CN1083874A - The heat treating method of nitrogenous czochralski silicon monocrystal - Google Patents

The heat treating method of nitrogenous czochralski silicon monocrystal Download PDF

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CN1083874A
CN1083874A CN 93112445 CN93112445A CN1083874A CN 1083874 A CN1083874 A CN 1083874A CN 93112445 CN93112445 CN 93112445 CN 93112445 A CN93112445 A CN 93112445A CN 1083874 A CN1083874 A CN 1083874A
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nitrogenous
silicon
heat treating
silicon monocrystal
treating method
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CN1029694C (en
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杨德仁
杨建松
李立本
姚鸿年
阙端磷
张锦心
樊瑞新
张奚文
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

A kind of heat treating method of nitrogenous czochralski silicon monocrystal is characterized in that under nitrogen atmosphere, handles through 850 ℃~1150 ℃ The high temperature anneal and 650 ℃ of medium annealings respectively.By the nitrogenous czochralski silicon monocrystal after this thermal treatment, could eliminate effectively that the additional alms giver of nitrogen content and oxygen level disturbs in the silicon, just be convenient to resistivity measurement and semiconducter device manufacturing.

Description

The heat treating method of nitrogenous czochralski silicon monocrystal
The present invention relates to a kind of aftertreatment technology of silicon single-crystal.
In the czochralski silicon monocrystal growth technique, the oxygen in the quartz crucible fuses into crystal, and oxygen level is up to 10 in the silicon single-crystal 17/ cm 3~10 18/ cm 3, this primary silicon single-crystal has produced the additional heat alms giver in 350 ℃~550 ℃ heat-processedes, P type single crystal silicon resistivity is risen, and n type single crystal silicon resistivity descends.Relevant this hot alms giver's phenomenon that contains the oxygen silicon single-crystal is in nineteen fifty-seven C.S.F ü ller, R.A.Logan[J.Appl, Phy, 28,1429(1957)] and W.Kaizer[Phys Rev, 105,1751(1957)] made report.
Long-term next, people place primary silicon single-crystal stove to carry out medium annealing in production practice and handle, and refer to be heated to 650 ℃ under nitrogen atmosphere, are incubated 0.5~1 hour, are quickly cooled to normal temperature thereafter.Handle by medium annealing, can eliminate and contain the hot alms giver of oxygen silicon single-crystal and disturb, make monocrystalline resistivity true, to be used in the monocrystalline test and to make semiconducter device.
The method that CN85100295,86100854,87105811,88100307,88102558, serial Chinese patents such as 89105564 adopt nitrogen to make czochralski silicon monocrystal as protective atmosphere has many superiority; widely apply aborning; the silicon single-crystal of being produced is all the nitrogenous oxygen silicon single-crystal that contains; be designated hereinafter simply as nitrogenous czochralski silicon monocrystal, and the czochralski silicon monocrystal of growing is called and contains the oxygen czochralski silicon monocrystal under argon atmosphere.Use existing medium annealing treatment process and be and to eliminate additional alms giver's interference problem that nitrogenous czochralski silicon monocrystal exists.
The heat treating method that the purpose of this invention is to provide a kind of nitrogenous czochralski silicon monocrystal of making under nitrogen atmosphere is eliminated additional alms giver effectively and is disturbed, for the test and the application of monocrystalline brings convenience.
Nitrogenous czochralski silicon monocrystal product is that Chinese patent 85100295 is announced the back appearance in February, 1986, adopts nitrogen atmosphere in single crystal growth process, comes down to a kind of nitrogenous oxygen silicon single-crystal that contains, and nitrogen content is 1 * 10 in the silicon 14/ cm 3~9 * 10 15/ cm 3, oxygen level is 5 * 10 17/ cm 3~2 * 10 18/ cm 3, additional alms giver's interference problem of oxygen adopts 650 ℃ of traditional process annealings to handle and achieves a solution.The additional alms giver's interference problem that solves nitrogen content is of equal importance, the behavior of nitrogen in silicon is more more complicated than oxygen, by deep research and a large amount of experiments think in nitrogen atmosphere, grow contain the oxygen czochralski silicon monocrystal, owing to introduced the nitrogen element, in crystal growth and process of cooling and oxygen element have electroactive equally in conjunction with forming new oxygen-nitrogen complex body.Therefore, adopt conventional medium annealing to handle, still can not eliminate the additional alms giver who produces by nitrogen, oxygen.Must handle the heat treating method that combines by The high temperature anneal and medium annealing, the additional alms giver that could eliminate nitrogen and oxygen disturbs.This heat treating method is different from following silicon single-crystal heat treatment technics:
A, silicon single-crystal are ion implantation back for recovering lattice and reducing the thermal treatment that defective is carried out;
B, the thermal treatment of silicon single-crystal after the high energy particle radiation;
C, silicon single-crystal are for forming processing place that clean area carries out;
The thermal treatment that D, the hot alms giver of silicon single-crystal, new alms giver produce and eliminate.
The heat treating method of nitrogenous czochralski silicon monocrystal of the present invention comprises that nitrogen content is 5 * 10 in the silicon 14/ cm 3~9 * 10 15/ cm 3, nitrogen content is 5 * 10 in the silicon 17/ cm 3~2 * 10 18/ cm 3, comprise that also this monocrystalline is heated to 650 ℃, insulation 0.5~1 hour under nitrogen atmosphere, the medium annealing that is quickly cooled to normal temperature is handled.The invention is characterized in: adopt The high temperature anneal and medium annealing to handle the heat treating method that combines, its processing step is:
A, under nitrogen atmosphere, be heated to 850 ℃~1150 ℃, be incubated 0.5~3 hour, slowly cool to normal temperature;
B, thereafter is heated to 650 ℃ under nitrogen atmosphere, be incubated 0.5~1 hour, is quickly cooled to normal temperature.
Above-mentioned The high temperature anneal, its best Heating temperature are 900 ℃~1000 ℃.
With prior art relatively, advantage of the present invention is that the nitrogen, the oxygen that successively adopt the anneal of the high temperature of 850 ℃~1050 ℃ and 650 ℃ and middle temperature can eliminate in the nitrogenous czochralski silicon monocrystal add alms giver's interference problem, the resistivity that measure this moment is only really, is convenient to the monocrystalline test and makes semiconducter device; And adopt existing heat treating method, then can't solve additional alms giver's interference problem of nitrogenous czochralski silicon monocrystal.
Accompanying drawing 1 is the thermal treatment process synoptic diagram of nitrogenous czochralski silicon monocrystal, and G is a The high temperature anneal among the figure, and Z is that medium annealing is handled, and the ordinate zou of figure is a temperature, and X-coordinate is hour.
Embodiment 1:
Nitrogenous czochralski silicon monocrystal, nitrogen content is 5 * 10 in the silicon 14/ cm 3, oxygen level is 5 * 10 17/ cm 3, being heated to 850 ℃, insulation is 3 hours under nitrogen atmosphere, and slow cooling is to normal temperature; Insulation 1 hour under 650 ℃ and nitrogen atmosphere more then is quickly cooled to normal temperature.
Embodiment 2:
Nitrogenous czochralski silicon monocrystal, nitrogen content is 9 * 10 in the silicon 15/ cm 3, oxygen level is 2 * 10 18/ cm 3, being heated to 900 ℃, insulation is 1 hour under nitrogen atmosphere, and slow cooling is to normal temperature; Insulation 1 hour under 650 ℃ and nitrogen atmosphere more then is quickly cooled to normal temperature.
Embodiment 3:
With the nitrogenous czochralski silicon monocrystal of embodiment 1 or 2 usefulness, high temperature anneal temperature is 950 ℃, is incubated 1 hour, and its protective atmosphere is identical with embodiment 1 or 2 with medium Temperature Annealing.
Embodiment 4:
Nitrogenous czochralski silicon monocrystal, high temperature anneal temperature are 1000 ℃, are incubated 1 hour, and all the other conditions are identical with embodiment 3.
Embodiment 5:
Nitrogenous czochralski silicon monocrystal, high temperature anneal temperature are 1050 ℃, are incubated 0.5 hour, and all the other conditions are identical with embodiment 3.
Embodiment 6:
Nitrogenous czochralski silicon monocrystal, high temperature anneal temperature are 1150 ℃, are incubated 0.5 hour, and all the other conditions are identical with embodiment 3.

