CN107385507A - A kind of method of monocrystalline silicon crystal pulling device and the application device - Google Patents
A kind of method of monocrystalline silicon crystal pulling device and the application device Download PDFInfo
- Publication number
- CN107385507A CN107385507A CN201710591130.0A CN201710591130A CN107385507A CN 107385507 A CN107385507 A CN 107385507A CN 201710591130 A CN201710591130 A CN 201710591130A CN 107385507 A CN107385507 A CN 107385507A
- Authority
- CN
- China
- Prior art keywords
- nitrogen
- argon gas
- crystal pulling
- heater
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
-
- 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
Abstract
The invention provides a kind of monocrystalline silicon crystal pulling device, including body of heater, Nitrogen source gases and argon gas source of the gas, the Nitrogen source gases are connected by the first pipeline with body of heater, and the argon gas source of the gas is connected by second pipe with body of heater, and first pipeline and second pipe are respectively equipped with mass flowmenter.In a kind of monocrystalline silicon crystal pulling device of the present invention, body of heater is connected with Nitrogen source gases and argon gas source of the gas, meets crystal pulling demand by the conversion of argon gas nitrogen during crystal pulling, is argon gas 1/5 because nitrogen price is low, therefore can reduce gas cost；Simultaneously as the dislocation activation of nitrating silicon single crystal can be higher than conventional single, it is fast that plastic deformation ability by dislocation movement by slip discharges more conventional monocrystalline, therefore nitrating monocrystalline can improve silicon chip mechanical strength and improve silicon chip mechanical strength；Secondly, nitrating promotes oxygen precipitation, reduces void-type defect region；In addition, the crystalline silicon obtained by the installation method, reduces battery light decay.
Description
Technical field
The invention belongs to monocrystalline silicon production technical field, more particularly, to a kind of monocrystalline silicon crystal pulling device and applies the dress
The method put.
Background technology
In vertical pulling technique prepared by monocrystalline silicon, argon gas is needed in crystal growing process as protective gas, continually
Be filled with argon gas and can take away volatile matter and reduce monocrystalline temperature, influenceed by steel industry, existing argon gas price turned over 5 compared with 16 years
Times, also continue growth trend, significantly increase crystal pulling cost.
The content of the invention
In view of this, the present invention is directed to propose a kind of monocrystalline silicon crystal pulling device and method, is given birth to reducing existing monocrystalline silicon
Produce cost.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of monocrystalline silicon crystal pulling device, including body of heater, Nitrogen source gases and argon gas source of the gas, the Nitrogen source gases pass through first
Pipeline is connected with body of heater, and the argon gas source of the gas is connected by second pipe with body of heater, the first pipeline and the second pipe difference
Provided with mass flowmenter.
Further, the body of heater is connected by Two In and One Out triple valve and the first pipeline and second pipe.
Relative to prior art, a kind of monocrystalline silicon crystal pulling of the present invention is had the advantage that with device：
In a kind of monocrystalline silicon crystal pulling device of the present invention, body of heater is connected with Nitrogen source gases and argon gas source of the gas, is drawing
Passing through argon gas during crystalline substance --- nitrogen conversion meets crystal pulling demand, is argon gas 1/5 because nitrogen price is low, therefore can reduce
Gas cost；Simultaneously as the dislocation activation of nitrating silicon single crystal can be higher than conventional single, plastic deformation ability is slided by dislocation
It is fast to move the more conventional monocrystalline of release, therefore nitrating monocrystalline can improve silicon chip mechanical strength and improve silicon chip mechanical strength；Secondly, nitrating
Promote oxygen precipitation, reduce void-type defect region；In addition, the crystalline silicon obtained by the installation method, reduces battery light decay.
A kind of crystal pulling method using monocrystalline silicon crystal pulling device, including material, steady temperature, seeding, shouldering, turn shoulder, be isometrical,
Ending, blowing out section, meet：
1), material section：The argon gas of 50slpm-120slpm flows is passed through into body of heater, and pressure is in holding furnace body
12Torr-17Torr；
2), steady temperature, seeding, shouldering, turn in each section of shoulder, continue to be passed through 50slpm-120slpm flows into body of heater
Argon gas, and pressure 12Torr-17Torr in holding furnace body；
3), isometrical section：
A) it is, isometrical to start to be gradually reduced closing argon gas input when isometrical 200mm of argon gas input quantity, at the same time, to
Input nitrogen in body of heater, and gradually increase nitrogen input quantity until the isometrical 200mm input all nitrogen of gas, now nitrogen is defeated
It is 50slpm-120slpm to enter amount；
B), for isometrical 200mm to isometrical end, it is 50slpm-120slpm to keep nitrogen input flow rate, and in holding furnace body
Pressure 12Torr-17Torr, rate of crystalline growth are more than 84mm/hr；
4) ending section：Continue to input nitrogen into stove, and ensure that nitrogen flow is 50slpm-100slpm, pressure
12Torr-17Torr；
5), blowing out section：Nitrogen is inputted into stove in blowing out 1h, and it is 50slpm-100slpm to keep nitrogen flow,
Nitrogen input is closed after blowing out 1h.
