CN106222735A - Improve the device and method of pulling of silicon single crystal pulling rate - Google Patents
Improve the device and method of pulling of silicon single crystal pulling rate Download PDFInfo
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- CN106222735A CN106222735A CN201610732992.6A CN201610732992A CN106222735A CN 106222735 A CN106222735 A CN 106222735A CN 201610732992 A CN201610732992 A CN 201610732992A CN 106222735 A CN106222735 A CN 106222735A
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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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
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Abstract
The invention discloses a kind of device improving pulling of silicon single crystal pulling rate and include that the cooling body of cylindrical shape, cooling medium inlet pipe, cooling medium go out pipe；The method improving pulling of silicon single crystal pulling rate comprises the steps: that (1) prepares, (2) heating material, (3) intermediate treatment, and (4) are isometrical, (5) ending and post processing.It is an advantage of the current invention that, advantages of the present invention: utilize the principle of inert element cooling medium gasification heat absorption, increase the axial-temperature gradient of silicon single crystal rod, makes monocrystal silicon pulling rate improve more than 20%, owing to not changing the mechanisms such as the top insulation of thermal field system, extra energy consumption is not therefore had to increase；Inert element cooling medium recycles, and reduces monocrystalline silicon production cost；The inert element cooling medium used is liquid helium or liquid argon, does not reacts with silicon melt, will not impact thermal field component, and more conventional method is safer, improves the safety of monocrystalline silicon production.
Description
Technical field:
The present invention relates to monocrystalline silicon production field, particularly to a kind of device and method improving pulling of silicon single crystal pulling rate.
Background technology:
Monocrystal silicon is the important component part of crystalline material, its be mainly used as semi-conducting material and solar energy power generating,
Heat supply assembly etc..In the last thirty years, along with the fast development of new energy technology, especially solar energy industry are research and development, business
Fast development in terms of industry metaplasia product, market development, increases sharply year by year for the demand of monocrystal silicon in market.Due to traditional monocrystalline
Silicon generates that the processing enterprise level of production is relatively low, and generation technique level is the highest, ultimately causes that monocrystalline silicon production efficiency is low, cost is high,
This pole is unfavorable for that monocrystal silicon generates the development of processing enterprise, and therefore monocrystal silicon generates processing enterprise and also exploring raising generation effect
Rate, the monocrystalline silicon production method of reduction cost.
The energy conservation equation of the growth interface according to pulling of silicon single crystal: Qin+QL=Qout→kmeltGmelt+ LV=kcryGcry
Wherein, QinFor the heat of the incoming crystalizing interface of melt, QoutThe heat paid to crystal for crystalizing interface, QLFor latent heat.?
Go out the real crystal speed of growth as follows:
Wherein, VcrysFor monocrystalline silicon growing speed, GcrysFor the axial-temperature gradient near grain boundary, GmeltFor growth
Axial-temperature gradient near interface melt, KcrysWith KmeltBeing respectively the heat transfer coefficient of crystal and melt, A is crystalizing interface
Area, DcrysFor the area of crystallization, L is latent heat.
Time from above formula it can be seen that grow fixed diameter monocrystal silicon, except crystal axial-temperature gradient GcrysWith melt
Axial-temperature gradient GmeltFor variable value, other is fixed value, and therefore improving pulling of silicon single crystal pulling rate should be near interface
The axial-temperature gradient of crystal and melt sets out, it may be assumed that 1. increase on interface axial-temperature gradient G in square crystalcrys；2. boundary is reduced
Axial-temperature gradient G in melt below facemelt。
The current method improving pulling of silicon single crystal pulling rate has:
1, weaken the methods such as the top insulation of thermal field system, the mechanism changing heat shielding or material and improve axial-temperature gradient,
And then raising pulling rate；The method can add the heat of melt simultaneously and scatter and disappear, and adds energy consumption, as a example by 26 cun of thermal fields, and upper guarantor
Temperature thickness often reduces 10mm, and power consumption increases about 3%.
2, use water device ring around silicon single crystal rod, improve axial-temperature gradient, and then improve pulling rate.Although the method
Pulling rate can be effectively improved；But furnace high-temperature, once occurring leaking vaporizing immediately reacts with thermal field component in stove, makes
Thermal field component cannot use.
Summary of the invention:
First purpose of the present invention is to provide one can reduce silicon single crystal rod axial-temperature gradient, reduce production cost
Improve pulling of silicon single crystal pulling rate device.
