CN106591946A - Device and method for increasing directional solidification and purification yield of polysilicon through reverse centrifuging - Google Patents
Device and method for increasing directional solidification and purification yield of polysilicon through reverse centrifuging Download PDFInfo
- Publication number
- CN106591946A CN106591946A CN201611184522.7A CN201611184522A CN106591946A CN 106591946 A CN106591946 A CN 106591946A CN 201611184522 A CN201611184522 A CN 201611184522A CN 106591946 A CN106591946 A CN 106591946A
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- Prior art keywords
- material container
- silicon material
- water
- heater
- polysilicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a device and method for increasing the directional solidification and purification yield of polysilicon through reverse centrifuging. The device comprises a furnace body and a silicon material container located in the furnace body; the outer side of the side wall of the silicon material container is provided with an annular heat generating body fixedly connected with the furnace body; an annular heating body fixedly connected with the furnace body is arranged on the outer side of the annular heat generating body; a rotating tray is arranged at the lower end of the silicon material container and is fixedly connected with the lower end of the silicon material container through a connecting bolt; the position of the axis of the silicon material container is provided with a water cooling column capable of moving up and down along the axis of the silicon material container; and a circulating flow channel is arranged in the water cooling column. The reverse solidification manner is adopted for the device, under the condition of the gravity effect, impurity diffusion is guaranteed, meanwhile, the centrifugal force guarantees that the thickness of a solid and liquid interface diffusion layer is lowered, and the fractional condensation effect of the device is improved.
Description
Technical field
The present invention relates to a kind of reverse centrifugation improves the apparatus and method that polysilicon directional freezing purifies yield.
Background technology
Directional solidification purification is the major technique for removing metal impurities in polysilicon, is widely used in polycrystalline silicon ingot casting, smelting
In golden method purification process.
What directional solidification purification was utilized is fractional condensation behavior of the impurity at solid liquid interface：In directional solidification process, due to miscellaneous
Different solubility of the prime element in solid phase and liquid phase, can occur redistributing for solute, again in the solid liquid interface of silicon melt
The degree of distribution is determined by segregation coefficient and freezing rate.The segregation coefficient k0 of metal impurities<<1, can be constantly to liquid-state silicon
Middle enrichment, the region impurity content of initial solidification is low, final set region impurity content highest.Directional solidification can make industrial silicon
In metals content impurity reduce more than two orders of magnitude, the Partial Resection of final set and then purification being reached in industrial production
Purpose.
But traditional directional solidification technique is solidified from bottom to top, and the clearance of impurity is relatively low, final set
Easily there is Inversion in extrinsic region, reduce the yield of product.
The content of the invention
According to technical problem set forth above, and a kind of reverse centrifugation is provided and improves polysilicon directional freezing purification yield
Apparatus and method.The technological means that the present invention is adopted is as follows：
A kind of reverse centrifugation improves the equipment that polysilicon directional freezing purifies yield, it is characterised in that including body of heater, be located at
Silicon material container in the body of heater, the side-wall outer side of the silicon material container is provided with the annular heating being fixedly connected with the body of heater
Body, the annular heater outside is provided with the annular-heating body being fixedly connected with the body of heater, and the lower end of the silicon material container sets
There is rotary-tray, the rotary-tray is fixedly connected by coupling bar with the lower end of the silicon material container, the silicon material container
The water-cooled column that can be moved up and down along the axis of the silicon material container is provided with axis, in the water-cooled column circulatory flow is provided with.
The material of the water-cooled column is stainless steel or copper.
The outer surface of the water-cooled column is provided with graphite linings.
The annular-heating body is toroidal inductor or ring-shaped graphite electrode.
The inwall of the silicon material container scribbles coating, and the coating is carborundum or silicon nitride layer, and the silicon material container is
Graphite sleeve, quartz ceramic crucible or graphite crucible.
The invention also discloses a kind of inversely centrifugation using above-mentioned equipment improves polysilicon directional freezing purification yield
Method, it is characterised in that with following steps：
S1, silicon material is placed in the silicon material container, the body of heater is evacuated to 0.1-3Pa backlash and enters the argon gas that flows,
Pressure is set in the body of heater to be 60000-120000Pa, the annular-heating body is with the programming rate of 10 DEG C/min by the annular
Heater is heated to 1550 DEG C, is incubated 0.5-1h, obtains the silicon melt being completely melt；
Pour after cooling water in S2, the circulatory flow, in the silicon melt that will be obtained in water-cooled column inserting step S1；
S3, when polysilicon starts to be solidified along the water-cooled column, institute is lifted with the speed of 0.07mm/min-0.8mm/min
Water-cooled column is stated, meanwhile, the silicon material container is rotated with the rotary-tray with the speed of 1-500r/min；
By the setting rate for controlling the flow control polysilicon of cooling water, because the water-cooled column is along the silicon material container
Axis lifting, it is ensured that polysilicon solidifies from the top of the water-cooled column to bottom, realizes Inversion.
