CN107604430A - Low oxygen content monocrystalline silicon growing method - Google Patents
Low oxygen content monocrystalline silicon growing method Download PDFInfo
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- CN107604430A CN107604430A CN201610536308.7A CN201610536308A CN107604430A CN 107604430 A CN107604430 A CN 107604430A CN 201610536308 A CN201610536308 A CN 201610536308A CN 107604430 A CN107604430 A CN 107604430A
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Abstract
The present invention provides a kind of growing method of low oxygen content monocrystalline silicon, before crystal pulling starts, by the control of carbon heater thermal field center below silicon melt surface；With the growth of crystal, carbon heater thermal field center gradually rises relative to silicon melt surface, in the process, gradually reduces the distance of heat shielding bottom and silicon melt surface, i.e., in silicon single-crystal pullup growth course, controls the relativeness of following two distances：Vertical range between carbon heater thermal field center and silicon melt surface, it is looped around the distance between heat shielding bottom and silicon melt surface around crystal bar.It can be in using the oxygen content of the silicon single crystal bar head of the technology of the present invention growth, middle part and afterbody in the range of same level, meet the requirement of large scale integrated circuit substrate.
Description
Technical field
The present invention relates to a kind of growing technology of low oxygen content monocrystalline silicon, the more particularly to heater center in vertical pulling method monocrystalline silicon growing technique and heat shielding bottom control technology, low oxygen content monocrystalline silicon is prepared.
Background technology
In the manufacturing process of monocrystalline silicon, most-often used is vertical pulling method（Czochralski, abridge CZ）, in vertical pulling method, polysilicon is to be filled in quartz glass crucibles（Also referred to as silica crucible）In, then heat melting and form melted silicon, immersed in melted silicon after seed crystal to upper rotary pulling, silicon is in seed crystal and the interface solidification and crystallization of liquation, formation monocrystal silicon.
Oxygen plays a part of two aspects in crystal, is beneficial aspect first, improving the mechanical strength of silicon wafer；Second, having done a kind of impurities phase causes point defect and dislocation defects etc., it is harmful aspect.At present, discovery can carry out intrinsic gettering using oxygen, and one layer of flawless perfect crystal is prepared on the surface of chip.But carry out intrinsic gettering using oxygen, it is high with technical process correlation, it is desirable to by Control for Oxygen Content at one it is very narrow within the scope of, therefore Control for Oxygen Content turns into one of governing factor important in silicon monocrystal growth.Under normal circumstances, the oxygen content on silicon single crystal head is high and afterbody oxygen content is low, the reason for this is possible is the growth with crystal, the contact area of silica crucible and silicon melt gradually decreases, body of heater periphery thermal environment changes and silicon melt flowing change, three cause the amount of oxygen element into melt to change.In order to suppress the fluctuation of oxygen content, control oxygen content suggested a variety of methods in an average level, patent JPH01160892, JPH0570279 and CN1932085 all the time.One of them most important method is to control silicon melt surface and the distance of heat shielding bottom.
As the design principle of great scale integrated circuit, due to the temperature of preparation technology to be reduced, it requires that the oxygen content in crystal is relatively low.It is generally acknowledged that the distance between silicon melt and heat shielding are more narrow more can reduce oxygen content, because can so accelerate the argon gas flowing velocity of silicon melt surface, so as to promote SiO gases to be evaporated from melt.But according to patent JPH01160892, the reduction of this distance sometimes instead results in the increase of oxygen content.
The reason for we have studied this contradiction is produced, it is due to caused by two fluctuations apart from height to find this.First, bath surface and the distance of heat shielding bottom, another is used to heat the distance between thermal field center and bath surface of silicon melt carbon heater.
Normal conditions, the position of heater are preferentially arranged to below silicon melt surface, because relatively low heating location improves silicon melt flow stability, also not high simultaneously for the technical requirements of pulling operation, crystal pulling technique is easier to operate.If the position of heater center is higher than bath surface, although relatively low oxygen content can be obtained by generally saying, such silicon melt mobility potentially unstable, it can cause occur a large amount of dislocations in crystal, so as to cause Crystallization polycrystalline.Therefore most of manufacturer the less oxygen content considered in crystal of meeting, is more likely to use relatively low heater locations relative to considering polycrystalline problem occur.And the technology of the present invention overcomes this defect.
