CN106587071B - A kind of lateral solidification superposition of electric field improves the device and method of polycrystalline silicon purifying yield - Google Patents
A kind of lateral solidification superposition of electric field improves the device and method of polycrystalline silicon purifying yield Download PDFInfo
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- CN106587071B CN106587071B CN201611258337.8A CN201611258337A CN106587071B CN 106587071 B CN106587071 B CN 106587071B CN 201611258337 A CN201611258337 A CN 201611258337A CN 106587071 B CN106587071 B CN 106587071B
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- graphite
- graphite crucible
- annular
- water
- electric field
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
Abstract
The invention discloses the equipment that a kind of lateral solidification superposition of electric field improves polycrystalline silicon purifying yield, it is characterized in that, including water-cooled column, the side-wall outer side of the water-cooled column is equipped with graphite sleeve, the side-wall outer side of the graphite sleeve is equipped with graphite crucible, the water-cooled column, the axis of the graphite sleeve and the graphite crucible is located along the same line, the side-wall outer side of the graphite crucible is equipped with annular heater, the side-wall outer side of the annular heater is equipped with annular-heating body, the bottom of the graphite crucible is equipped with rotary-tray, circulatory flow is equipped in the water-cooled column, the graphite sleeve and the graphite crucible are connect with power positive cathode respectively.The present invention and reduces solid liquid interface thickness of diffusion layer using the mode of lateral solidification superposition of electric field using centrifugal force and electric field force, increases its and segregates effect.
Description
Technical field
The present invention relates to the device and method that a kind of lateral solidification superposition of electric field improves polycrystalline silicon purifying yield.
Background technology
Directional solidification purification is to remove the major technique of metal impurities in polysilicon, is widely used in polycrystalline silicon ingot casting, smelting
In golden method purification process.
What directional solidification purification 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, solute can redistribute behavior at solid liquid interface, redistribute
Degree codetermined by segregation coefficient and solidification rate.Segregation coefficient k0 of the metal impurities in silicon<<1, it can be constantly to liquid
It is enriched in state silicon, the region impurity content of initial solidification is low, final solidified region impurity content highest.Directional solidification can make work
Metals content impurity in industry silicon reduces by two orders of magnitude or more, and final solidified part is cut off and then reached in industrial production
The purpose of purification.
But traditional directional solidification technique is solidified from bottom to top, the removal rate of impurity is relatively low, final solidified
Inversion easily occurs for extrinsic region, reduces the yield of product.
Invention content
According to technical problem set forth above, and a kind of lateral solidification superposition of electric field is provided and improves polycrystalline silicon purifying yield
Device and method.The technological means that the present invention uses is as follows：
A kind of equipment that lateral solidification superposition of electric field improves polycrystalline silicon purifying yield, which is characterized in that including water-cooled column, institute
The side-wall outer side for stating water-cooled column is equipped with graphite sleeve, and the side-wall outer side of the graphite sleeve is equipped with graphite crucible, the water-cooled column,
The axis of the graphite sleeve and the graphite crucible is located along the same line, and the side-wall outer side of the graphite crucible is equipped with annular
The side-wall outer side of heater, the annular heater is equipped with annular-heating body, and the bottom of the graphite crucible is equipped with rotary-tray,
Circulatory flow is equipped in the water-cooled column, the graphite sleeve and the graphite crucible are connect with power positive cathode respectively.
The graphite sleeve is connect with the rotary-tray.The rotary-tray can make the graphite crucible and the graphite
Sleeve is rotated by axis of its axis respectively.
The graphite sleeve damages the water-cooled column for preventing silicon material from splashing.
The material of the water-cooled column is stainless steel or copper.
The annular heater is ring-shaped graphite heater.
The annular-heating body is toroidal inductor or ring-shaped graphite electrode.
The inner wall of the graphite crucible is coated with coating, and the coating is silicon carbide or silicon nitride layer, the graphite crucible
Topple over demoulding after facilitating polycrystalline silicon ingot casting to solidify in isosceles trapezoid shape in longitudinal section.
The invention also discloses a kind of sides for improving polycrystalline silicon purifying yield using above equipment lateral solidification superposition of electric field
Method, it is characterised in that there are following steps：
S1, silicon material is placed in the graphite crucible, reaction compartment, which is evacuated to 0.1-3Pa backlash, to be entered to flow argon
Gas, it is 60000-100000Pa to make pressure in reaction compartment, and the annular-heating body will be described with the heating rate of 10 DEG C/min
Annular heater is heated to 1550 DEG C, keeps the temperature 0.5-1h, the silicon melt being completely melt；
Cooling water is poured in S2, the circulatory flow, opening the power supply makes the graphite sleeve and the graphite crucible
Between form electric field, start after the outer wall forming core of the graphite sleeve after polysilicon, the graphite sleeve and the graphite earthenware
Crucible is rotated with the rotary-tray with the speed of 1-300r/min, meanwhile, the annular heater is with the cooling speed of 1-10 DEG C/h
Degree makes the inside in the graphite crucible form stable temperature gradient, promotes polysilicon along radial direction with 0.7mm-
The speed of 2mm/min is grown；
S3, when 80% silicon melt is frozen into polysilicon, the rotary speed of the rotary-tray promotes 10-50%, together
When, increase the electric current of the power supply, improves the fractional condensation of impurity；
S4, when 90% silicon melt is frozen into polysilicon, close the power supply, take out the water-cooled column and the graphite
Casing.