Further, Nitrogen source gases pressure used is equal with argon gas bleed pressure, and the pressure is 0.5Mpa-0.7Mpa.
In a kind of crystal pulling method using monocrystalline silicon crystal pulling device of the present invention, body of heater be connected with Nitrogen source gases and
Argon gas source of the gas, passes through argon gas during crystal pulling --- and nitrogen conversion meets crystal pulling demand, is argon gas 1/5 because nitrogen price is low,
Therefore gas cost can be reduced；Simultaneously as the dislocation activation of nitrating silicon single crystal can be higher than conventional single, plastic deformation
It is fast that more conventional monocrystalline can be discharged by dislocation movement by slip, therefore nitrating monocrystalline can improve silicon chip mechanical strength and improve silicon chip machinery by force
Degree；Secondly, nitrating promotes oxygen precipitation, reduces void-type defect region；In addition, the crystalline silicon obtained by the installation method, subtracts
Small battery light decay.Therefore, this method reduces production cost under the conditions of monocrystalline silicon quality requirement is met.
Brief description of the drawings
The accompanying drawing for forming the part of the present invention is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate to be used to explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is a kind of monocrystalline silicon crystal pulling apparatus structure schematic diagram described in the embodiment of the present invention；
Fig. 2 is argon gas as Monocrystalline silicon cell piece fragment rate of the Monocrystalline silicon cell piece and nitrogen for protecting gas as protection gas
Contrast；
Fig. 3 is argon gas as Monocrystalline silicon cell piece light decay pair of the Monocrystalline silicon cell piece and nitrogen for protecting gas as protection gas
Than；
Fig. 4 is argon gas as monocrystalline silicon production Cost comparisons of the monocrystalline silicon and nitrogen for protecting gas as protection gas.
Description of reference numerals：
1- Nitrogen source gases；2- argon gas sources of the gas；3- mass flowmenters；
4- Two In and One Out triple valves；5- bodies of heater；The pipelines of 6- first；
7- second pipes.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", " under ",
The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer " are
Based on orientation shown in the drawings or position relationship, it is for only for ease of the description present invention and simplifies description, rather than instruction or dark
Show that the device of meaning or element there must be specific orientation, with specific azimuth configuration and operation, thus it is it is not intended that right
The limitation of the present invention.In addition, term " first ", " second " etc. are only used for describing purpose, and it is not intended that instruction or hint phase
To importance or the implicit quantity for indicating indicated technical characteristic.Thus, the feature for defining " first ", " second " etc. can
To express or implicitly include one or more this feature.In the description of the invention, unless otherwise indicated, " multiple "
It is meant that two or more.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary, Ke Yishi
The connection of two element internals.For the ordinary skill in the art, above-mentioned term can be understood by concrete condition
Concrete meaning in the present invention.
Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
As shown in figure 1, a kind of monocrystalline silicon crystal pulling device, including body of heater 5, Nitrogen source gases 1 and argon gas source of the gas 2, the nitrogen
Gas source of the gas 1 is connected by the first pipeline 6 with body of heater 5, and the argon gas source of the gas 2 is connected by second pipe with body of heater 5, the present embodiment
In, the body of heater 5 is connected by Two In and One Out triple valve and the first pipeline 6 and second pipe 7；First pipeline 6 and second
Pipeline 7 is respectively equipped with mass flowmenter 3.