The content of the invention
It is an object of the invention to provide a kind of growing method of low oxygen content monocrystalline silicon, the head of monocrystal rod is set to be in the oxygen content of afterbody in the range of same level.
In order to reach the above object, the present invention provides a kind of growing method of low oxygen content monocrystalline silicon：Specific steps include：Before crystal pulling starts, by the control of carbon heater thermal field center below silicon melt surface；With the growth of crystal, carbon heater thermal field center gradually rises relative to silicon melt surface, in the process, gradually reduces the distance of heat shielding bottom and silicon melt surface, i.e., in silicon single-crystal pullup growth course, controls the relativeness of following two distances：Vertical range between carbon heater thermal field center and silicon melt surface, it is looped around the distance between heat shielding bottom and silicon melt surface around crystal bar.
Preferably, when the vertical range between carbon heater thermal field center and silicon melt surface is in -10mm to -30mm, i.e. carbon heater thermal field center below silicon melt surface within 10mm-30mm scopes when, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 40mm, in the range of 60mm.Now carbon heater thermal field center is less than bath surface, and melt flows are stable, and operation difficulty is small, and oxygen content is suitable with conventional method.
Preferably, when the vertical range between carbon heater thermal field center and silicon melt surface is ± 10mm, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 30mm, in the range of 50mm.With the growth of crystal, melt amount in crucible reduces, approached when carbon heater thermal field center with silicon melt surface, therefore the oxygen in silica crucible enters the amount of melt and there is also change for high concentration position, the research of the present invention shows, the appropriate distance for reducing heat shielding bottom and bath surface can keep the oxygen in silicon single crystal be in monocrystalline club head similar in concentration.
Preferably, when the vertical range between carbon heater thermal field center and silicon melt surface is in 10mm to 50mm, i.e. carbon heater thermal field center is when within silicon melt surface above 10mm-50mm scopes, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 5mm, in the range of 30mm.
With the further growth of crystal, carbon heater thermal field center is risen on silicon melt surface, now the mobility unstability increase of melt, and the temperature on silica crucible top is high, and the temperature of melt portion is relatively low.The stabilization of silicon melt temperature and mobility can be kept by further reducing the distance of heat shielding bottom and bath surface, keep the oxygen in silicon single crystal be in monocrystalline club head similar in concentration.
Brief description of the drawings
Fig. 1 is shown as in the vertical pulling method monocrystalline silicon growing technique that is provided in the embodiment of the present invention distance structure schematic diagram between silicon single crystal bar, heat shielding, carbon heater, heat shielding bottom, thermal field center and silicon melt surface.
Component label instructions；
1 silicon single crystal bar,
2 heat shieldings,
3 carbon heaters,
4 heat shielding bottoms,
5 silicon melt surfaces,
6 thermal field centers.
Embodiment
Polysilicon block is fitted into silica crucible, is put into single crystal growing furnace, heating fusing is carried out after vacuumizing.See whether to hang side phenomenon, after polysilicon all melts, static more than 3h.
Then the position of silica crucible is adjusted, makes vertical range between carbon heater thermal field center 6 and silicon melt surface 5 in -10mm to -30mm, the distance between heat shielding bottom 4 and silicon melt surface 5 are more than 40mm, in the range of 60mm, preferably in 50-60mm.Then seeding, shouldering are proceeded by, turns shoulder and isodiametric growth process.The vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is observed simultaneously.With the growth of crystal, silicon melt surface 5 declines, when the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is ± 10mm, control is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5 more than 30mm, in the range of 50mm.With the growth of crystal, silicon melt surface 5 further declines, when the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is in 10mm to 50mm, i.e. carbon heater thermal field center 6 is when within the 10mm-50mm scopes of silicon melt surface more than 5, control is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5 more than 5mm, in the range of 30mm.Head and the qualified silicon single crystal bar 1 of afterbody oxygen concentration distribution can be obtained.
Embodiment 1
Using the method for the above, 8 inches of silicon single crystal are grown.After silicon melt is stable, the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is adjusted and arrives -30mm by seeding before starting, and the distance between heat shielding bottom 4 and silicon melt surface 5 are adjusted to 50mm.Then start seeding, shouldering, turn shoulder and isodiametric growth process.The vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is observed simultaneously.With the growth of crystal, silicon melt surface 5 declines, and when the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 0mm, it is 40mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.When the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 30mm, it is 20mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.The oxygen content for detecting silicon single crystal head, middle part and afterbody is respectively 7.5ppm, 7.2ppm and 6.9ppm, and the variable quantity of oxygen content is：8%.