S4, when 80% silicon melt is frozen into polysilicon, the rotary speed of the rotary-tray lifts 10-50%, enters
One step increase centrifugal force improves the fractional condensation of impurity；
S5, when 90% silicon melt is frozen into polysilicon, the water-cooled column is lifted rapidly, it is ensured that enrichment impurity silicon melt
Body is remained in the silicon material container.
The present invention uses Inversion mode, under the conditions of Action of Gravity Field, it is ensured that impurity spreads, while using centrifugal force
Ensure that solid liquid interface thickness of diffusion layer is reduced, increase its fractional condensation effect.
The present invention has advantages below：
1. utilization rate of silicon ingot 5-10% is effectively improved.
2. high-purity region proportion is realized, actual yield 5-15% is improve.
3rd, separation of solid and liquid is realized, prevents magazine from inversely spreading.
4th, the refining effect of polysilicon impurity 2N to 5.5N can be realized.
For the foregoing reasons the present invention can be widely popularized in fields such as polycrystalline silicon purifyings.
Description of the drawings
With reference to the accompanying drawings and detailed description the present invention is further detailed explanation.
Fig. 1 is that a kind of reverse centrifugation improves the equipment that polysilicon directional freezing purifies yield in embodiments of the invention 1
Structural representation.
Specific embodiment
Embodiment 1
As shown in figure 1, a kind of reverse centrifugation improves the equipment that polysilicon directional freezing purifies yield, including body of heater 1, it is located at
Silicon material container 2 in the body of heater 1, the side-wall outer side of the silicon material container 2 is provided with the annular being fixedly connected with the body of heater 1 and sends out
Hot body 3, the outside of the annular heater 3 is provided with the annular-heating body 4 being fixedly connected with the body of heater 1, the silicon material container 2
Lower end is provided with rotary-tray 5, and the rotary-tray 5 is fixedly connected by coupling bar 6 with the lower end of the silicon material container 2, described
It is provided with the axis of silicon material container 2 in the water-cooled column 7 that can be moved up and down along the axis of the silicon material container 2, the water-cooled column 7 and sets
There is circulatory flow 8.
The material of the water-cooled column 7 is copper.
The outer surface of the water-cooled column 7 is provided with graphite linings.
The annular-heating body 4 is toroidal inductor.
The inwall of the silicon material container 2 scribbles coating, and the coating is carborundum or silicon nitride layer, the silicon material container 2
For graphite crucible.
Embodiment 2
A kind of equipment described in use embodiment 1 is inversely centrifuged the method that polysilicon directional freezing purifies yield that improves, tool
Have the following steps：
S1, silicon material is placed in the graphite crucible, the body of heater 1 is evacuated to 0.1-3Pa backlash and enters the argon gas that flows,
Pressure in the body of heater 1 is set to be 60000-120000Pa, the toroidal inductor will be described with the programming rate of 10 DEG C/min
Annular heater 3 is heated to 1550 DEG C, is incubated 0.5-1h, obtains the silicon melt 9 being completely melt；
Pour after cooling water in S2, the circulatory flow 8, the silicon melt 9 that will be obtained in inserting step S1 of the water-cooled column 7
In；
S3, when polysilicon 10 starts to be solidified along the water-cooled column 7, lifted with the speed of 0.07mm/min-0.8mm/min
The water-cooled column 7, meanwhile, the graphite crucible is rotated with the rotary-tray 5 with the speed of 1-500r/min；
S4, when 80% silicon melt 9 is frozen into polysilicon 10, the rotary speed of the rotary-tray 5 lifts 10-
50%；
S5, when 90% silicon melt 9 is frozen into polysilicon 10, the water-cooled column 7 is lifted rapidly.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (6)
1. a kind of reverse centrifugation improves the equipment that polysilicon directional freezing purifies yield, it is characterised in that including body of heater, positioned at institute
The silicon material container in body of heater is stated, the side-wall outer side of the silicon material container is provided with the annular heater being fixedly connected with the body of heater,
The annular heater outside is provided with the annular-heating body being fixedly connected with the body of heater, and the lower end of the silicon material container is provided with rotation
Ask disk, and the rotary-tray is fixedly connected by coupling bar with the lower end of the silicon material container, the axis of the silicon material container
Place is provided with the water-cooled column that can be moved up and down along the axis of the silicon material container, and in the water-cooled column circulatory flow is provided with.
2. equipment according to claim 1, it is characterised in that：The material of the water-cooled column is stainless steel or copper.
