CN106637386A - Single crystal straight-pulling heater capable of increasing crystal pulling rate, and single crystal straight-pulling method - Google Patents

Single crystal straight-pulling heater capable of increasing crystal pulling rate, and single crystal straight-pulling method Download PDF

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Publication number
CN106637386A
CN106637386A CN201510727379.0A CN201510727379A CN106637386A CN 106637386 A CN106637386 A CN 106637386A CN 201510727379 A CN201510727379 A CN 201510727379A CN 106637386 A CN106637386 A CN 106637386A
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CN
China
Prior art keywords
pulling
heater
crystals
heating ring
heating
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Pending
Application number
CN201510727379.0A
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Chinese (zh)
Inventor
吴丹
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Longi Green Energy Technology Co Ltd
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XI'AN TONGXIN SEMICONDUCTOR ACCESSORY MATERIAL Co Ltd
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Publication date
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Priority to CN201510727379.0A priority Critical patent/CN106637386A/en
Publication of CN106637386A publication Critical patent/CN106637386A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14Heating of the melt or the crystallised materials
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Abstract

The present invention provides a single crystal straight-pulling heater capable of increasing the crystal pulling rate. The single crystal straight-pulling heater comprises connection plates and heating rings, wherein the connection plates are axially arranged along the heater main body, and a plurality of the heating rings are sequentially arranged along the axial direction of the heater main body and are connected between the connection plates. The single crystal straight-pulling method comprises: loading a material; melting the material by using the single crystal straight-pulling heater capable of increasing the crystal pulling rate to form a melt; and adjusting the power of the heater, controlling the longitudinal temperature gradient of the melt, carrying out fusion splicing, and sequentially carrying out seeding, crystal diameter achieving, rotary growth, equal diameter growing and ending so as to obtain the monocrystalline silicon. According to the present invention, the single crystal straight-pulling heater has the heating rings arranged along the axial direction of the heater at intervals and can adjust the longitudinal temperature gradient of the heating zone to tend to the uniform state; and with the single crystal straight-pulling method, by using the heater, the melt convection can be improved, the length and the cross section of the heating ring can be adjusted, and by using different heat generations of the heating rings, the longitudinal temperature gradient of the melt can be reduced so as to be adapted to different thermal fields.

