercrystallineGu=VGu/SThe end=M/ρGu/ SThe end=273mm
Floor height H=H inside the base distance crucible 2 of spout hole 7Liquid+ (HGu-HLiquid) 20%, i.e. the position, base of spout hole 7 is away from crucible 2 inside bottom surface 265mm.When silicon material is completely melt, liquid level reaches 263mm, and when bottom starts directional long crystal, liquid level will be gradually increasing, and when reaching bore position 265mm, silicon liquid is flowed in collecting tank 8 by spout hole 7.The height of spout hole 7 can be adjusted by production technology, thus controls to arrange silicon amount, reaches the equilibrium point of economic benefit and production cost.
Claims (3)
1. the crucible with exhausting impurity function of application in a polycrystalline silicon purifying or ingot casting link, crucible body (2) including column, it is characterized in that: be provided with spout hole (7) on the sidewall of crucible body (2), the bottom being positioned at spout hole (7) in the outside of crucible body (2) is provided with collecting tank (8)；The base of described spout hole (7) the height H=H away from crucible body (2) inside bottom surfaceLiquid+ (HGu-HLiquid) 20%, wherein said HLiquidFor the liquid level in crucible body, H during polysilicon liquidGuHeight after crystallizing in crucible body for polysilicon.
The crucible with exhausting impurity function of application in polycrystalline silicon purifying the most according to claim 1 or ingot casting link, it is characterized in that: described crucible body (2) is quadrangular shape, described spout hole (7) and collecting tank (8) are distributed on each side of crucible body (2), and spout hole (7) is circular hole.
3. one kind utilizes crucible as claimed in claim 1 or 2 to purify polysilicon or the method for ingot casting, it is characterised in that: step is as follows:
(1), in crucible body, load polycrystalline silicon material, load the silicon material diameter loaded after silicon material reaches spout hole height and should be greater than overflow orifice diameter；
(2), shove charge carries out vacuum and takes out in advance；
(3), when vacuum values to programmed values, system carries out equipment self-inspection, clicks on and automatically run after no problem
Enter first stage heating；
, the heating period complete after Automatic Program enter the melting stage, after Programmable detection is completely melt to silicon material, alarm, manual confirmation be completely melt after entrance next stage；
, crystal growing stage, Automatic Program is run, until crystal occurs to silicon material top in Programmable detection, alarm, after the long crystalline substance in manual confirmation top, entrance next stage, discharges, from spout hole, the liquid-state silicon that impurity content is high during long crystalline substance in collecting tank；
, annealing stage, eliminate crystal internal stress；
, cooling stage, cool to 400 DEG C with the furnace, open furnace chamber and come out of the stove；
(8), come out of the stove and be cooled to room temperature；
(9), take out silicon ingot and collect spilling silicon material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410339742.7A CN104131337B (en) | 2014-07-17 | 2014-07-17 | The crucible with exhausting impurity function of application and polycrystalline silicon purifying or casting ingot method in polycrystalline silicon purifying or ingot casting link |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410339742.7A CN104131337B (en) | 2014-07-17 | 2014-07-17 | The crucible with exhausting impurity function of application and polycrystalline silicon purifying or casting ingot method in polycrystalline silicon purifying or ingot casting link |
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| Publication Number | Publication Date |
|---|---|
| CN104131337A CN104131337A (en) | 2014-11-05 |
| CN104131337B true CN104131337B (en) | 2016-08-17 |
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| CN201410339742.7A Expired - Fee Related CN104131337B (en) | 2014-07-17 | 2014-07-17 | The crucible with exhausting impurity function of application and polycrystalline silicon purifying or casting ingot method in polycrystalline silicon purifying or ingot casting link |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106048718B (en) * | 2016-08-19 | 2018-10-12 | 西安华晶电子技术股份有限公司 | A kind of polysilicon fritting ingot casting sundries discharging method |
| CN106119959A (en) * | 2016-08-30 | 2016-11-16 | 常熟华融太阳能新型材料有限公司 | A kind of quartz ceramic crucible for polycrystalline silicon ingot casting |
| CN107585770A (en) * | 2016-12-07 | 2018-01-16 | 安徽爱森能源有限公司 | A kind of method of purification of silicon |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206855A (en) * | 2010-03-29 | 2011-10-05 | 上海杰姆斯电子材料有限公司 | Czochralski crystal grower graphite crucible |
| CN202226676U (en) * | 2011-05-16 | 2012-05-23 | 大连隆田科技有限公司 | Device for purifying polycrystalline silicon by directional solidification and slag filter smelting |
| CN202246997U (en) * | 2011-09-19 | 2012-05-30 | 浙江思博恩新材料科技有限公司 | Double-layer crucible |
| CN103668437A (en) * | 2012-08-30 | 2014-03-26 | 上海杰姆斯电子材料有限公司 | Crucible used for preparing monocrystalline silicon by czochralski method |
| CN203653256U (en) * | 2013-11-28 | 2014-06-18 | 青岛天和达石墨有限公司 | Graphite crucible for graphitization furnace |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3475407B2 (en) * | 1997-03-31 | 2003-12-08 | キヤノン株式会社 | Apparatus and method for producing fluoride crystal and crucible |
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- 2014-07-17 CN CN201410339742.7A patent/CN104131337B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206855A (en) * | 2010-03-29 | 2011-10-05 | 上海杰姆斯电子材料有限公司 | Czochralski crystal grower graphite crucible |
| CN202226676U (en) * | 2011-05-16 | 2012-05-23 | 大连隆田科技有限公司 | Device for purifying polycrystalline silicon by directional solidification and slag filter smelting |
| CN202246997U (en) * | 2011-09-19 | 2012-05-30 | 浙江思博恩新材料科技有限公司 | Double-layer crucible |
| CN103668437A (en) * | 2012-08-30 | 2014-03-26 | 上海杰姆斯电子材料有限公司 | Crucible used for preparing monocrystalline silicon by czochralski method |
| CN203653256U (en) * | 2013-11-28 | 2014-06-18 | 青岛天和达石墨有限公司 | Graphite crucible for graphitization furnace |
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| CN104131337A (en) | 2014-11-05 |
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Granted publication date: 20160817 Termination date: 20190717 |