Comparative example 1
Using the method for embodiment 1, the vertical range between fixed carbon heater thermal field center 6 and silicon melt surface 5 is -30mm, and the distance between heat shielding bottom 4 and silicon melt surface 5 are 20mm.The oxygen content that silicon single crystal head, middle part and afterbody are detected after crystal growth is respectively 8.9ppm, 7.9ppm and 6.9ppm, and the variable quantity of oxygen content is：29%.
Embodiment 2
Using the method for the above, 8 inches of silicon single crystal are grown.After silicon melt is stable, the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is adjusted and arrives -10mm by seeding before starting, and the distance between heat shielding bottom 4 and silicon melt surface 5 are adjusted to 40mm.Then start seeding, shouldering, turn shoulder and isodiametric growth process.The vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is observed simultaneously.With the growth of crystal, silicon melt surface 5 declines, and when the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 10mm, it is 30mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.When the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 40mm, it is 10mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.The oxygen content for detecting silicon single crystal head, middle part and afterbody is respectively 7.3ppm, 6.9ppm and 6.6ppm, and the variable quantity of oxygen content is：10.6%.
Comparative example 2
Using the method for embodiment 1, the vertical range between fixed carbon heater thermal field center 6 and silicon melt surface 5 is 0mm, and the distance between heat shielding bottom 4 and silicon melt surface 5 are 40mm.The oxygen content that silicon single crystal head, middle part and afterbody are detected after crystal growth is respectively 8.5ppm, 7.2ppm and 7.9ppm, and the variable quantity of oxygen content is：18%.
Embodiment 3
Using the method for the above, 8 inches of silicon single crystal are grown.After silicon melt is stable, the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is adjusted and arrives 0mm by seeding before starting, and the distance between heat shielding bottom 4 and silicon melt surface 5 are adjusted to 40mm.Then start seeding, shouldering, turn shoulder and isodiametric growth process.The vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is observed simultaneously.With the growth of crystal, silicon melt surface declines, and when the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 10mm, it is 30mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.When the vertical range between carbon heater thermal field center 6 and silicon melt surface 5 is 40mm, it is 5mm that control, which is looped around the distance between the surrounding heat shielding bottom 4 of crystal bar 1 and silicon melt surface 5,.The oxygen content for detecting silicon single crystal head, middle part and afterbody is respectively 7.0ppm, 6.5ppm and 6.6ppm, and the variable quantity of oxygen content is：10.6%.
Comparative example 3
Using the method for embodiment 1, the vertical range between fixed carbon heater thermal field center 6 and silicon melt surface 5 is 0mm, and the distance between heat shielding bottom 4 and silicon melt surface 5 are 40mm.The oxygen content that silicon single crystal head, middle part and afterbody are detected after crystal growth is respectively 8.5ppm, 7.2ppm and 6.3ppm, and the variable quantity of oxygen content is：19%.
Claims (4)
1. a kind of growing method of low oxygen content monocrystalline silicon, it is characterised in that specific steps include：Before crystal pulling starts, by the control of carbon heater thermal field center below silicon melt surface；With the growth of crystal, carbon heater thermal field center gradually rises relative to silicon melt surface, in the process, gradually reduces the distance of heat shielding bottom and silicon melt surface, i.e., in silicon single-crystal pullup growth course, controls the relativeness of following two distances：Vertical range between carbon heater thermal field center and silicon melt surface, it is looped around the distance between heat shielding bottom and silicon melt surface around crystal bar.
2. the growing method of low oxygen content monocrystalline silicon as claimed in claim 1, it is characterized in that, when the vertical range between carbon heater thermal field center and silicon melt surface is in -10mm to -30mm, i.e. carbon heater thermal field center below silicon melt surface within 10mm-30mm scopes when, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 40mm, in the range of 60mm.
3. the growing method of low oxygen content monocrystalline silicon as claimed in claim 1, it is characterized in that, when the vertical range between carbon heater thermal field center and silicon melt surface is ± 10mm, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 30mm, in the range of 50mm.