Description

Improve the pulling of crystals heater and pulling of crystals method of pulling rate
Technical field
The invention belongs to single crystal silicon material preparing technical field, and in particular to a kind of raising pulling rate it is straight Crystal-pulling heater, further relates to using the pulling of crystals method of above-mentioned pulling of crystals heater.
Background technology
Vertical pulling method is also called Czochralski method, abbreviation CZ methods.The characteristics of CZ methods is will to be mounted in crucible In polysilicon material to form melt, then by seed crystal insertion bath surface carry out welding, while rotate And seed crystal is lifted, sequentially pass through seeding, shouldering, turn shoulder, isodiametric growth and epilog, pulling growth Silicon single crystal.
With the development of photovoltaic industry, industry competition is more and more fierce, reduces pulling of crystals cost and seems outstanding For important.It is to improve pulling rate that a kind of effective cost reduces method.In theory, pulling rate Vcrys Depending on crystal and the difference of melt heat flow:
Wherein, ρcrysFor crystalline density, Δ H is latent heat, λcrys、λmeltRespectively crystal and melt Thermal conductivity factor,The respectively longitudinal temperature gradient of crystallization front crystal and melt. To increase pulling rate Vcrys, the thermograde of crystallization front crystal should be increasedOr reduction melt Longitudinal temperature gradientThat is, to realize the raising of pulling rate, need to optimize thermal field Thermograde and corresponding technique.
The content of the invention
It is an object of the invention to provide a kind of pulling of crystals heater for improving pulling rate, it passes through Heater structure design improvement, realizes the raising of pulling rate.
The present invention also aims to provide a kind of pulling of crystals using aforementioned raising pulling rate and use add The pulling of crystals method of hot device.
A kind of technical scheme of the present invention is:The pulling of crystals heater of pulling rate is improved, Including heater body, it is characterised in that also including multiple connecting plates and multiple heating rings, multiple connections Along the axially arranged of heater body, multiple heating rings set successively plate along the axis direction of heater body Put, each heating ring is all connected between multiple connecting plates.
Of the invention the characteristics of, also resides in,
Connecting plate is two or more, and heating ring is two or more.
Heating number of rings amount is three or more than three, there is gap between two neighboring heating ring, gap Apart from identical or different.
The resistance value of heating ring is different, and heating ring is square-wave form.
Another kind of technical scheme of the present invention is:Pulling of crystals method, comprises the following steps:
Charging;
Using the pulling of crystals heater material of aforementioned raising pulling rate forming melt;
The power of the pulling of crystals heater for improving pulling rate is adjusted, the longitudinal temperature ladder of melt is controlled Degree, by seed crystal insertion bath surface welding is carried out, and is carried out seeding, shouldering successively, turned shoulder, isometrical life Monocrystalline silicon is obtained final product after long and ending.
Of the invention the characteristics of, also resides in,
During isodiametric growth, furnace pressure is controlled for 10-20Torr, inert gas flow 50-90slpm, earthenware Crucible rotating speed is 4-10 rev/min, and the rotating speed of seed crystal is 8-14 rev/min.
Improve the pulling of crystals heater of pulling rate, including heater body, multiple connecting plates and many Individual heating ring, along the axially arranged of heater body, multiple heating rings are along heater master for multiple connecting plates The axis direction of body sets gradually, and each heating ring is all connected between multiple connecting plates.
Connecting plate is two or more, and heating ring is two or more.
Heating number of rings amount is three or more than three, there is gap between two neighboring heating ring, gap Apart from identical or different.
The resistance value of heating ring is different, and heating ring is square-wave form.
The invention has the beneficial effects as follows:The pulling of crystals of the raising pulling rate of the present invention has with heater Along multiple heating rings that heater axially spaced-apart is arranged, thermal treatment zone longitudinal temperature gradient can be adjusted and tend to equal It is even, and heater weight is alleviated, so that carrying and easy for installation.The pulling of crystals of the present invention Method can improve melt convection using the pulling of crystals heater of aforementioned raising pulling rate;Also, The length of each heating ring can be adjusted with section according to actual conditions, using each heating of heater The difference of ring caloric value, can reduce the longitudinal temperature gradient of melt in the thermal field of different inventorysSo as to obtain the advantage for improving pulling of silicon single crystal pulling rate.
Description of the drawings
Fig. 1 is a kind of structural representation of the pulling of crystals heater of the raising pulling rate of the present invention;
Fig. 2 is another kind of structural representation of the pulling of crystals heater of the raising pulling rate of the present invention.
In figure, 1. on heat ring, 2. space, 3. lower heating ring, 4. connecting plate, 5. the first heating ring, 6. First gap, 7. second heats ring, 8. the second gap, 9. the 3rd heating ring, 10. connector.
Specific embodiment
The pulling of crystals of the raising pulling rate that the present invention is provided includes heater body with heater, also wraps Multiple connecting plates and multiple heating rings are included, multiple connecting plates are multiple along the axially arranged of heater body Heating ring sets gradually along the axis direction of heater body, and each heating ring is all connected to multiple connecting plates Between.
Connecting plate is two or more, and heating ring is two or more.
Heating number of rings amount is three or more than three, there is gap between two neighboring heating ring, gap Apart from identical or different.
The resistance value of heating ring is different.
Heating ring is square-wave form.
With reference to the accompanying drawings and detailed description the present invention is described in detail.
Embodiment 1
The pulling of crystals heater structure of the raising pulling rate of the present embodiment is as shown in figure 1, including edge Two axially arranged connecting plates 4 of heater body and set successively perpendicular to heater body axis direction The upper heating ring 1 put and lower heating ring 3, have space 2 between upper heating ring 1 and lower heating ring 3, And be all connected between two connecting plates 4.
The bottom of connecting plate 4 can have the connecting pin being connected with electrode.Upper heating ring 1 and lower heating ring 3 are square-wave form.In the present embodiment, upper heating ring 1 is identical with lower heating ring 3.That is, upper heating Ring 1 and the lower structure for heating ring 3, shape and size all same.Certainly, upper heating ring 1 and lower heating Ring 3 can also be different, and ring 1 and shape, length, sectional area of lower heating ring 3 etc. are heated in change can To heat the resistance of ring 1 and lower heating ring 3 in regulation, the heating for heating ring 1 and lower heating ring 3 is made Power is different, so as to produce different thermogrades.Meanwhile, between coordinating change to heat between ring up and down Gap size, can also play thermograde adjustment effect.
Embodiment 2
The pulling of crystals heater structure of the raising pulling rate of the present embodiment is as shown in Fig. 2 itself and reality The structure for applying example 1 is essentially identical, and difference is that the pulling of crystals of the present embodiment includes two with heater Connector 10 and three heating rings.Three heating rings are respectively the first heating ring 5, second and heat ring 7 With the 3rd heating ring 9.With the first gap 6 between the first heating heating ring 7 of ring 5 and second, second There is the second gap 8 between the heating heating ring 9 of ring 7 and the 3rd.
The present embodiment increased a heating ring and an interannular gap compared to the scheme of embodiment 1, Warming temperature gradient can be made to control finer.
Certainly, the quantity of the heating ring of the pulling of crystals heater of raising pulling rate of the invention is not Be limited to two or three, can also for four or more, corresponding interannular number of gaps is also therewith Adjustment, also the size in gap can change when using.The quantity of connecting plate is not limited to as two, may be used also Think three or more than four.
The pulling of crystals method that the present invention is provided, the method can be used to manufacture the pulling of crystals of various sizes, Originally as a example by sentencing 8 inch, the pulling of crystals method is illustrated.Specifically, the method is comprised the following steps:
The first step, charging, according to a conventional method by the process of single crystal growing furnace prepurging, installs thermal field, confirms fault-free Afterwards, be initially added into polycrystalline silicon raw material, inventory 200kg, close vacuumized after stove, hunted leak, pressure Change;
Second step, material lifts the power of aforementioned pulling of crystals heater to 85kw forming melt Left and right, holding argon flow amount is 50-90slpm, and furnace pressure is 10-20Torr, and crucible switchs to 4-9 rev/min, Melt is formed after polysilicon melting;
3rd step, using common process, adjusts the power of the pulling of crystals heater for improving pulling rate, Seeding, shouldering are carried out successively, turns shoulder and isodiametric growth, finally carry out ending and obtain final product monocrystalline silicon;Wherein, Seeding length is reached after 150mm, is carried out shouldering and is turned shoulder;During isodiametric growth, keep crystalline substance to turn 8-14 and turn / minute, crucible turns 4-10 rev/min, and argon flow amount is 50-90slpm, and furnace pressure is 10-20Torr, can be real Existing crystal growth average pull rate is 1.2mm/min.After ending, cooling completes i.e. removable stove.
The pulling of crystals method of the present invention uses the pulling of crystals heater of the raising pulling rate, and it adds The longitudinal temperature of thermal region is easy to adjustment, can improve melt convection;Using each heating ring heating of heater Amount is different, can form the longitudinal temperature gradient of optimizationSo as to improve the crystal pulling of pulling of silicon single crystal Speed.