Second object of the present invention is that providing a kind of generates raising vertical pulling list that safety coefficient is high, that production efficiency is high
The method of crystal silicon pulling rate.
First purpose of the present invention is implemented by following technical scheme, improves the device of pulling of silicon single crystal pulling rate, and it includes
Cooling body, cooling medium inlet pipe, cooling medium go out pipe, and described cooling body includes the cooling of lower open mouth, hollow cylindrical
If main body and dry tablet fin, described cooling main body includes some sections of VERTICAL TUBE and some sections of U-tube, adjacent two sections of described VERTICAL TUBE
The mouth of pipe between be provided with one section of described U-tube, between adjacent described VERTICAL TUBE and described U-tube head and the tail be sequentially communicated composition snakelike
Coil pipe, is arranged with fin described in a pair on outer wall inside every section of described VERTICAL TUBE, be provided with in the upper end of described cooling main body with
The described cooling medium inlet pipe of described cooling body interior connection, is provided with and described cooling main body in the lower end of described cooling main body
The described cooling medium of internal connection goes out pipe.
Further, described cooling medium inlet pipe goes out pipe with described cooling medium and is oppositely arranged.
Further, the ratio of the height H and diameter D of described cooling main body is 1:2-3.
Further, described fin is high temperature resistant fin, fin described in adjacent two in VERTICAL TUBE described in the most adjacent two
Between angle α be 90 °-150 °.
Further, described cooling medium go out pipe connect with cooling medium recycling can.
Second object of the present invention is implemented by following technical scheme, and what the device of raising pulling of silicon single crystal pulling rate was carried out carries
The method of high pulling of silicon single crystal pulling rate, it comprises the steps: that (1) prepares, (2) heating material, (3) intermediate treatment, (4) etc.
Footpath, (5) ending and post processing；Wherein,
(1) prepare: described cooling body is installed at the above 500-1000mm in monocrystalline silicon growing interface；
(2) heating material: after being ready to complete, polycrystalline silicon raw material is placed in silica crucible and evacuation, backward described
Silica crucible is passed through argon so that the furnace pressure in described silica crucible is 10-20torr, treats the furnace pressure in described silica crucible
Beginning to warm up material after Wen Ding, heating power is 70-100kw, is entered by described cooling medium while described heating material
Pipe carries inert element cooling medium in described cooling body, and the feed flow of described inert element cooling medium is 20-
50mL/min, the described heating material time is 5-10h；
(3) intermediate treatment: after heating material terminates, carries out steady temperature, seeding, shouldering successively, turns shoulder, in described steady temperature, institute
State during seeding, described shouldering, described turn of shoulder all with the feed flow of 20-50mL/min in described cooling medium inlet pipe defeated
Send described inert element cooling medium；
(4) isometrical: after intermediate treatment terminates, after entering the isometrical stage, the feed flow of described inert element cooling medium
Increasing to 50-100mL/min, now pull rate is set to 60-75mm/min, treats that monocrystal silicon head enters described cooling body
During 200-300mm, the feed flow of described inert element cooling medium increases to 100-200mL/min, and described pull rate carries
Up to 62-80mm/min, treats that the head of described monocrystal silicon enters described higher than the afterbody of described cooling body and described monocrystal silicon
After cooling body, the feed flow of described inert element cooling medium maintains 100-200mL/min, and described pull rate improves
To 67-90mm/min；When to described silica crucible, remaining described raw material liq is 7-10Kg, the described isometrical stage terminates；
(5) ending and post processing: enter finishing phase, the most described inert element cooling medium defeated after isometrical end
Sending flow-reduction to 20-50mL/min, after described finishing phase terminates, blowing out cools down, and 200-is improved in the position of described monocrystal silicon
400mm, the position of described silica crucible reduces 100-200mm, and the feed flow of the most described inert element cooling medium maintains
At 20-50mL/min until tearing stove open, described in tear open when stove starts stop in described cooling medium inlet pipe, be passed through described inert element
Cooling medium.
Further, described step (2) heating material, described step (3) intermediate treatment, described step (4) isometrical and
Described step (5) ending and last handling process are entered the described inertia unit in described cooling body by described cooling medium inlet pipe
Element cooling medium is gone out bank of tubes by described cooling medium and goes out and be recycled in described cooling medium recycling can.
