CN107858751A - A kind of crystal pulling method for improving pulling of crystals method crystal forming rate - Google Patents
A kind of crystal pulling method for improving pulling of crystals method crystal forming rate Download PDFInfo
- Publication number
- CN107858751A CN107858751A CN201610841507.9A CN201610841507A CN107858751A CN 107858751 A CN107858751 A CN 107858751A CN 201610841507 A CN201610841507 A CN 201610841507A CN 107858751 A CN107858751 A CN 107858751A
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- Prior art keywords
- pulling
- crystal
- flow amount
- argon flow
- seeding
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of crystal pulling method for improving pulling of crystals method crystal forming rate disclosed by the invention, including step：Draw and propose one section of polycrystalline；Heating power is brought up to more than seeding power, reduces argon flow amount, and silica crucible position is dropped to below seeding crucible position with the impurity that volatilizees；Brushed after adjustment argon flow amount, setting throttle valve opening；Readjust silica crucible position and change seed crystal and weight, adjust silica crucible rotating speed and argon flow amount；Then seeding, shouldering, isometrical, ending, blowing out process are performed using pulling of crystals method, obtains monocrystalline bar.A kind of crystal pulling method of raising pulling of crystals method crystal forming rate of the present invention is solved the problems, such as during existing pulling of crystals method crystal pulling because monocrystalline table causes crystal into brilliant difficult extremely, it passes through the change to step during crystal pulling and parameter, crystal is reduced into brilliant difficulty, reduce personnel labor intensity, reduce production cost, improve single crystal growing furnace monocrystalline crystal forming rate and yield rate.
Description
Technical field
The invention belongs to monocrystalline silicon manufacturing technology field, and in particular to a kind of crystal pulling side for improving pulling of crystals method crystal forming rate
Method.
Background technology
At present, photovoltaic industry pulling monocrystal silicon rod, more than 80% is there are about using cutting krousky
(Czochralski) method manufactures, and is commonly called as pulling of crystals method, and whole technological process is roughly divided into charging, material, proposes impurity, adjusts
The work step such as temperature, seeding, shouldering, isometrical, ending, blowing out.
Due to the competition of polycrystalline and monocrystalline, the electric cost of plating, monocrystalline manufacturing cost and crystal quality aspect are finally embodied in,
Therefore for pulling of crystals, it is particularly important that production cost, lifting crystal quality are reduced.In photovoltaic industry, in pulling monocrystal mistake
Cheng Zhong, because the monocrystalline table caused by factor such as silica crucible exception, unit exception, personnel's maloperation and material quality difference is transported
Row is abnormal, can all cause crystal to draw into brilliant difficulty and put number increase, run time lengthens, and can eventually even cause can not be normal
Pulling monocrystal so that the production cost increase of pulling monocrystal, personnel labor intensity increase, under single stove monocrystalline crystal forming rate and yield rate
Drop.
The content of the invention
It is an object of the invention to provide a kind of crystal pulling method for improving pulling of crystals method crystal forming rate, solves existing straight
During crystal pulling crystal pulling due to monocrystalline table cause extremely crystal into it is brilliant difficult the problem of.
A kind of technical scheme of the present invention is：A kind of crystal pulling method for improving pulling of crystals method crystal forming rate, including
Following steps：
The first step, draw and propose one section of polycrystalline；
Second step, heating power being brought up to more than seeding power, adjustment argon flow amount is less than normal crystal pulling argon flow amount,
And silica crucible position is dropped to below seeding crucible position and is kept for a period of time with the impurity that volatilizees；
3rd step, adjustment argon flow amount are brushed and protected higher than after normal crystal pulling argon flow amount, setting throttle valve opening
Hold a period of time；
4th step, readjust silica crucible position and change seed crystal and weight, adjust silica crucible rotating speed and argon gas stream
Amount；
5th step, the follow-up seeding of pulling of crystals method, shouldering, isometrical, ending, blowing out process are then performed, obtains monocrystalline
Bar.
The features of the present invention also resides in,
The polycrystalline quality for drawing and proposing in the first step is that the 10%-20% of material quality is remained in silica crucible.
Heating power is higher 10kW than seeding power in second step, and argon flow amount is lower 20slpm than normal crystal pulling argon flow amount,
Silica crucible position drops to 20mm-30mm below seeding crucible position and keeps 1.2h-1.8h with the impurity that volatilizees.
Argon flow amount is set as that 80slpm-100slpm, throttle valve opening are set as 95% in 3rd step, then brushes
25min-35min。
3mm-5mm below silica crucible position adjustment to seeding crucible position in 4th step, the rotating ratio of silica crucible routinely turn
The high 1 turn/min-3 of speed turns/min, and argon flow amount gives normal crystal pulling argon flow amount ± 20slpm.