Claims (10)

1. the pulling of crystals heater of pulling rate, including heater body are improved, it is characterised in that Also include multiple connecting plates and multiple heating rings, the plurality of connecting plate is along the axle of the heater body To setting, the plurality of heating ring sets gradually along the axis direction of the heater body, each heating Ring is all connected between the plurality of connecting plate.
2. the pulling of crystals heater of pulling rate is improved as claimed in claim 1, and its feature exists In the connecting plate is two or more, and the heating ring is two or more.
3. the pulling of crystals heater of pulling rate is improved as claimed in claim 1, and its feature exists In the heating number of rings amount is three or more than three, there is gap between two neighboring heating ring, institute The distance for stating gap is identical or different.
4. as described in any one of claim 1-3 raising pulling rate pulling of crystals heater, Characterized in that, the resistance value of the heating ring is different, the heating ring is square-wave form.
5. pulling of crystals method, it is characterised in that comprise the following steps:
Charging;
Using the pulling of crystals heater of the raising pulling rate as described in any one of claim 1-4 Expect to form melt;
The power of the pulling of crystals heater for improving pulling rate is adjusted, the longitudinal direction temperature of the melt is controlled Degree gradient, by seed crystal insertion bath surface welding is carried out, and carry out successively seeding, shouldering, turn shoulder, etc. Monocrystalline silicon is obtained final product after Diameter growth and ending.
6. pulling of crystals method as claimed in claim 5, it is characterised in that the isodiametric growth mistake Cheng Zhong, controls furnace pressure and turns for 4-10 for 10-20Torr, inert gas flow 50-90slpm, crucible rotation / minute, the rotating speed of seed crystal is 8-14 rev/min.
7. pulling of crystals method as claimed in claim 5, it is characterised in that the raising crystal pulling speed The pulling of crystals heater of degree, including heater body, multiple connecting plates and multiple heating rings, it is described , along the axially arranged of the heater body, the plurality of heating ring is along the heater for multiple connecting plates The axis direction of main body sets gradually, and each heating ring is all connected between the plurality of connecting plate.
8. pulling of crystals method as claimed in claim 7, it is characterised in that the connecting plate is two Individual or two or more, the heating ring is two or more.
9. pulling of crystals method as claimed in claim 7, it is characterised in that the heating number of rings amount For three or more than three, there is gap between two neighboring heating ring, the distance in the gap it is identical or It is different.
10. the pulling of crystals method as described in any one of claim 7-9, it is characterised in that it is described plus The resistance value of hot ring is different, and the heating ring is square-wave form.
CN201510727379.0A 2015-10-30 2015-10-30 Single crystal straight-pulling heater capable of increasing crystal pulling rate, and single crystal straight-pulling method Pending CN106637386A (en)

