CN105439149B - The method that improved Siemens reduction furnace improves polysilicon primary depositing rate - Google Patents
The method that improved Siemens reduction furnace improves polysilicon primary depositing rate Download PDFInfo
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- CN105439149B CN105439149B CN201510969103.3A CN201510969103A CN105439149B CN 105439149 B CN105439149 B CN 105439149B CN 201510969103 A CN201510969103 A CN 201510969103A CN 105439149 B CN105439149 B CN 105439149B
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- cycle
- sihcl
- reduction furnace
- hydrogen
- polysilicon
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 30
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 28
- 238000000151 deposition Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 11
- 229910003822 SiHCl3 Inorganic materials 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 16
- 239000006227 byproduct Substances 0.000 claims description 20
- 229910003910 SiCl4 Inorganic materials 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000004134 energy conservation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
Abstract
The present invention is a kind of method that improved Siemens reduction furnace improves polysilicon primary depositing rate.It is characterized in that into the H of reduction furnace2/SiHCl3Molar ratio improves the mol ratio value of hydrogen and trichlorosilane in the range of 38, and polysilicon primary depositing rate will be by formula η=(1+0.06)nη0It is improved.In formula, η0：Primary deposit rate；η：Change the primary depositing rate after mol ratio；n：More original mol ratio raising value, n=0,1,2,3 ....
Description
Technical field
It is particularly a kind of the present invention relates to a kind of energy-conservation of improved Siemens reduction furnace growing polycrystalline silicon, consumption-reducing method
The method that improved Siemens reduction furnace improves polysilicon primary depositing rate.
Background technology
Improved Siemens reduction furnace, it in improvement Siemens process with hydrogen and trichlorosilane is raw material to be, reacted life
Grow the special equipment of polysilicon.Carried out into the hydrogen inside reduction furnace and trichlorosilane in 1080 DEG C or so of silicon wicking surface
Reaction, the silicon of generation constantly increases in silicon wicking surface deposition, crystallization, diameter, ultimately forms rod-like polycrystal silicon product.It is reacted
Accessory substance H2、SiHCl3、SiCl4Etc. it is recovered, separation, conversion, purification after reusable edible.In reduction furnace and system design, many
Under the premise of crystal silicon growth deposition surface temperature is fixed, rationally whether operating condition, can be by polysilicon primary depositing rate, many
Crystal silicon sedimentation rate, SiCl4Several index expression of by-product rate.
Rational feed quantity, H in polysilicon growth process2/SiHCl3The condition such as proportioning and operating pressure passes through science meter
Good energy-conservation, consumption reduction effect can be obtained by calculating and coordinating control.Except the surface temperature of whole polycrystalline silicon growth, deposition process is protected
Hold beyond reasonable, stabilization, H2、SiHCl3Mixing, proportioning, inventory etc. realize continuous regulation and control by technological requirement, be operation, fortune
Capable necessary condition.
The content of the invention
In view of can be made full use of in improved Siemens reduction furnace production polysilicon process the recovery of accessory substance, separation,
Conversion, purification, utilization, reach energy-conservation, the effect of consumption reduction, and the purpose of the present invention aims to provide a kind of improved Siemens reduction furnace
The method for improving polysilicon primary depositing rate, it is characterised in that enter the molar ratio of both the hydrogen and trichlorosilane of reduction furnace
H2/SiHCl3Improved in the range of 3-8, polysilicon primary depositing rate will be improved as the following formula：
η=(1+0.06)nη0
In formula：
η0：Primary deposit rate
η：Change the primary depositing rate after mol ratio
n：More original mol ratio raising value, n=0,1,2,3 ....
Polysilicon primary depositing rate=cycle polysilicon quantum of output/cycle enters the total amount of silicon in reduction furnace material.Can
See, it is one of target of cycle polysilicon output capacity that the producer pursues to improve polysilicon primary depositing rate.Taken off according to the present invention
The hydrogen shown and the changing rule of the mol ratio value and raising polysilicon primary depositing rate of trichlorosilane, according to computing formula：
η=(1+0.06)nη0
Limiting the molar ratio of molar ratio excursion internal control hydrogen and trichlorosilane, you can reach raising polycrystalline
The purpose of silicon primary depositing rate.
The present invention is produced to the purification, separation, conversion of polysilicon by-product, circulation profit for improved Siemens reduction furnace
With the output capacity of cycle polysilicon can be improved from byproduct hydrogen, trichlorosilane and silicon tetrachloride, and reduce byproduct trichlorine
The output of hydrogen silicon and silicon tetrachloride, so as to reach energy-saving purpose.
Embodiment
Embodiment 1：
According to raising H2/SiHCl3Molar ratio, can be improved in the changing rule of polysilicon primary depositing rate, the present embodiment,
The original molar ratio of hydrogen and trichlorosilane is 4, the molar ratio of the hydrogen after raising and trichlorosilane for 8, i.e. n=8-
4 = 4.Original primary depositing rate η0For 9-11%, mol ratio is brought up to after 8, substitutes into formula：η=(1+0.06)nη0, polysilicon
Primary depositing rate η brings up to 12-14%.Primary depositing polysilicon amount（I.e. one reduction furnace production per cycle）Reach 4.1 tons/week
Phase platform.