3. equipment according to claim 1, it is characterised in that：The outer surface of the water-cooled column is provided with graphite linings.
4. equipment according to claim 1, it is characterised in that：The annular-heating body is toroidal inductor or annular stone
Electrode ink.
5. the equipment according to claim 1-4 any claim, it is characterised in that：The inwall of the silicon material container is scribbled
Coating, the coating is carborundum or silicon nitride layer, and the silicon material container is graphite sleeve, quartz ceramic crucible or graphite earthenware
Crucible.
6. a kind of usage right requires that the equipment described in 5 is inversely centrifuged the method that polysilicon directional freezing purifies yield that improves, its
It is characterized by following steps：
S1, silicon material is placed in the silicon material container, the body of heater is evacuated to 0.1-3Pa backlash and enters the argon gas that flows, and makes institute
It is 60000-120000Pa to state pressure in body of heater, and the annular-heating body is generated heat the annular with the programming rate of 10 DEG C/min
Body is heated to 1550 DEG C, is incubated 0.5-1h, obtains the silicon melt being completely melt；
Pour after cooling water in S2, the circulatory flow, in the silicon melt that will be obtained in water-cooled column inserting step S1；
S3, when polysilicon starts to be solidified along the water-cooled column, the water is lifted with the speed of 0.07mm/min-0.8mm/min
Cold post, meanwhile, the silicon material container is rotated with the rotary-tray with the speed of 1-500r/min；
S4, when 80% silicon melt is frozen into polysilicon, the rotary speed of the rotary-tray lifts 10-50%；
S5, when 90% silicon melt is frozen into polysilicon, the water-cooled column is lifted rapidly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611184522.7A CN106591946A (en) | 2016-12-20 | 2016-12-20 | Device and method for increasing directional solidification and purification yield of polysilicon through reverse centrifuging |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611184522.7A CN106591946A (en) | 2016-12-20 | 2016-12-20 | Device and method for increasing directional solidification and purification yield of polysilicon through reverse centrifuging |
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| Publication Number | Publication Date |
|---|---|
| CN106591946A true CN106591946A (en) | 2017-04-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611184522.7A Pending CN106591946A (en) | 2016-12-20 | 2016-12-20 | Device and method for increasing directional solidification and purification yield of polysilicon through reverse centrifuging |
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| CN (1) | CN106591946A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110565162A (en) * | 2019-09-23 | 2019-12-13 | 大同新成新材料股份有限公司 | Thermal field crucible with heat preservation structure for multi-product silicon and use method thereof |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202529852U (en) * | 2011-12-08 | 2012-11-14 | 王洪举 | Polycrystalline silicon centrifuging purifying furnace |
| CN103553052A (en) * | 2013-10-30 | 2014-02-05 | 大连理工大学 | Polysilicon reverse solidification device and method |
| CN105088330A (en) * | 2005-06-10 | 2015-11-25 | 埃尔凯姆太阳能公司 | Method and apparatus for refining amolten material |
| CN204898124U (en) * | 2015-08-27 | 2015-12-23 | 宁夏金海金晶光电产业有限公司 | Polycrystalline silicon ingot casting is with purification stove |
-
2016
- 2016-12-20 CN CN201611184522.7A patent/CN106591946A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088330A (en) * | 2005-06-10 | 2015-11-25 | 埃尔凯姆太阳能公司 | Method and apparatus for refining amolten material |
| CN202529852U (en) * | 2011-12-08 | 2012-11-14 | 王洪举 | Polycrystalline silicon centrifuging purifying furnace |
| CN103553052A (en) * | 2013-10-30 | 2014-02-05 | 大连理工大学 | Polysilicon reverse solidification device and method |
| CN204898124U (en) * | 2015-08-27 | 2015-12-23 | 宁夏金海金晶光电产业有限公司 | Polycrystalline silicon ingot casting is with purification stove |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110565162A (en) * | 2019-09-23 | 2019-12-13 | 大同新成新材料股份有限公司 | Thermal field crucible with heat preservation structure for multi-product silicon and use method thereof |
| CN110565162B (en) * | 2019-09-23 | 2024-02-27 | 大同新成新材料股份有限公司 | Production equipment with heat preservation structure for polysilicon and application method of production equipment |
| CN113584586A (en) * | 2021-08-06 | 2021-11-02 | 宁夏红日东升新能源材料有限公司 | Method and device for purifying polycrystalline silicon by centrifugal directional solidification |
| CN113584586B (en) * | 2021-08-06 | 2024-04-26 | 宁夏红日东升新能源材料有限公司 | Centrifugal directional solidification purification method and device for polysilicon |
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Application publication date: 20170426 |