4. the growing method of low oxygen content monocrystalline silicon as claimed in claim 1, it is characterized in that, when the vertical range between carbon heater thermal field center and silicon melt surface is in 10mm to 50mm, i.e. carbon heater thermal field center is when within silicon melt surface above 10mm-50mm scopes, control is looped around around crystal bar the distance between heat shielding bottom and silicon melt surface more than 5mm, in the range of 30mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107268080A (en) * | 2017-07-06 | 2017-10-20 | 锦州神工半导体有限公司 | A kind of pulling growth method of the unparalleled crest line monocrystalline silicon of major diameter |
| CN110923810A (en) * | 2019-12-11 | 2020-03-27 | 包头美科硅能源有限公司 | Device and process for regulating and controlling liquid level position in equal-diameter growth process of large-size monocrystalline silicon |
| CN113529163A (en) * | 2020-04-17 | 2021-10-22 | 隆基绿能科技股份有限公司 | Crystal pulling method |
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| JPH01160892A (en) * | 1987-12-16 | 1989-06-23 | Mitsubishi Metal Corp | Method for controlling oxygen concentration in silicon single crystal |
| CN1034400A (en) * | 1987-12-08 | 1989-08-02 | 日本钢管株式会社 | The manufacture method of silicon single crystal and equipment |
| JPH0570279A (en) * | 1991-09-17 | 1993-03-23 | Nippon Steel Corp | Production of silicon single crystal |
| JP3085568B2 (en) * | 1993-11-01 | 2000-09-11 | コマツ電子金属株式会社 | Apparatus and method for producing silicon single crystal |
| CN1932085A (en) * | 2005-06-15 | 2007-03-21 | 硅电子股份公司 | Production process of silicon single crystal |
| CN101435105A (en) * | 2008-12-01 | 2009-05-20 | 浙江碧晶科技有限公司 | Method for preparing low oxygen content silicon crystal |
| CN101922040A (en) * | 2009-06-10 | 2010-12-22 | 江国庆 | Device of oxygen control growth in single crystal furnace |
| CN102011181A (en) * | 2010-12-24 | 2011-04-13 | 温州神硅电子有限公司 | Thermal field device for growing 8-inch silicon single crystals for solar energy by Czochralski method |
| CN104818524A (en) * | 2015-04-28 | 2015-08-05 | 汤灏 | Method and heater for improving quality of monocrystal silicon grown by Czochralski method |
| CN105506731A (en) * | 2015-12-09 | 2016-04-20 | 上海超硅半导体有限公司 | Monocrystalline silicon growth oxygen content control technology |
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2016
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Patent Citations (10)
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| CN1034400A (en) * | 1987-12-08 | 1989-08-02 | 日本钢管株式会社 | The manufacture method of silicon single crystal and equipment |
| JPH01160892A (en) * | 1987-12-16 | 1989-06-23 | Mitsubishi Metal Corp | Method for controlling oxygen concentration in silicon single crystal |
| JPH0570279A (en) * | 1991-09-17 | 1993-03-23 | Nippon Steel Corp | Production of silicon single crystal |
| JP3085568B2 (en) * | 1993-11-01 | 2000-09-11 | コマツ電子金属株式会社 | Apparatus and method for producing silicon single crystal |
| CN1932085A (en) * | 2005-06-15 | 2007-03-21 | 硅电子股份公司 | Production process of silicon single crystal |
| CN101435105A (en) * | 2008-12-01 | 2009-05-20 | 浙江碧晶科技有限公司 | Method for preparing low oxygen content silicon crystal |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107268080A (en) * | 2017-07-06 | 2017-10-20 | 锦州神工半导体有限公司 | A kind of pulling growth method of the unparalleled crest line monocrystalline silicon of major diameter |
| CN107268080B (en) * | 2017-07-06 | 2019-08-02 | 锦州神工半导体股份有限公司 | A kind of pulling growth method of the major diameter without double ridge monocrystalline silicon |
| CN110923810A (en) * | 2019-12-11 | 2020-03-27 | 包头美科硅能源有限公司 | Device and process for regulating and controlling liquid level position in equal-diameter growth process of large-size monocrystalline silicon |
| CN113529163A (en) * | 2020-04-17 | 2021-10-22 | 隆基绿能科技股份有限公司 | Crystal pulling method |
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Application publication date: 20180119 |