CN106757336A - It is a kind of laterally to improve the apparatus and method that polysilicon directional freezing purifies yield - Google Patents
It is a kind of laterally to improve the apparatus and method that polysilicon directional freezing purifies yield Download PDFInfo
- Publication number
- CN106757336A CN106757336A CN201611184955.2A CN201611184955A CN106757336A CN 106757336 A CN106757336 A CN 106757336A CN 201611184955 A CN201611184955 A CN 201611184955A CN 106757336 A CN106757336 A CN 106757336A
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- ring
- graphite crucible
- shaped graphite
- water
- annular
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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 apparatus and method that polysilicon directional freezing purifies yield are laterally improved the invention discloses a kind of, the equipment includes water-cooled column, the side-wall outer side of the water-cooled column is provided with ring-shaped graphite crucible, the axis of the water-cooled column and the ring-shaped graphite crucible is located along the same line, the side-wall outer side of the ring-shaped graphite crucible is provided with annular heater, the side-wall outer side of the annular heater is provided with annular-heating body, the bottom of the ring-shaped graphite crucible is provided with rotary-tray, and circulatory flow is provided with the water-cooled column.The present invention uses lateral solidification mode, and material centrifugal force ensures the reduction of solid liquid interface thickness of diffusion layer, increases its fractional condensation effect.
Description
Technical field
The apparatus and method that polysilicon directional freezing purifies yield are laterally improved the present invention relates to a kind of.
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 two orders of magnitude of reduction more than, by the Partial Resection of final set and then reach purification in industrial production
Purpose.
But traditional directional solidification technique is solidified to top from bottom, 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 provide a kind of equipment for laterally improving polysilicon directional freezing purification yield
And method.The technological means that the present invention is used is as follows：
It is a kind of laterally to improve the equipment that polysilicon directional freezing purifies yield, including water-cooled column, the side wall of the water-cooled column
Outside is provided with ring-shaped graphite crucible, and the axis of the water-cooled column and the ring-shaped graphite crucible is located along the same line, the ring
The side-wall outer side of shape graphite crucible is provided with annular heater, and the side-wall outer side of the annular heater is provided with annular-heating body, institute
The bottom for stating ring-shaped graphite crucible is provided with rotary-tray, and circulatory flow is provided with the water-cooled column.The rotary-tray can make institute
Ring-shaped graphite crucible is stated to be rotated by axle of its axis.
The material of the water-cooled column is stainless steel or copper, and the outer wall of the water-cooled column is provided with sheath, and the sheath is graphite
Sheath or carbon felt sheath, the sheath are used to prevent silicon material splashing from damaging the water-cooled column.
The annular heater is ring-shaped graphite heater.
The annular-heating body is toroidal inductor or ring-shaped graphite electrode.
The inwall of the ring-shaped graphite crucible scribbles coating, and the coating is carborundum or silicon nitride layer, the annular stone
The longitudinal section of black crucible facilitates polycrystalline silicon ingot casting to topple over the demoulding after solidifying in isosceles trapezoid shape.
The equipment, method that polysilicon directional freezing purifies yield is laterally improved the invention also discloses a kind of use the said equipment,
It is characterized in that having following steps：
S1, silicon material is placed in the ring-shaped graphite crucible, reaction compartment is evacuated into 0.1-3Pa backlash enters flowing
Argon gas, makes in reaction compartment pressure be 60000-120000Pa, and the annular-heating body is with the programming rate of 10 DEG C/min by institute
State annular heater and be heated to 1550 DEG C, be incubated 0.5-1h, the silicon melt being completely melt；
Cooling water is poured in S2, the circulatory flow, the temperature of the annular heater is uniform near 1450 in 20min
DEG C, after polysilicon starts in the inner side forming core of the ring-shaped graphite crucible, the ring-shaped graphite crucible is with the rotary-tray
Rotated with the speed of 1-300r/min, meanwhile, the annular heater is lowered the temperature with the cooling rate of 1-10 DEG C/h, is made in the ring
The thermograde of stabilization is formed between the inner side and outer side of shape graphite crucible, promotes polysilicon along radial direction with 0.7mm-
The speed of 2mm/min is grown, and the inner side and outer side of the ring-shaped graphite crucible refers to the interior of the ring-shaped graphite crucible
The inner side and outer side of wall；
S4, when 80% silicon melt is frozen into polysilicon, the rotary speed of rotary-tray lifting 10-50% (enters
One step increase centrifugal force improves the fractional condensation of impurity), until silicon melt is completely solidified into polysilicon.
The present invention uses lateral solidification mode, and material centrifugal force ensures that solid liquid interface thickness of diffusion layer drops
It is low, 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.
The present invention can be widely popularized in fields such as polycrystalline silicon purifyings for the foregoing reasons.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is a kind of structure of the equipment for laterally improving polysilicon directional freezing purification yield in embodiments of the invention 1
Schematic diagram.
The top view of annular graphite crucible in Fig. 2 embodiments of the invention 1.
Specific embodiment
Embodiment 1
It is as depicted in figs. 1 and 2, a kind of laterally to improve the equipment that polysilicon directional freezing purifies yield, including water-cooled column 1,
The side-wall outer side of the water-cooled column 1 is provided with the axis position of ring-shaped graphite crucible 2, the water-cooled column 1 and the ring-shaped graphite crucible 2
In on same straight line, the side-wall outer side of the ring-shaped graphite crucible 2 is provided with annular heater 3, the side wall of the annular heater 3
Outside is provided with annular-heating body 4, and the bottom of the ring-shaped graphite crucible 2 is provided with to be provided with rotary-tray 5, the water-cooled column 1 and follows
Circulation road 6.