Claims (2)

1, a kind of heat treating method of nitrogenous czochralski silicon monocrystal comprises that nitrogen content is 5 * 10 in the silicon 14/ cm 3~9 * 10 15/ cm 3, oxygen level is 5 * 10 in the silicon 17/ cm 3~2 * 10 18/ cm 3Also comprise be heated to 650 ℃, under nitrogen atmosphere, be incubated 0.5~1 hour, the medium annealing that is quickly cooled to normal temperature handles; the invention is characterized in: adopt The high temperature anneal and medium annealing to handle the heat treating method that combines, its processing step is:
A, under nitrogen atmosphere, be heated to 850 ℃~1150 ℃, be incubated 0.5~3 hour, slowly cool to normal temperature;
B, thereafter is heated to 650 ℃ under nitrogen atmosphere, be incubated 0.5~1 hour, is quickly cooled to normal temperature.
2, according to the method for claim 1, it is characterized in that: described The high temperature anneal, its optimum heating temperature are 900 ℃~1000 ℃.
CN 93112445 1993-05-22 1993-05-22 Heat treating method of straightly pulled monocrystalline silicon in nitrogen-containing atmosphere Expired - Fee Related CN1029694C (en)

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CN 93112445 CN1029694C (en) 1993-05-22 1993-05-22 Heat treating method of straightly pulled monocrystalline silicon in nitrogen-containing atmosphere

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CN1029694C CN1029694C (en) 1995-09-06

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110074C (en) * 1995-07-10 2003-05-28 罗姆股份有限公司 Method of manufacturing semiconductor device
CN100338270C (en) * 2004-11-05 2007-09-19 北京有色金属研究总院 Monocrystalline silicon buffing sheet heat treatment process
CN102995125A (en) * 2012-10-12 2013-03-27 孙新利 Heat treatment process of semiconductor silicon wafer
CN113417010A (en) * 2021-08-23 2021-09-21 杭州盾源聚芯半导体科技有限公司 High-cleanliness annealing method for polycrystalline silicon rod material
CN115369486A (en) * 2022-10-26 2022-11-22 新美光(苏州)半导体科技有限公司 Method for solving problem of false height of resistance and inversion of conductivity type of abnormal silicon rod

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110074C (en) * 1995-07-10 2003-05-28 罗姆股份有限公司 Method of manufacturing semiconductor device
CN100338270C (en) * 2004-11-05 2007-09-19 北京有色金属研究总院 Monocrystalline silicon buffing sheet heat treatment process
CN102995125A (en) * 2012-10-12 2013-03-27 孙新利 Heat treatment process of semiconductor silicon wafer
CN102995125B (en) * 2012-10-12 2015-06-24 浙江中晶科技股份有限公司 Heat treatment process of semiconductor silicon wafer
CN113417010A (en) * 2021-08-23 2021-09-21 杭州盾源聚芯半导体科技有限公司 High-cleanliness annealing method for polycrystalline silicon rod material
CN115369486A (en) * 2022-10-26 2022-11-22 新美光(苏州)半导体科技有限公司 Method for solving problem of false height of resistance and inversion of conductivity type of abnormal silicon rod

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