Further, described inert element cooling medium is the one in liquid helium or liquid argon.
Further, in described step (3) intermediate treatment, the heating power during described steady temperature is 40-70kw, surely temperature
Time is 1-3h；During described seeding, the distance of described raw material liq to described silica crucible guide shell is 10-25mm, brilliant
Rotary speed is 6-14r/min, and described silica crucible rotating speed is 6-12r/min, and seeding total length is 100-200mm, and seeding is average
Pulling rate is 100-200mm/h；During described shouldering, shouldering pulling rate is 40-70mm/h, and heating power is 40-70kw, during shouldering
Between be 1.5-3h；During described turn of shoulder, turning shoulder pulling rate is 80-180mm/h.
Advantages of the present invention: 1, inert element cooling medium is entered inside cooling wall by cooling medium inlet pipe, and by cooling down
Medium goes out bank of tubes and goes out, and utilizes the principle of inert element cooling medium gasification heat absorption, increases the axial-temperature gradient of silicon single crystal rod, make
Monocrystal silicon pulling rate improves more than 20%, owing to not changing the mechanisms such as the top insulation of thermal field system, does not therefore have extra energy consumption
Increase；2, via cooling medium go out that bank of tubes goes out, gasification after inert element cooling medium be recycled in cooling medium recycling can,
Make inert element cooling medium recoverable, reduce monocrystalline silicon production cost；3, cooling wall can be passed through by control
Interior inert element cooling medium consumption controls pulling rate, to improve monocrystalline silicon production controllability；4, the inert element cooling used
Medium is liquid helium or liquid argon, even if there is leakage, inert element cooling medium does not reacts with silicon melt, will not be to thermal field portion
Part impacts, and more conventional method is safer, improves the safety of monocrystalline silicon production.
Accompanying drawing illustrates:
Fig. 1 is the overall structure schematic diagram of embodiment 1.
Fig. 2 is the top view of Fig. 1.
Fig. 3 is the overall structure schematic diagram of embodiment 2.
Fig. 4 is the top view of Fig. 3.
Cooling body 1, cooling medium inlet pipe 2, cooling medium goes out pipe 3, cools down main body 4, fin 5, VERTICAL TUBE 6, U-tube 7,
Cooling medium recycling can 8.
Detailed description of the invention:
Embodiment 1:
As shown in Figure 1-2, improving the device of pulling of silicon single crystal pulling rate, it includes cooling body 1, cooling medium inlet pipe 2, cold
But medium goes out pipe 3, and cooling body 1 includes lower open mouth, the cooling main body 4 of hollow cylindrical and 60 fins 5, cools down main body
The ratio of the height H and diameter D of 4 is 1:2, and cooling main body 4 includes 30 sections of VERTICAL TUBE 6 and 30 sections of U-tube 7, adjacent two sections
Being provided with one section of U-tube 7 between the mouth of pipe of VERTICAL TUBE 6, between adjacent upright pipe 6 and U-tube 7, head and the tail are sequentially communicated the snakelike dish of composition
Pipe, is arranged with a pair fin 5 on outer wall inside each VERTICAL TUBE 6, fin 5 is high temperature resistant fin, and it is main that fin 5 can increase cooling
The area of dissipation of body 4；The angle α between two fins 5 adjacent in two the most adjacent VERTICAL TUBE 6 is 150 °, in cooling main body 4
Upper end is provided with and cools down the internal cooling medium inlet pipe 2 connected of main body 4, is provided with and cools down in the lower end of cooling main body 4 in main body 4
The cooling medium of portion's connection goes out pipe 3, and inert element cooling medium is entered in cooling main body 4 by cooling medium inlet pipe 2, and by cooling down
Medium goes out pipe 3 and discharges, and utilizes the principle of inert element cooling medium gasification heat absorption, increases the axial-temperature gradient of silicon single crystal rod,
Monocrystal silicon pulling rate is made to improve more than 20%；Cooling medium goes out pipe 3 and connects with cooling medium recycling can 8, goes out pipe 3 via cooling medium
Discharge, gasification after inert element cooling medium be recycled in cooling medium recycling can 8 so that inert element cooling medium can
Recycle, reduce monocrystalline silicon production cost；Cooling medium inlet pipe 2 and cooling medium go out pipe 3 and are oppositely arranged, it is ensured that cooling is main
The stability of temperature inside body 4.
