CN85100295B - Direct drawing of monocrystalline sillicon with nitrogen blanketing - Google Patents

Direct drawing of monocrystalline sillicon with nitrogen blanketing Download PDF

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Publication number
CN85100295B
CN85100295B CN85100295A CN85100295A CN85100295B CN 85100295 B CN85100295 B CN 85100295B CN 85100295 A CN85100295 A CN 85100295A CN 85100295 A CN85100295 A CN 85100295A CN 85100295 B CN85100295 B CN 85100295B
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China
Prior art keywords
nitrogen
silicon single
silicon
crystal
czochralski
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Expired
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CN85100295A
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Chinese (zh)
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CN85100295A (en
Inventor
阙端麟
李立本
林玉瓶
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN85100295A priority Critical patent/CN85100295B/en
Publication of CN85100295A publication Critical patent/CN85100295A/en
Publication of CN85100295B publication Critical patent/CN85100295B/en
Expired legal-status Critical Current

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Abstract

The present invention relates to a nitrogen atmosphere for pulling a silicon single crystal, which belongs to the manufacturing technology of semiconductor material. Nitrogen serves as protective gas of a crystal pulling method in a silicon single crystal pulling (Czochralski method) technology, the purity of the nitrogen is above 99.999%, the flow rate of the nitrogen flowing in a silicon single crystal furnace is from 2 to 50 l/min, and nitrogen pressure in the furnace is from 0.5 to 60 torr. Because a nitrogen source is rich and price is low, the present invention can greatly reduce the cost of silicon single crystals, and generates positive effects.

Description

Adopt nitrogen atmosphere to make the method for vertical pulling (czochralski therapy) silicon single-crystal
The present invention is a kind of method about vertical pulling (czochralski therapy) silicon single-crystal.
The method of the most frequently used growing semiconductor grade silicon has czochralski therapy (CZ) and floating zone melting (FZ), and wherein the occupancy volume of the silicon single-crystal of czochralski therapy growth is about about 90% of total amount.
In czochralski therapy silicon monocrystal growth process, molten silicon and quartz crucible reaction (Si+SiO 2→ 2SiO ↑) upwards evaporation and influence the normal growth of silicon single-crystal of the SiO that generates, when making large diameter silicon monocrystal, it drew for up to 10 hours, make this problem particularly outstanding, no matter under vacuum or normal pressure argon atmospher, can't avoid all that silicon oxide particle falls into molten silicon face and destroys the stability that monocrystalline continues growth in the crystal pulling process.U.S. Varian company had reported large-scale silicon single-crystal drawing process (the Solid State Technology1975 VOL under a kind of argon filling condition that reduces pressure in 1975.18.31~33), with CO and the SiO gas that constantly produces in the silicon single crystal pulling process, take out of outside the stove by the decompression argon that top in stove enters, eliminated the interference of SiO, reduce the carbon content in the silicon, thereby improved the yield rate of czochralski therapy dislocation-free monocrystalline silicon, and improved quality product.
The weak point of above-mentioned decompression argon filling Qie Shi crystal pulling method is: bottled argon gas is easily polluted by impurity, and purity is difficult to guarantee; If use liquid argon, then need produce with the ultra-large type air device, cost an arm and a leg.
Task of the present invention is to seek originates the gas abundant, that price is cheaper as the protection gas that draws high quality silicon single crystal.
Nineteen fifty-nine, WKaiser (seeing JAppl phys 30.427(1959)) points out, the reaction grown silicon nitride of nitrogen and molten silicon liquid is disturbed crystal growth, and in floating zone melting (FZ) single crystal growing, fill the nitrogen test, prove under normal pressure because of silicon and the impossible growing silicon single crystal of nitrogen generation chemical reaction.So far in the czochralski silicon monocrystal technology, still do not have and adopt the precedent of purity nitrogen as the shielding gas of making czochralski silicon monocrystal.
The present invention in experimental study in depth the actual conditions of nitrogen and chemistry of silicones reaction; and on the basis of the fractional condensation state of nitrogen in silicon; having overcome long-standing pure nitrogen gas can not propose with the method for nitrogen as the manufacturing czochralski silicon monocrystal of protective atmosphere as the technology prejudice of crystal pulling shielding gas.
Adopt the purity nitrogen protective atmosphere need control pressure and the flow that enters furnace gas.The airing system that the present invention has adopted liquid nitrogen storage, vaporizer, static organ, pressure-regulator to form; The adjusting measuring system of the pressure flow that mass flowmeter, precision resistance vacuumometer, corrugated stainless steel tubing valve are formed; The air-bleed system that stopping valve, strainer, sliding valve vacuum pump are formed.Constitute the decompression and the flow control system of pure nitrogen gas protective atmosphere, suppressed the interference of SiO effectively, created the condition of silicon crystal normal growth under reduced atmosphere.The technical parameter of control is as follows:
Nitrogen gas purity is more than 99.999%
0.5~60 holder of nitrogen pressure in furnace scope, 2~50 liters/minute of nitrogen flows.
Under the nitrogen protection atmospheric condition of above-mentioned relative broad range, can both with adopt the argon atmosphere dislocation-free monocrystalline silicon of similarly growing, quality product meets the requirement of making semiconducter device.
The present invention and existing argon filling (Ar) decompression czochralski therapy technology is compared, and it is abundant to have a nitrogen source, cheap (at present the nitrogen price be about argon gas 1/3), under silicon single-crystal condition identical in quality, can reduce the silicon single-crystal cost significantly.And make no argon gas area can use present technique to draw high-quality silicon single-crystal.
Embodiment:
Adopt nitrogen protection atmosphere to make the method for czochralski silicon monocrystal, used nitrogen gas purity is more than 99.999%, and control silicon single-crystal furnace inner nitrogen pressure is 10~30 holders, and nitrogen flow is 10~30 liters/minute.Used inflation extraction equipment and control method are identical with argon filling technology.The silicon single-crystal quality that is drawn into satisfies the requirement of making silicon semiconductor device.