After mol ratio increase, byproduct accordingly changes, and is confirmed from one group of following reference data：
The molar ratio of hydrogen and trichlorosilane：Mol ratio=8 of mol ratio=4
It is fed SiHCl3Measure (ton/cycle)： 221--181 166--133
By-product SiHCl3Measure (ton/cycle)： 100.0--102.0 80.0--78.0
By-product SiCl4Measure (ton/cycle)： 126.0--75.0 84.0--45.0
By-product SiHCl3/SiCl4(mol ratios): 1.0--1.7 1.2--2.2
Other micro summaries.
From correction data above, reacted accessory substance SiHCl3、SiCl4After recovered, separation, conversion, purification
Participation is recycled so that the polysilicon product output capacity of needs is improved, byproduct SiHCl3、SiCl4Output declines.
Embodiment 2：
According to raising H2/SiHCl3Molar ratio can be improved in the changing rule of polysilicon primary depositing rate, the present embodiment,
Hydrogen is 3 with the original molar ratio of trichlorosilane, and the hydrogen after raising is 6, i.e. n=6-3=with the molar ratio of trichlorosilane
3.Original primary depositing rate η0=7-9%, mol ratio is brought up to after 6, substitutes into formula：
Polysilicon primary depositing rate η=(1+0.06)nη0 = 9-11%。
After mol ratio increase, byproduct accordingly changes, and is confirmed from one group of following reference data：
The molar ratio of hydrogen and trichlorosilane：Mol ratio=6 of mol ratio=3
It is fed SiHCl3Measure (ton/cycle)： 235--195 195--155
By-product SiHCl3Measure (ton/cycle)： 106--108 90--88
By-product SiCl4Measure (ton/cycle)： 135--85.0 100--50
By-product SiHCl3/SiCl4(mol ratios): 1.0--1.3 1.16--2.17
Other micro summaries.
From the correction data of above example, reacted accessory substance SiHCl3、SiCl4It is recovered, separation, conversion,
Participate in recycling after purification so that the polysilicon product output capacity of needs is improved, byproduct SiHCl3、SiCl4Output declines.
Prove the present invention be can practical operation energy-saving method with practical value.
Claims (1)
1. a kind of method that improved Siemens reduction furnace improves polysilicon primary depositing rate, it is characterised in that hydrogen and trichlorine
The original molar ratio of hydrogen silicon is 4, and the hydrogen after raising is 8, i.e. n=8-4=4 with the molar ratio of trichlorosilane；Original one
Secondary deposition η0For 9-11%, mol ratio is brought up to after 8, substitutes into formula：η=(1+0.06)nη0, polysilicon primary depositing rate η
Bring up to 12-14%；Primary depositing polysilicon amount, i.e., one reduction furnace production per cycle reaches 4.1 tons/cycle platforms；
During the molar ratio of hydrogen and trichlorosilane=4；It is fed SiHCl3Amount：221-181 tons/cycle；By-product SiHCl3Amount：
100.0--102.0 tons/cycle；By-product SiCl4Amount：126.0--75.0 tons/cycle；By-product SiHCl3/SiCl4Mol ratios：
1.0--1.7；Other micro summaries；
During the molar ratio of hydrogen and trichlorosilane=8；It is fed SiHCl3Amount：166-133 tons/cycle；By-product SiHCl3Amount：
80.0--78.0 tons/cycle；By-product SiCl4Amount：84.0--45.0 tons/cycle；By-product SiHCl3/SiCl4Mol ratios：1.2--
2.2；Other micro summaries.
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|---|---|---|---|
| CN201510969103.3A CN105439149B (en) | 2015-12-22 | 2015-12-22 | The method that improved Siemens reduction furnace improves polysilicon primary depositing rate |
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| CN105439149A CN105439149A (en) | 2016-03-30 |
| CN105439149B true CN105439149B (en) | 2017-07-11 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717087A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method for producing polysilicon rod |
| CN101717088A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method and device for efficiently producing polycrystalline silicon |
| CN101717086A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method for producing polysilicon |
| CN101780956A (en) * | 2010-03-03 | 2010-07-21 | 清华大学 | Method and device for preparing high purity polysilicon particles by using fluid bed reactor |
-
2015
- 2015-12-22 CN CN201510969103.3A patent/CN105439149B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717087A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method for producing polysilicon rod |
| CN101717088A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method and device for efficiently producing polycrystalline silicon |
| CN101717086A (en) * | 2009-11-25 | 2010-06-02 | 江苏中能硅业科技发展有限公司 | Method for producing polysilicon |
| CN101780956A (en) * | 2010-03-03 | 2010-07-21 | 清华大学 | Method and device for preparing high purity polysilicon particles by using fluid bed reactor |
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Effective date of registration: 20240318 Address after: 610000 Xincai 18th Road, new material industrial functional zone, Xinjin Industrial Park, Xinjin County, Chengdu City, Sichuan Province Patentee after: CHENGDU SHULING TECHNOLOGY DEVELOPMENT Co.,Ltd. Guo jiahuodiqu after: Zhong Guo Address before: 611400 No. 445, Qingyun South Road, Puxing street, Xinjin District, Xinjin County, Chengdu, Sichuan Patentee before: Sichuan mintian Technology Development Co.,Ltd. Guo jiahuodiqu before: Zhong Guo |