The electric current of power supply described in the step S2 is 1A-50A.
The enrichment that the power positive cathode realizes different impurities can be exchanged, for example, institute can be added on the graphite bush
State power supply positive electricity, on the graphite crucible plus the power supply negative electricity, since the electronegativity of iron, copper is higher than silicon, in electric field force and
Under the collective effect of centrifugal force, the elements such as iron, copper can be flowed to the graphite crucible side-walls, and it is miscellaneous that iron, copper may be implemented in this way
The enrichment of matter；The electronegativity such as titanium, aluminium, magnesium are less than with the metal of silicon, the power positive cathode position, realization pair can be exchanged
The enrichment of the metals such as titanium, aluminium, magnesium.
The present invention and reduces solid-liquid using the mode of lateral solidification superposition of electric field using centrifugal force and electric field force
Interface diffusion layer thickness increases it and segregates effect.
The present invention has the following advantages：
1. effectively improving polycrystal silicon ingot utilization rate 5~10%；
2. realizing high-purity region proportion, practical yield 5~15% is improved.
3, separation of solid and liquid easy to implement prevents the back-diffusion of impurity.
The present invention can be widely popularized in fields such as polycrystalline silicon purifyings based on the above reasons.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 be the present invention specific implementation mode in a kind of lateral solidification superposition of electric field improve setting for polycrystalline silicon purifying yield
Standby structural schematic diagram.
Specific implementation mode
Embodiment 1
As shown in Figure 1, the equipment that a kind of lateral solidification superposition of electric field improves polycrystalline silicon purifying yield, including water-cooled column 1, institute
The side-wall outer side for stating water-cooled column 1 is equipped with graphite sleeve 2, and the side-wall outer side of the graphite sleeve 2 is equipped with graphite crucible 3, the water
The axis of cold column 1, the graphite sleeve 2 and the graphite crucible 3 is located along the same line, outside the side wall of the graphite crucible 3
Side is equipped with annular heater 4, and the side-wall outer side of the annular heater 4 is equipped with annular-heating body 5, the bottom of the graphite crucible 3
Portion is equipped with rotary-tray 6, is equipped with circulatory flow 7 in the water-cooled column 1, the graphite sleeve 2 and the graphite crucible 3 respectively with
8 positive and negative anodes of power supply connect.
The graphite sleeve 2 is connect with the rotary-tray 6.
The material of the water-cooled column 1 is stainless steel or copper.
The annular heater 4 is ring-shaped graphite heater.
The annular-heating body 5 is toroidal inductor or ring-shaped graphite electrode.
The inner wall of the graphite crucible 3 is coated with coating, and the coating is silicon carbide or silicon nitride layer, the graphite crucible 3
Longitudinal section in fall isosceles trapezoid shape.
Embodiment 2
A method of improving polycrystalline silicon purifying yield, tool using equipment lateral solidification superposition of electric field described in embodiment 1
It has the following steps：
S1, silicon material is placed in the graphite crucible 3, reaction compartment, which is evacuated to 0.1-3Pa backlash, to be entered to flow argon
Gas, it is 60000-100000Pa to make pressure in reaction compartment, and the annular-heating body 5 will be described with the heating rate of 10 DEG C/min
Annular heater 4 is heated to 1550 DEG C, keeps the temperature 0.5-1h, the silicon melt 9 being completely melt；
Cooling water is poured in S2, the circulatory flow 7, opening the power supply 8 makes the graphite sleeve 2 and the graphite earthenware
Electric field is formed between crucible 3, is started after the outer wall forming core of the graphite sleeve 2 after polysilicon 10, the graphite sleeve 2 and described
Graphite crucible 3 is rotated with the rotary-tray 6 with the speed of 1-300r/min, meanwhile, the annular heater 4 is with 1-10 DEG C/h
Cooling rate cooling；
S3, when 80% silicon melt 9 is frozen into polysilicon 10, the rotary speed of the rotary-tray 6 promotes 10-
50%, meanwhile, increase the electric current of the power supply 8；
S4, when 90% silicon melt 9 is frozen into polysilicon 10, close the power supply 8, take out the water-cooled column 1 and institute
State graphite bush 2.