A kind of crystal pulling method using monocrystalline silicon crystal pulling device, keep the Nitrogen source gases pressure of monocrystalline silicon crystal pulling device
Equal with argon gas bleed pressure, the pressure is 0.5Mpa-0.7Mpa, crystal pulling process include material, steady temperature, seeding, shouldering, turn
Shoulder, isometrical, ending, the several sections of blowing out, meet：
1), material section：The primary polycrystalline of solid-state is put into quartz crucible, the primary polycrystalline of solid-state is changed into molten state by heating
It is stored in quartz crucible, the section is passed through merely the argon gas of 50slpm-120slpm flows into body of heater, and is pressed in holding furnace body
Power is 12Torr-17Torr；
2), steady temperature, seeding, shouldering, turn in each section of shoulder, continue to be passed through 50slpm-120slpm merely into body of heater and flow
The argon gas of amount, and pressure 12Torr-17Torr in holding furnace body；
3), isometrical section：
A) it is, isometrical to start to be gradually reduced closing argon gas input when isometrical 200mm of argon gas input quantity, it is being gradually reduced argon
Gas input quantity simultaneously, starts to input nitrogen into body of heater, and gradually increases nitrogen input quantity until isometrical 200mm input gases are complete
Portion is nitrogen, and now nitrogen input quantity is 50slpm-120slpm；
B), for isometrical 200mm to isometrical end, it is 50slpm-120slpm to keep nitrogen input flow rate, and in holding furnace body
Pressure 12Torr-17Torr, rate of crystalline growth are more than 84mm/hr；
In the section, it is passed through nitrogen and is reacted with monocrystalline silicon, generates silicon nitride, silicon nitride energy pinning dislocation, make nitrating
Skidding distance when dislocation in monocrystalline is heat-treated at the same temperature is respectively less than common czochralski silicon monocrystal, and nitrating silicon single crystal
Dislocation activation can be higher than conventional single, it is fast that plastic deformation ability by dislocation movement by slip discharges more conventional monocrystalline, therefore nitrating
Monocrystalline can improve silicon chip machinery, reduce silicon chip fragment rate, see Fig. 2, illustrated by Fig. 2, the nitrogen electricity manufactured using this method
Pond piece fragment rate lower than argon gas fragment rate 0.9%；In the heterogeneous forming core that oxygen can be turned into due to the N-O complexs in nitrating monocrystalline
The heart, can promote the formation of oxygen precipitation, and oxygen precipitation promotes the release of silicon self-interstitials atom, and nitrating can reduce cavity in monocrystalline silicon
Type defect area, while the increase of oxygen precipitation and the formation of N-O complexs reduce interstitial oxygen content and boron formation B-O is compound
The probability of body, and then battery light decay is reduced, see Fig. 3, nitrogen cell piece light decay reduces by 0.12% than argon gas cell piece light decay.
4) ending section：Continue to input nitrogen into stove, and ensure that nitrogen flow is 50slpm-100slpm, pressure
12Torr-17Torr；
5), blowing out section：Nitrogen is inputted into stove in blowing out 1h, and it is 50slpm-100slpm to keep nitrogen flow,
Nitrogen input is closed after blowing out 1h.
When manufacturing monocrystalline silicon by this method, because at isometrical section, protective gas is exchanged with nitrogen by argon gas, therefore, drop
Low production cost, is shown in Fig. 4, uses nitrogen crystal pulling, and production cost reduces by 1.9 yuan/kg.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (4)
- A kind of 1. monocrystalline silicon crystal pulling device, it is characterised in that：Including body of heater (5), Nitrogen source gases (1) and argon gas source of the gas (2), institute State Nitrogen source gases (1) to connect with body of heater (5) by the first pipeline (6), the argon gas source of the gas (2) passes through second pipe (7) and stove Body (5) connects, and first pipeline (6) and second pipe (7) are respectively equipped with mass flowmenter (3).
- A kind of 2. monocrystalline silicon crystal pulling device according to claim 1, it is characterised in that：The body of heater (5) is entered by two One goes out triple valve and the first pipeline (6) and second pipe (7) connection.
- 3. a kind of crystal pulling method using monocrystalline silicon crystal pulling device, including material, steady temperature, seeding, shouldering, turn shoulder, be isometrical, receipts Tail, blowing out section, it is characterised in that：Meet：1), material section：The argon gas of 50slpm-120slpm flows is passed through into body of heater, and pressure is in holding furnace body 12Torr-17Torr；2), steady temperature, seeding, shouldering, turn in each section of shoulder, continue to be passed through the argon gas of 50slpm-120slpm flows into body of heater, And pressure 12Torr-17Torr in holding furnace body；3), isometrical section：A) it is, isometrical to start to be gradually reduced closing argon gas input when isometrical 200mm of argon gas input quantity, at the same time, to body of heater Interior input nitrogen, and gradually increase nitrogen input quantity until the isometrical 200mm input all nitrogen of gas, now nitrogen input quantity For 50slpm-120slpm；B), isometrical 200mm is to isometrical end, and it is 50slpm-120slpm to keep nitrogen input flow rate, and pressure in holding furnace body 12Torr-17Torr, rate of crystalline growth are more than 84mm/hr；4) ending section：Continue to input nitrogen into stove, and ensure that nitrogen flow is 50slpm-100slpm, pressure 12Torr- 17Torr；5), blowing out section：Nitrogen is inputted into stove in blowing out 1h, and it is 50slpm-100slpm to keep nitrogen flow, blowing out Nitrogen input is closed after 1h.