The material of the water-cooled column 1 is copper, and the outer wall of the water-cooled column 1 is provided with sheath 7, and the sheath 7 is graphite protecting bush.
The annular heater 3 is ring-shaped graphite heater.
The annular-heating body 4 is toroidal inductor.
The inwall of the ring-shaped graphite crucible 2 scribbles coating, and the coating is carborundum or silicon nitride layer, the annular stone
The longitudinal section of black crucible 2 is in isosceles trapezoid shape.
Embodiment 2
A kind of equipment described in use embodiment 1 laterally improves the equipment, method that polysilicon directional freezing purifies yield, has
Following steps：
S1, silicon material is placed in the ring-shaped graphite crucible 2, reaction compartment is evacuated into 0.1-3Pa backlash becomes a mandarin
Dynamic argon gas, makes pressure in reaction compartment be 60000-120000Pa, and the annular-heating body 4 will with the programming rate of 10 DEG C/min
The annular heater 3 is heated to 1550 DEG C, is incubated 0.5-1h, the silicon melt 8 being completely melt；
Cooling water is poured in S2, the circulatory flow 6, the temperature of the annular heater 3 is uniform near in 20min
1450 DEG C, after polysilicon 9 starts in the inner side forming core of the ring-shaped graphite crucible 2, the ring-shaped graphite crucible 2 is with the rotation
The disk 5 that asks is rotated with the speed of 1-300r/min, meanwhile, the annular heater 3 is lowered the temperature with the cooling rate of 1-10 DEG C/h；
S4, when 80% silicon melt 8 is frozen into polysilicon 9, the rotary speed of the rotary-tray 5 lifting 10-50%,
Until silicon melt 8 is completely solidified into polysilicon 9.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (6)
1. it is a kind of laterally to improve the equipment that polysilicon directional freezing purifies yield, it is characterised in that including water-cooled column, the water-cooled
The side-wall outer side of post is provided with ring-shaped graphite crucible, and the axis of the water-cooled column and the ring-shaped graphite crucible is located at same straight line
On, the side-wall outer side of the ring-shaped graphite crucible is provided with annular heater, and the side-wall outer side of the annular heater is provided with annular
Calandria, the bottom of the ring-shaped graphite crucible is provided with rotary-tray, and circulatory flow is provided with the water-cooled column.
2. equipment according to claim 1, it is characterised in that：The material of the water-cooled column is stainless steel or copper, the water
The outer wall of cold post is provided with sheath, and the sheath is graphite protecting bush or carbon felt sheath.
3. equipment according to claim 1, it is characterised in that：The annular heater is ring-shaped graphite heater.
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 claims, it is characterised in that：The inwall of the ring-shaped graphite crucible
Coating is scribbled, the coating is carborundum or silicon nitride layer, and the longitudinal section of the ring-shaped graphite crucible is in isosceles trapezoid shape.
6. the equipment described in a kind of usage right requirement 5 laterally improves the equipment, method that polysilicon directional freezing purifies yield, and it is special
Levy is with following steps：
S1, silicon material is placed in the ring-shaped graphite crucible, reaction compartment is evacuated into 0.1-3Pa backlash enters to flow argon
Gas, makes pressure in reaction compartment be 60000-120000Pa, and the annular-heating body will be described with the programming rate of 10 DEG C/min
Annular heater is heated to 1550 DEG C, is incubated 0.5-1h, the silicon melt being completely melt；
Cooling water is poured in S2, the circulatory flow, the temperature of the annular heater is uniform near 1450 DEG C in 20min,
After polysilicon starts in the inner side forming core of the ring-shaped graphite crucible, the ring-shaped graphite crucible is with the rotary-tray with 1-
The speed rotation of 300r/min, meanwhile, the annular heater is lowered the temperature with the cooling rate of 1-10 DEG C/h；
S4, when 80% silicon melt is frozen into polysilicon, the rotary speed of rotary-tray lifting 10-50%, until silicon
Melt is completely solidified into polysilicon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611184955.2A CN106757336A (en) | 2016-12-20 | 2016-12-20 | It is a kind of laterally to improve the apparatus and method that polysilicon directional freezing purifies yield |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611184955.2A CN106757336A (en) | 2016-12-20 | 2016-12-20 | It is a kind of laterally to improve the apparatus and method that polysilicon directional freezing purifies yield |
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| Publication Number | Publication Date |
|---|---|
| CN106757336A true CN106757336A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611184955.2A Pending CN106757336A (en) | 2016-12-20 | 2016-12-20 | It is a kind of laterally to improve the apparatus and method that polysilicon directional freezing purifies yield |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110578169A (en) * | 2019-10-18 | 2019-12-17 | 衡水学院 | Apparatus for purifying silicon |
| CN114086240A (en) * | 2021-11-09 | 2022-02-25 | 北京华卓精科科技股份有限公司 | Annular crucible, and crystal transverse directional growth device and method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351188A (en) * | 2011-07-07 | 2012-02-15 | 陈评 | Method for preparing acicular high-purity silicon aggregates and equipment thereof |
| 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 CN201611184955.2A patent/CN106757336A/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 |
| CN102351188A (en) * | 2011-07-07 | 2012-02-15 | 陈评 | Method for preparing acicular high-purity silicon aggregates and equipment thereof |
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110578169A (en) * | 2019-10-18 | 2019-12-17 | 衡水学院 | Apparatus for purifying silicon |
| CN114086240A (en) * | 2021-11-09 | 2022-02-25 | 北京华卓精科科技股份有限公司 | Annular crucible, and crystal transverse directional growth device and method |
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Application publication date: 20170531 |