The electric current of power supply 8 described in the step S2 is 1A-50A.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. the equipment that a kind of lateral solidification superposition of electric field improves polycrystalline silicon purifying yield, which is characterized in that described including water-cooled column
The side-wall outer side of water-cooled column is equipped with graphite sleeve, and the side-wall outer side of the graphite sleeve is equipped with graphite crucible, the water-cooled column, institute
The axis for stating graphite sleeve and the graphite crucible is located along the same line, and the side-wall outer side of the graphite crucible is equipped with annular and sends out
The side-wall outer side of hot body, the annular heater is equipped with annular-heating body, and the bottom of the graphite crucible is equipped with rotary-tray, institute
It states and is equipped with circulatory flow in water-cooled column, the graphite sleeve and the graphite crucible are connect with power positive cathode respectively.
2. equipment according to claim 1, it is characterised in that：The graphite sleeve is connect with the rotary-tray.
3. equipment according to claim 1, it is characterised in that：The material of the water-cooled column is stainless steel or copper.
4. equipment according to claim 1, it is characterised in that：The annular heater is ring-shaped graphite heater.
5. equipment according to claim 1, it is characterised in that：The annular-heating body is toroidal inductor or annular stone
Electrode ink.
6. according to the equipment described in claim 1-5 any claims, it is characterised in that：The inner wall of the graphite crucible is coated with
Coating, the coating are silicon carbide or silicon nitride layer, and the longitudinal section of the graphite crucible is in isosceles trapezoid shape.
7. a kind of method that equipment lateral solidification superposition of electric field using described in claim 6 improves polycrystalline silicon purifying yield,
It is characterized by having following steps：
S1, silicon material is placed in the graphite crucible, reaction compartment, which is evacuated to 0.1-3Pa backlash, to be entered to flow argon gas, is made
Pressure is 60000-100000Pa in reaction compartment, and the annular-heating body is sent out the annular with the heating rate of 10 DEG C/min
Hot body is heated to 1550 DEG C, keeps the temperature 0.5-1h, the silicon melt being completely melt；
Cooling water is poured in S2, the circulatory flow, opening the power supply makes between the graphite sleeve and the graphite crucible
Form electric field, start after the outer wall forming core of the graphite sleeve after polysilicon, the graphite sleeve and the graphite crucible with
The rotary-tray is rotated with the speed of 1-300r/min, meanwhile, the annular heater is dropped with the cooling rate of 1-10 DEG C/h
Temperature；
S3, when 80% silicon melt is frozen into polysilicon, the rotary speed of the rotary-tray promotes 10-50%, meanwhile, increase
Add the electric current of the power supply；
S4, when 90% silicon melt is frozen into polysilicon, close the power supply, take out the water-cooled column and the graphite cannula
Pipe.
8. according to the method described in claim 7, it is characterized in that：The electric current of power supply described in the step S2 is 1A-50A.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611258337.8A CN106587071B (en) | 2016-12-30 | 2016-12-30 | A kind of lateral solidification superposition of electric field improves the device and method of polycrystalline silicon purifying yield |
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| CN201611258337.8A CN106587071B (en) | 2016-12-30 | 2016-12-30 | A kind of lateral solidification superposition of electric field improves the device and method of polycrystalline silicon purifying yield |
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| CN106587071A CN106587071A (en) | 2017-04-26 |
| CN106587071B true CN106587071B (en) | 2018-09-04 |
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| 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 |
|---|---|---|---|---|
| CN202529852U (en) * | 2011-12-08 | 2012-11-14 | 王洪举 | Polycrystalline silicon centrifuging purifying furnace |
| US8409319B2 (en) * | 2008-08-12 | 2013-04-02 | Ulvac, Inc. | Silicon purification method |
| CN104131342A (en) * | 2014-07-17 | 2014-11-05 | 大连理工大学 | Electromagnetic disturbance polysilicon impurity-removing device and method |
| CN105819451A (en) * | 2016-03-08 | 2016-08-03 | 大连理工大学 | Technology for inducing alloy directional solidification growth and reinforcing alloy refining process by direct current electric field |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8427915D0 (en) * | 1984-11-05 | 1984-12-12 | Tsl Thermal Syndicate Plc | Vitreous silica products |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8409319B2 (en) * | 2008-08-12 | 2013-04-02 | Ulvac, Inc. | Silicon purification method |
| CN202529852U (en) * | 2011-12-08 | 2012-11-14 | 王洪举 | Polycrystalline silicon centrifuging purifying furnace |
| CN104131342A (en) * | 2014-07-17 | 2014-11-05 | 大连理工大学 | Electromagnetic disturbance polysilicon impurity-removing device and method |
| CN105819451A (en) * | 2016-03-08 | 2016-08-03 | 大连理工大学 | Technology for inducing alloy directional solidification growth and reinforcing alloy refining process by direct current electric field |
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