Embodiment 2:
As shown in Figure 3-4, improving the device of pulling of silicon single crystal pulling rate, it includes cooling body 1, cooling medium inlet pipe 2, cold
But medium goes out pipe 3, and cooling body 1 includes lower open mouth, the cooling main body 4 of hollow cylindrical and 60 fins 5, cools down main body
The ratio of the height H and diameter D of 4 is 1:3, and cooling main body 4 includes 30 sections of VERTICAL TUBE 6 and 30 sections of U-tube 7, adjacent two sections
Being provided with one section of U-tube 7 between the mouth of pipe of VERTICAL TUBE 6, between adjacent upright pipe 6 and U-tube 7, head and the tail are sequentially communicated the snakelike dish of composition
Pipe, is arranged with a pair fin 5 on outer wall inside each VERTICAL TUBE 6, fin 5 is high temperature resistant fin 5, and fin 5 can increase cooling
The area of dissipation of main body 4；The angle α between two fins 5 adjacent in two the most adjacent VERTICAL TUBE 6 is 90 °, in cooling main body 4
Upper end be provided with and cool down the internal cooling medium inlet pipe 2 connect of main body 4, be provided with and cool down main body 4 in the lower end cooling down main body 4
The cooling medium of internal connection goes out pipe 3, and inert element cooling medium is entered in cooling main body 4 by cooling medium inlet pipe 2, and by cold
But medium goes out pipe 3 and discharges, and utilizes the principle of inert element cooling medium gasification heat absorption, increases the axial temperature ladder of silicon single crystal rod
Degree, makes monocrystal silicon pulling rate improve more than 20%；Cooling medium goes out pipe 3 and connects with cooling medium recycling can 8, goes out via cooling medium
Pipe 3 discharge, gasification after inert element cooling medium be recycled in cooling medium recycling can 8 so that inert element cooling be situated between
Matter recoverable, reduces monocrystalline silicon production cost；Cooling medium inlet pipe 2 and cooling medium go out pipe 3 and are oppositely arranged, it is ensured that cold
But the stability of temperature inside main body 4.
Embodiment 3:
Utilizing the method improving pulling of silicon single crystal pulling rate that embodiment 1 is carried out, it comprises the steps: that (1) prepares, (2)
Heating material, (3) intermediate treatment, (4) are isometrical, (5) ending and post processing；Wherein,
(1) prepare: cooling body 1 is installed at the above 500mm in monocrystalline silicon growing interface；
(2) heating material: after being ready to complete, polycrystalline silicon raw material is placed in silica crucible and evacuation, backward quartz
Crucible is passed through argon so that the furnace pressure in silica crucible is 10torr, begins to warm up after the furnace pressure in silica crucible is stable
Material, heating power is 70kw, carries inertia unit by cooling medium inlet pipe 2 while heating material in cooling body 1
Element cooling medium, the feed flow of inert element cooling medium is 20mL/min, and the heating material time is 5-10h, to quartz earthenware
Polycrystalline silicon raw material in crucible all turns to raw material liq to be terminated；
(3) intermediate treatment: after heating material terminates, carries out steady temperature, seeding, shouldering successively, turns shoulder, at steady temperature, seeding, put
All in cooling medium inlet pipe 2, inert element cooling medium is carried with the feed flow of 20mL/min during shoulder, turn shoulder；Its
In, the heating power during steady temperature is 40kw, and the steady temperature time is 1h；During seeding, raw material liq is to silica crucible water conservancy diversion
The distance of cylinder is 10mm, and brilliant rotary speed is 6r/min, and silica crucible rotating speed is 6r/min, and seeding total length is 100mm, and seeding is put down
All pulling rates are 100mm/h；During shouldering, shouldering pulling rate is 40mm/h, and heating power is 40kw, and the shouldering time is 1.5h；Turn
During shoulder, turning shoulder pulling rate is 80mm/h.