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460539A (en) * 2017-06-30 2017-12-12 内蒙古中环光伏材料有限公司 A kind of monocrystalline silicon production method of heater and the application heater
CN109837593A (en) * 2019-03-29 2019-06-04 徐州晶睿半导体装备科技有限公司 Heater and single crystal growing furnace with it
CN112391676A (en) * 2019-08-13 2021-02-23 新特能源股份有限公司 Single crystal furnace thermal field, control method thereof and single crystal furnace

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1107646A1 (en) * 1999-12-09 2001-06-13 Freiberger Compound Materials GmbH Heating element for smelt crucibles and arrangement of heating elements
US20020195045A1 (en) * 2001-06-26 2002-12-26 Zheng Lu Crystal puller and method for growing monocrystalline silicon ingots
WO2005095680A1 (en) * 2004-03-31 2005-10-13 Komatsu Denshi Kinzoku Kabushiki Kaisha Semiconductor single crystal manufacturing equipment and graphite crucible
CN201588005U (en) * 2009-12-29 2010-09-22 北京有色金属研究总院 Two-stage side heater in vertical gradient freeze crystal growing furnace
CN102108543A (en) * 2009-12-29 2011-06-29 北京有色金属研究总院 Multi-stage side heater in vertical gradient freezing crystal growing furnace
CN102758254A (en) * 2012-06-20 2012-10-31 合肥景坤新能源有限公司 Heating system for single crystal furnace
CN102851745A (en) * 2012-09-26 2013-01-02 南京晶升能源设备有限公司 Sectional wolfram wire mesh heater for sapphire single crystal furnace
CN202945379U (en) * 2012-09-26 2013-05-22 南京晶升能源设备有限公司 Sectional type tungsten filament net heater for sapphire single crystal furnace
CN203295656U (en) * 2013-04-28 2013-11-20 西安隆基硅材料股份有限公司 Heater for pulling of crystals
CN104451892A (en) * 2014-12-10 2015-03-25 上海汇淬光学科技有限公司 Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1107646A1 (en) * 1999-12-09 2001-06-13 Freiberger Compound Materials GmbH Heating element for smelt crucibles and arrangement of heating elements
US20020195045A1 (en) * 2001-06-26 2002-12-26 Zheng Lu Crystal puller and method for growing monocrystalline silicon ingots
WO2005095680A1 (en) * 2004-03-31 2005-10-13 Komatsu Denshi Kinzoku Kabushiki Kaisha Semiconductor single crystal manufacturing equipment and graphite crucible
CN201588005U (en) * 2009-12-29 2010-09-22 北京有色金属研究总院 Two-stage side heater in vertical gradient freeze crystal growing furnace
CN102108543A (en) * 2009-12-29 2011-06-29 北京有色金属研究总院 Multi-stage side heater in vertical gradient freezing crystal growing furnace
CN102758254A (en) * 2012-06-20 2012-10-31 合肥景坤新能源有限公司 Heating system for single crystal furnace
CN102851745A (en) * 2012-09-26 2013-01-02 南京晶升能源设备有限公司 Sectional wolfram wire mesh heater for sapphire single crystal furnace
CN202945379U (en) * 2012-09-26 2013-05-22 南京晶升能源设备有限公司 Sectional type tungsten filament net heater for sapphire single crystal furnace
CN203295656U (en) * 2013-04-28 2013-11-20 西安隆基硅材料股份有限公司 Heater for pulling of crystals
CN104451892A (en) * 2014-12-10 2015-03-25 上海汇淬光学科技有限公司 Multistage graphite heating system of sapphire crystal growth equipment and using method of multistage graphite heating system

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107460539A (en) * 2017-06-30 2017-12-12 内蒙古中环光伏材料有限公司 A kind of monocrystalline silicon production method of heater and the application heater
CN109837593A (en) * 2019-03-29 2019-06-04 徐州晶睿半导体装备科技有限公司 Heater and single crystal growing furnace with it
CN112391676A (en) * 2019-08-13 2021-02-23 新特能源股份有限公司 Single crystal furnace thermal field, control method thereof and single crystal furnace

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Effective date of registration: 20200213

Address after: 710100 No. 388, middle route, Xi'an, Shaanxi, Changan District

Applicant after: Longji green energy Polytron Technologies Inc

Address before: 710300 Shaanxi city of Xi'an province Huxian Fengjing Industrial Park Lake Waterfront Road No. 3

Applicant before: Xi'an Tongxin Semiconductor Accessory Material Co., Ltd.

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