The beneficial effects of the invention are as follows：A kind of crystal pulling method of raising pulling of crystals method crystal forming rate of the present invention solves existing
During some pulling of crystals method crystal pullings due to monocrystalline table cause extremely crystal into it is brilliant difficult the problem of.One kind of the present invention carries
The crystal pulling method of high pulling of crystals method crystal forming rate reduces crystal Cheng Jingnan by the change to step during crystal pulling and parameter
Degree, personnel labor intensity is reduced, reduces production cost, improves single crystal growing furnace monocrystalline crystal forming rate and yield rate.
Embodiment
A kind of crystal pulling method of raising pulling of crystals method crystal forming rate of the present invention, specific aim processing crystal pulling process exception table
Into brilliant technique, specifically include following steps：
The first step, draw and propose one section of polycrystalline；So do after on the one hand helping to stagger and repeatedly drawing and put, in silicon liquid and stove
Corrosion or crystallization of the atmosphere to inner surface of crucible herein, cause to draw and put difficulty；On the other hand one section of melt is proposed, helps to propose
The impurity of part surface of the silicon liquid；
The polycrystalline quality for drawing and proposing in the first step, depending on the initially surplus doses in run time and stove, propose
Polycrystalline quality accounts for the 10%-20% of surplus material quality.
Second step, heater power is brought up to more than seeding power, adjustment argon flow amount is less than normal crystal pulling argon gas stream
Amount, and silica crucible position is dropped to below seeding crucible position and is kept for a period of time with the impurity that volatilizees, as volatile matter SiO in stove,
Impurity etc. in silicon liquid；
Example, heater power is higher 10kW than seeding power in second step, and argon flow amount is lower than normal crystal pulling flow
20slpm, silica crucible position drop to 20mm-30mm below seeding crucible position and keep 1.2-1.8h with the impurity that volatilizees.
3rd step, adjustment argon flow amount is brushed after being higher than normal crystal pulling argon flow amount, setting throttle valve opening, and is protected
Hold a period of time；So do and on the one hand brush ullage part or the white residue and batting of body of heater surface attachment, reduce crystal pulling
During the risk that drops of impurity；On the other hand, there is center to blow to edge the impurity of surface of the silicon liquid and be attached to crucible internal walls,
To reduce the impurity of crystal growth interface；
Example, argon flow amount is higher than normal crystal pulling argon flow amount 20slpm-40slpm, throttle valve opening in the 3rd step
95% is set to, and brushes 25min-35min.
4th step, readjust silica crucible position and change seed crystal and weight, adjust silica crucible rotating speed and argon gas stream
Measure, do not occur air-back in stove, argon flow amount is the bigger the better, and vice versa；Crucible position is lowerd, and reduces argon flow amount to liquid level
Effect, contribute to the expansion of shouldering prometaphase shoulder diameter, the success rate of shouldering can be improved；Seed crystal is changed to be to reduce brilliant change
The probability of generation；On the one hand impurity that weight proposes weight surface attachment is changed, this stove weight exception is on the other hand reduced, if not
Vertically, collide with；Improve crucible to turn to contribute to the stability for lifting silicon liquid temperature, be easy into crystalline substance；After gas being returned in stove, ullage drift
Floating impurity is more, need to reduce argon flow amount, reduces the risk that impurity drops, and does not return steam stove platform, and increase argon flow amount more helps
In the discharge of volatile matter in stove, pure environment is created for crystal pulling；
Example, 3mm-5mm below silica crucible position adjustment to normal seeding crucible position in the 4th step, silica crucible
The high 1 turn/min-3 of rotating ratio conventional rotating speed turns/min, and argon flow amount gives normal argon flow amount ± 20slpm, do not returned in stove
Gas phenomenon, argon flow amount are the bigger the better, and vice versa.
5th step, normal pulling of crystals method subsequent technique is then performed, seeding, shouldering, isometrical, ending, blowing out process, is obtained
To monocrystalline bar.
With reference to specific embodiment, the present invention is described in detail.
The crystal pulling method for solving pulling of crystals method difficulty Cheng Jing of the present embodiment, to remain molten silicon of the material for 100kg or so in stove,
Seeding power 55kW, normal seeding crucible position 100mm, normal crystal pulling argon flow amount 60slpm, 7 turns/min of crystal pulling crucible rotation, stove
Inside return gas it is serious exemplified by, carry out crystal pulling specification, it comprises the following steps：
The first step, draw and propose one section of 10kg-20kg polycrystalline；
Second step, heating power is improved into 65kW, reduce argon flow amount and dropped to 40slpm, and by silica crucible position
70mm-80mm simultaneously keeps 1.2h-1.8h with the impurity that volatilizees；
3rd step, adjustment argon flow amount be 80slpm-100slpm, set throttle valve opening as 95% after brush 25min-
35min；
4th step, silica crucible position is readjusted to 95mm-97mm, and change seed crystal and weight, adjust silica crucible
Rotating speed turns/min to 8 turns/min-10, and argon flow amount is given into 40slpm；
5th step, normal pulling of crystals method subsequent technique is then performed, seeding, shouldering, isometrical, ending, blowing out process, is obtained
To monocrystalline bar.