(4) isometrical: after intermediate treatment completes, after entering the isometrical stage, the feed flow of inert element cooling medium increases
To 50mL/min, now pull rate is set to 60mm/min, when monocrystal silicon head enters cooling body 1 1200mm, and inertia unit
The feed flow of element cooling medium increases to 100mL/min, and pull rate improves to 62mm/min, treats that the head of monocrystal silicon is higher than
After the afterbody of cooling body 1 and monocrystal silicon enters cooling body 1, the feed flow of inert element cooling medium maintains 100mL/
Min, pull rate improves to 67mm/min；When to silica crucible, remaining raw material liq is 7Kg, the isometrical stage terminates；
(5) ending and post processing: enter finishing phase, the now transportation flow of inert element cooling medium after isometrical end
Amount is reduced to 20mL/min, and after finishing phase terminates, blowing out cools down, and 200mm, the position of silica crucible are improved in the position of monocrystal silicon
Reducing 100mm, now the feed flow of inert element cooling medium maintains 20mL/min until tearing stove open, tears open and stops when stove starts
Inert element cooling medium it is passed through in cooling medium inlet pipe 2.
Additionally, step (2) heating material, step (3) intermediate treatment, step (4) are isometrical and step (5) ending and after locate
The inert element cooling medium entered in cooling body 1 by cooling medium inlet pipe 2 during reason is gone out pipe 3 by cooling medium and discharges
And be recycled in cooling medium recycling can 8, inert element cooling medium is liquid helium.
Embodiment 4:
Utilizing the method improving pulling of silicon single crystal pulling rate that embodiment 1 is carried out, it comprises the steps: that (1) prepares, (2)
Heating material, (3) intermediate treatment, (4) are isometrical, (5) ending and post processing；Wherein,
(1) prepare: cooling body 1 is installed at the above 700mm in monocrystalline silicon growing interface；
(2) heating material: after being ready to complete, polycrystalline silicon raw material is placed in silica crucible and evacuation, backward quartz
Crucible is passed through argon so that the furnace pressure in silica crucible is 15torr, begins to warm up after the furnace pressure in silica crucible is stable
Material, heating power is 85kw, carries inertia unit by cooling medium inlet pipe 2 while heating material in cooling body 1
Element cooling medium, the feed flow of inert element cooling medium is 35mL/min, and the heating material time is 7h, to silica crucible
Polycrystalline silicon raw material all turn to raw material liq and terminate；
(3) intermediate treatment: after heating material terminates, carries out steady temperature, seeding, shouldering successively, turns shoulder, at steady temperature, seeding, put
All in cooling medium inlet pipe 2, inert element cooling medium is carried with the feed flow of 35mL/min during shoulder, turn shoulder；Steady temperature
During heating power be 55kw, the steady temperature time is 2h；During seeding, the distance of raw material liq to silica crucible guide shell
For 17mm, brilliant rotary speed is 10r/min, and silica crucible rotating speed is 10r/min, and seeding total length is 150mm, seeding average pull rate
For 150mm/h；During shouldering, shouldering pulling rate is 55mm/h, and heating power is 55kw, and the shouldering time is 2.3h；Turn shoulder process
In, turning shoulder pulling rate is 130mm/h.
(4) isometrical: after intermediate treatment completes, after entering the isometrical stage, the feed flow of inert element cooling medium increases
To 75mL/min, now pull rate is set to 70mm/min, when monocrystal silicon head enters cooling body 1 1250mm, and inertia unit
The feed flow of element cooling medium increases to 150mL/min, and pull rate improves to 71mm/min, treats that the head of monocrystal silicon is higher than
After the afterbody of cooling body 1 and monocrystal silicon enters cooling body 1, the feed flow of inert element cooling medium maintains 150mL/
Min, pull rate improves to 78mm/min；When to silica crucible, remaining raw material liq is 8.5Kg, the isometrical stage terminates；
(5) ending and post processing: enter finishing phase, the now transportation flow of inert element cooling medium after isometrical end
Amount is reduced to 35mL/min, and after finishing phase terminates, blowing out cools down, and 300mm, the position of silica crucible are improved in the position of monocrystal silicon
Reducing 150mm, now the feed flow of inert element cooling medium maintains 35mL/min until tearing stove open, tears open and stops when stove starts
Inert element cooling medium it is passed through in cooling medium inlet pipe 2.
Additionally, step (2) heating material, step (3) intermediate treatment, step (4) are isometrical and step (5) ending and after locate
The inert element cooling medium entered in cooling body 1 by cooling medium inlet pipe 2 during reason is gone out pipe 3 by cooling medium and discharges
And be recycled in cooling medium recycling can 8, inert element cooling medium is liquid argon.
