CN1029694C - Heat treating method of straightly pulled monocrystalline silicon in nitrogen-containing atmosphere - Google Patents
Heat treating method of straightly pulled monocrystalline silicon in nitrogen-containing atmosphere Download PDFInfo
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- CN1029694C CN1029694C CN 93112445 CN93112445A CN1029694C CN 1029694 C CN1029694 C CN 1029694C CN 93112445 CN93112445 CN 93112445 CN 93112445 A CN93112445 A CN 93112445A CN 1029694 C CN1029694 C CN 1029694C
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- nitrogen
- silicon
- heat treating
- treating method
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000012298 atmosphere Substances 0.000 title description 4
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 41
- 239000010703 silicon Substances 0.000 claims abstract description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 17
- 238000009413 insulation Methods 0.000 description 5
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to a heat treating method for a nitrogen-containing straightly-pulled silicon monocrystalline, which is characterized in that high-temperature (850 to 1150 DEG C) annealing treatment and middle-temperature (650 DEG C) annealing treatment are respectively carried out under a nitrogen atmosphere. The nitrogen-containing straightly-pulled silicon monocrystalline after the heat treatment can effectively eliminate the interference of additional donors with nitrogen content and oxygen content in silicon so as to benefit resistivity test and the manufacture of semiconductor devices.
Description
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 medium 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, think the nitrogenous oxygen czochralski silicon monocrystal that contains of in nitrogen atmosphere, growing by deep research and a large amount of experiments, 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, oxygen level 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
15/ cm
3, oxygen level is 5 * 10
18/ 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
3, also 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, it is characterized in that: 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, under nitrogen atmosphere, be heated to 650 ℃, be incubated 0.5~1 hour, be quickly cooled to normal temperature.
2, according to the method for claim 1, it is characterized in that: described The high temperature anneal, its Heating temperature are 900 ℃~1000 ℃.
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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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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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Publication Number | Publication Date |
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CN1083874A CN1083874A (en) | 1994-03-16 |
CN1029694C true CN1029694C (en) | 1995-09-06 |
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Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0927613A (en) * | 1995-07-10 | 1997-01-28 | Rohm Co Ltd | Manufacture of 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 |
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 |
CN113417010B (en) * | 2021-08-23 | 2021-11-09 | 杭州盾源聚芯半导体科技有限公司 | High-cleanliness annealing method for polycrystalline silicon rod material |
CN115369486B (en) * | 2022-10-26 | 2023-04-11 | 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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1993
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