Claims (5)
- A kind of 1. crystal pulling method for improving pulling of crystals method crystal forming rate, it is characterised in that comprise the following steps：The first step, draw and propose one section of polycrystalline；Second step, heating power is brought up to more than seeding power, adjustment argon flow amount is less than normal crystal pulling argon flow amount, and will Silica crucible position, which is dropped to below seeding crucible position, is kept for a period of time with the impurity that volatilizees；3rd step, adjustment argon flow amount after normal crystal pulling argon flow amount, setting throttle valve opening higher than being brushed and keep one The section time；4th step, readjust silica crucible position and change seed crystal and weight, adjust silica crucible rotating speed and argon flow amount；5th step, the follow-up seeding of pulling of crystals method, shouldering, isometrical, ending, blowing out process are then performed, obtains monocrystalline bar.
- 2. a kind of crystal pulling method for improving pulling of crystals method crystal forming rate as claimed in claim 1, it is characterised in that described first The polycrystalline quality for drawing and proposing in step is that the 10%-20% of material quality is remained in silica crucible.
- 3. a kind of crystal pulling method for improving pulling of crystals method crystal forming rate as claimed in claim 1, it is characterised in that described second Heating power is higher 10kW than seeding power in step, and argon flow amount is lower 20slpm than normal crystal pulling argon flow amount, silica crucible position Drop to 20mm-30mm below seeding crucible position and keep 1.2h-1.8h with the impurity that volatilizees.
- 4. a kind of crystal pulling method for improving pulling of crystals method crystal forming rate as claimed in claim 1, it is characterised in that the described 3rd Argon flow amount is set as that 20slpm-40slpm, throttle valve opening are set as 95% in step, then brushes 25min-35min.
- 5. a kind of crystal pulling method for improving pulling of crystals method crystal forming rate as claimed in claim 1, it is characterised in that the described 4th 3mm-5mm below silica crucible position adjustment to seeding crucible position in step, the rotating ratio conventional rotating speed of the silica crucible is high 1 turn/ Min-3 turns/min, and the argon flow amount gives normal crystal pulling argon flow amount ± 20slpm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610841507.9A CN107858751A (en) | 2016-09-22 | 2016-09-22 | A kind of crystal pulling method for improving pulling of crystals method crystal forming rate |
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|---|---|---|---|
| CN201610841507.9A CN107858751A (en) | 2016-09-22 | 2016-09-22 | A kind of crystal pulling method for improving pulling of crystals method crystal forming rate |
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| CN107858751A true CN107858751A (en) | 2018-03-30 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109468681A (en) * | 2018-11-30 | 2019-03-15 | 邢台晶龙新能源有限责任公司 | A kind of single crystal growing furnace argon gas energy conservation Supply Method |
| CN111394783A (en) * | 2019-01-02 | 2020-07-10 | 宁夏隆基硅材料有限公司 | Crystal pulling method |
| CN113373508A (en) * | 2020-02-25 | 2021-09-10 | 内蒙古中环协鑫光伏材料有限公司 | Section-taking crystallization process |
| CN115369482A (en) * | 2021-05-21 | 2022-11-22 | 内蒙古中环协鑫光伏材料有限公司 | Limit crystal pulling process suitable for material suction experiment |
| WO2023207641A1 (en) * | 2022-04-29 | 2023-11-02 | Tcl中环新能源科技股份有限公司 | Process for increasing crystallization rates in shoulder expansion and isodiametric early stage of large-size single crystal |
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Patent Citations (8)
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| JPH10324596A (en) * | 1997-05-23 | 1998-12-08 | Shin Etsu Handotai Co Ltd | Production of silicon single crystal |
| CN101148777A (en) * | 2007-07-19 | 2008-03-26 | 任丙彦 | Method and device for growing gallium-mixing silicon monocrystal by czochralski method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109468681A (en) * | 2018-11-30 | 2019-03-15 | 邢台晶龙新能源有限责任公司 | A kind of single crystal growing furnace argon gas energy conservation Supply Method |
| CN111394783A (en) * | 2019-01-02 | 2020-07-10 | 宁夏隆基硅材料有限公司 | Crystal pulling method |
| CN113373508A (en) * | 2020-02-25 | 2021-09-10 | 内蒙古中环协鑫光伏材料有限公司 | Section-taking crystallization process |
| CN115369482A (en) * | 2021-05-21 | 2022-11-22 | 内蒙古中环协鑫光伏材料有限公司 | Limit crystal pulling process suitable for material suction experiment |
| WO2023207641A1 (en) * | 2022-04-29 | 2023-11-02 | Tcl中环新能源科技股份有限公司 | Process for increasing crystallization rates in shoulder expansion and isodiametric early stage of large-size single crystal |
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