Embodiment 5:
Utilizing the method improving pulling of silicon single crystal pulling rate that embodiment 2 is carried out, it comprises the steps: that (1) prepares, (2)
Heating material, (3) intermediate treatment, (4) are isometrical, (5) ending and post processing；Wherein,
(1) prepare: cooling body 1 is installed at the above 1000mm in monocrystalline silicon growing interface；
(2) heating material: after being ready to complete, polycrystalline silicon raw material is placed in silica crucible and evacuation, backward quartz
Crucible is passed through argon so that the furnace pressure in silica crucible is 20torr, begins to warm up after the furnace pressure in silica crucible is stable
Material, heating power is 100kw, carries inertia unit by cooling medium inlet pipe 2 while heating material in cooling body 1
Element cooling medium, the feed flow of inert element cooling medium is 50mL/min, and the heating material time is 5-10h, to quartz earthenware
Polycrystalline silicon raw material in crucible all turns to raw material liq to be terminated；
(3) intermediate treatment: after heating material terminates, carries out steady temperature, seeding, shouldering successively, turns shoulder, at steady temperature, seeding, put
All in cooling medium inlet pipe 2, inert element cooling medium is carried with the feed flow of 50mL/min during shoulder, turn shoulder；Its
In, the heating power during steady temperature is 70kw, and the steady temperature time is 3h；During seeding, raw material liq is to silica crucible water conservancy diversion
The distance of cylinder is 25mm, and brilliant rotary speed is 14r/min, and silica crucible rotating speed is 12r/min, and seeding total length is 200mm, seeding
Average pull rate is 200mm/h；During shouldering, shouldering pulling rate is 70mm/h, and heating power is 70kw, and the shouldering time is 3h；Turn
During shoulder, turning shoulder pulling rate is 180mm/h.
(4) isometrical: after intermediate treatment completes, after entering the isometrical stage, the feed flow of inert element cooling medium increases
To 100mL/min, now pull rate is set to 75mm/min, when monocrystal silicon head enters cooling body 1 1300mm, and inertia
The feed flow of element cooling medium increases to 200mL/min, and pull rate improves to 80mm/min, treats that the head of monocrystal silicon is high
After the afterbody of cooling body 1 and monocrystal silicon enters cooling body 1, the feed flow of inert element cooling medium maintains
200mL/min, pull rate improves to 90mm/min；When to silica crucible, remaining raw material liq is 10Kg, the isometrical stage
Terminate；
(5) ending and post processing: enter finishing phase, the now transportation flow of inert element cooling medium after isometrical end
Amount is reduced to 50mL/min, and after finishing phase terminates, blowing out cools down, and 400mm, the position of silica crucible are improved in the position of monocrystal silicon
Reducing 200mm, now the feed flow of inert element cooling medium maintains 50mL/min until tearing stove open, tears open and stops when stove starts
Inert element cooling medium it is passed through in cooling medium inlet pipe 2.
Additionally, step (2) heating material, step (3) intermediate treatment, step (4) are isometrical and step (5) ending and after locate
The inert element cooling medium entered in cooling body 1 by cooling medium inlet pipe 2 during reason is gone out pipe 3 by cooling medium and discharges
And be recycled in cooling medium recycling can 8, inert element cooling medium is liquid helium.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (9)
1. improve the device of pulling of silicon single crystal pulling rate, it is characterised in that it includes that cooling body, cooling medium inlet pipe, cooling are situated between
Matter goes out pipe, if described cooling body includes lower open mouth, the cooling main body of hollow cylindrical and dry tablet fin, described cooling main body
Including some sections of VERTICAL TUBE and some sections of U-tube, between the mouth of pipe of adjacent two sections of described VERTICAL TUBE, it is provided with one section of described U-tube,
Between adjacent described VERTICAL TUBE and described U-tube, head and the tail are sequentially communicated composition serpentine coil, outer wall inside every section of described VERTICAL TUBE
On be arranged with fin described in a pair, be provided with described cold with what described cooling body interior connected in the upper end of described cooling main body
But medium inlet pipe, is provided with the described cooling medium connected with described cooling body interior and goes out pipe in the lower end of described cooling main body.
The device of raising pulling of silicon single crystal pulling rate the most according to claim 1, it is characterised in that described cooling medium inlet pipe
Go out pipe with described cooling medium to be oppositely arranged.
The device of raising pulling of silicon single crystal pulling rate the most according to claim 1, it is characterised in that the height of described cooling main body
The ratio of degree H and diameter D is 1:2-3.