Claims (3)

1, a kind of manufacture method that has vertical pulling (czochralski therapy) silicon single-crystal of the gas-filled protective that reduces pressure is characterized in that adopting purity nitrogen as the protective atmosphere that draws silicon single-crystal.
2, according to the manufacture method of the described czochralski silicon monocrystal of claim 1, it is characterized in that used nitrogen gas purity is more than 99.999%, nitrogen pressure in furnace is 0.5~60 holder, nitrogen flow is 2~50 liters/minute.
3, in accordance with the method for claim 2, the optimum technology parameter that it is characterized in that it is that nitrogen pressure in furnace is 10~30 holders, and nitrogen flow is 10~30 liters/minute.
CN85100295A 1985-04-01 1985-04-01 Direct drawing of monocrystalline sillicon with nitrogen blanketing Expired CN85100295B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN85100295A CN85100295B (en) 1985-04-01 1985-04-01 Direct drawing of monocrystalline sillicon with nitrogen blanketing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN85100295A CN85100295B (en) 1985-04-01 1985-04-01 Direct drawing of monocrystalline sillicon with nitrogen blanketing

Publications (2)

Publication Number Publication Date
CN85100295A CN85100295A (en) 1986-02-10
CN85100295B true CN85100295B (en) 1986-02-10

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Application Number Title Priority Date Filing Date
CN85100295A Expired CN85100295B (en) 1985-04-01 1985-04-01 Direct drawing of monocrystalline sillicon with nitrogen blanketing

Country Status (1)

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CN (1) CN85100295B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109518269A (en) * 2017-09-20 2019-03-26 内蒙古中环光伏材料有限公司 Doped monocrystalline silicon stick and its production method

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560629A (en) * 2012-03-10 2012-07-11 天津市环欧半导体材料技术有限公司 Method for producing low-cost czochralski silicon
CN102758253A (en) * 2012-06-20 2012-10-31 合肥景坤新能源有限公司 Czochralski polycrystalline silicon or monocrystal silicon preparation technology

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109518269A (en) * 2017-09-20 2019-03-26 内蒙古中环光伏材料有限公司 Doped monocrystalline silicon stick and its production method

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CN85100295A (en) 1986-02-10

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