- 4. the crystal pulling side according to claim 3 using monocrystalline silicon crystal pulling device, it is characterised in that：Nitrogen source gases used Pressure is equal with argon gas bleed pressure, and the pressure is 0.5Mpa-0.7Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710591130.0A CN107385507A (en) | 2017-07-19 | 2017-07-19 | A kind of method of monocrystalline silicon crystal pulling device and the application device |
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| CN201710591130.0A CN107385507A (en) | 2017-07-19 | 2017-07-19 | A kind of method of monocrystalline silicon crystal pulling device and the application device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330538A (en) * | 2018-04-13 | 2018-07-27 | 内蒙古中环光伏材料有限公司 | Disk and method are matched in a kind of nitrogen control for pulling single crystal silicon process |
| CN108411360A (en) * | 2018-04-13 | 2018-08-17 | 内蒙古中环光伏材料有限公司 | A kind of method of full nitrogen growth czochralski silicon monocrystal |
| CN108425149A (en) * | 2018-04-13 | 2018-08-21 | 内蒙古中环光伏材料有限公司 | A kind of full nitrogen silicon single crystal crystal pulling device |
| CN109576778A (en) * | 2018-12-25 | 2019-04-05 | 内蒙古中环光伏材料有限公司 | A method of reducing the impurity content that CZ method prepares monocrystalline |
| CN109695056A (en) * | 2019-01-28 | 2019-04-30 | 内蒙古中环光伏材料有限公司 | A kind of nitrogen crystal pulling pipeline and nitrating crystal-pulling technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87105811A (en) * | 1987-08-22 | 1988-02-24 | 浙江大学 | The gas phase nitrogen-doping method of czochralski silicon monocrystal |
| CN101597787A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Under nitrogen, cast the method for the controlled doped monocrystalline silicon of nitrogen concentration |
| CN102409401A (en) * | 2010-09-26 | 2012-04-11 | 江国庆 | Technology for removing impurities by utilizing nitrogen-argon mixed gas in process of growing single crystal silicon by Czochralski method |
-
2017
- 2017-07-19 CN CN201710591130.0A patent/CN107385507A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87105811A (en) * | 1987-08-22 | 1988-02-24 | 浙江大学 | The gas phase nitrogen-doping method of czochralski silicon monocrystal |
| CN101597787A (en) * | 2009-06-24 | 2009-12-09 | 浙江大学 | Under nitrogen, cast the method for the controlled doped monocrystalline silicon of nitrogen concentration |
| CN102409401A (en) * | 2010-09-26 | 2012-04-11 | 江国庆 | Technology for removing impurities by utilizing nitrogen-argon mixed gas in process of growing single crystal silicon by Czochralski method |
Non-Patent Citations (1)
| Title |
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| "《机械工程概论》" * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108330538A (en) * | 2018-04-13 | 2018-07-27 | 内蒙古中环光伏材料有限公司 | Disk and method are matched in a kind of nitrogen control for pulling single crystal silicon process |
| CN108411360A (en) * | 2018-04-13 | 2018-08-17 | 内蒙古中环光伏材料有限公司 | A kind of method of full nitrogen growth czochralski silicon monocrystal |
| CN108425149A (en) * | 2018-04-13 | 2018-08-21 | 内蒙古中环光伏材料有限公司 | A kind of full nitrogen silicon single crystal crystal pulling device |
| CN109576778A (en) * | 2018-12-25 | 2019-04-05 | 内蒙古中环光伏材料有限公司 | A method of reducing the impurity content that CZ method prepares monocrystalline |
| CN109695056A (en) * | 2019-01-28 | 2019-04-30 | 内蒙古中环光伏材料有限公司 | A kind of nitrogen crystal pulling pipeline and nitrating crystal-pulling technique |
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Application publication date: 20171124 |