The device of raising pulling of silicon single crystal pulling rate the most according to claim 1, it is characterised in that described fin is high temperature resistant
Fin, in VERTICAL TUBE described in the most adjacent two, angle α between fin described in adjacent two is 90 °-150 °.
The device of raising pulling of silicon single crystal pulling rate the most according to claim 1, it is characterised in that described cooling medium goes out pipe
Connect with cooling medium recycling can.
6. the raising pulling of silicon single crystal utilizing the arbitrary described device improving pulling of silicon single crystal pulling rate of claim 1-5 to carry out draws
The method of speed, it is characterised in that it comprises the steps: that (1) prepares, (2) heating material, (3) intermediate treatment, (4) are isometrical,
(5) ending and post processing；Wherein,
(1) prepare: described cooling body is installed at the above 500-1000mm in monocrystalline silicon growing interface；
(2) heating material: after being ready to complete, polycrystalline silicon raw material is placed in silica crucible and evacuation, backward described quartz
Crucible is passed through argon so that the furnace pressure in described silica crucible is 10-20torr, treats that the furnace pressure in described silica crucible is stable
After begin to warm up material, heating power is 70-100kw, while described heating material by described cooling medium inlet pipe to
Conveying inert element cooling medium in described cooling body, the feed flow of described inert element cooling medium is 20-50mL/
Min, the described heating material time is 5-10h；
(3) intermediate treatment: heating after material terminates, carries out steady temperature, seeding, shouldering successively, turns shoulder, described steady temperature, described in draw
All in described cooling medium inlet pipe, institute is carried with the feed flow of 20-50mL/min during shouldering brilliant, described, described turn of shoulder
State inert element cooling medium；
(4) isometrical: after intermediate treatment terminates, after entering the isometrical stage, the feed flow of described inert element cooling medium increases
To 50-100mL/min, now pull rate is set to 60-75mm/min, treats that monocrystal silicon head enters described cooling body 200-
During 300mm, the feed flow of described inert element cooling medium increases to 100-200mL/min, and described pull rate improves extremely
62-80mm/min, treats that the head of described monocrystal silicon enters described cooling higher than the afterbody of described cooling body and described monocrystal silicon
After mechanism, the feed flow of described inert element cooling medium maintains 100-200mL/min, and described pull rate improves extremely
67-90mm/min；When to described silica crucible, remaining described raw material liq is 7-10Kg, the described isometrical stage terminates；
(5) ending and post processing: enter finishing phase, the transportation flow of the most described inert element cooling medium after isometrical end
Amount is reduced to 20-50mL/min, and after described finishing phase terminates, blowing out cools down, and 200-is improved in the position of described monocrystal silicon
400mm, the position of described silica crucible reduces 100-200mm, and the feed flow of the most described inert element cooling medium maintains
At 20-50mL/min until tearing stove open, described in tear open when stove starts stop in described cooling medium inlet pipe, be passed through described inert element
Cooling medium.
The method of raising pulling of silicon single crystal pulling rate the most according to claim 6, it is characterised in that described step (2) heats
Material, described step (3) intermediate treatment, described step (4) be isometrical and in described step (5) ending and last handling process by institute
The described inert element cooling medium stated in the cooling medium inlet pipe described cooling body of entrance is gone out bank of tubes by described cooling medium
Go out and be recycled in described cooling medium recycling can.
8. according to the arbitrary described method improving pulling of silicon single crystal pulling rate of claim 6 or 7, it is characterised in that described inertia
Element cooling medium is the one in liquid helium or liquid argon.
The method of raising pulling of silicon single crystal pulling rate the most according to claim 6, it is characterised in that in the middle of described step (3)
In process, the heating power during described steady temperature is 40-70kw, and the steady temperature time is 1-3h；During described seeding, described former
Feed liquid body is 10-25mm to the distance of described silica crucible guide shell, and brilliant rotary speed is 6-14r/min, and described silica crucible turns
Speed is 6-12r/min, and seeding total length is 100-200mm, and seeding average pull rate is 100-200mm/h；During described shouldering,
Shouldering pulling rate is 40-70mm/h, and heating power is 40-70kw, and the shouldering time is 1.5-3h；During described turn of shoulder, turn shoulder and draw
Speed is 80-180mm/h.
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| WO2021243993A1 (en) * | 2020-06-05 | 2021-12-09 | 隆基绿能科技股份有限公司 | Heat exchange device and single crystal furnace |
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