CN108840340A - A kind of preparation method of polysilicon - Google Patents
A kind of preparation method of polysilicon Download PDFInfo
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- CN108840340A CN108840340A CN201811075034.1A CN201811075034A CN108840340A CN 108840340 A CN108840340 A CN 108840340A CN 201811075034 A CN201811075034 A CN 201811075034A CN 108840340 A CN108840340 A CN 108840340A
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- Prior art keywords
- gas
- mixture
- silicon
- dichlorosilane
- preparation
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229920005591 polysilicon Polymers 0.000 title abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 66
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 49
- 239000010703 silicon Substances 0.000 claims abstract description 49
- 239000000203 mixture Substances 0.000 claims abstract description 44
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000008016 vaporization Effects 0.000 claims description 12
- 238000009388 chemical precipitation Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 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 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- -1 silicon free radical Chemical class 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 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
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention discloses a kind of preparation method of polysilicon, including：Dichlorosilane gas, trichlorosilane gas and hydrogen are mixed, mixture is obtained；Reduction furnace is fed the mixture into, third mixture carries out gas chemistry precipitation reaction, generates polysilicon in silicon wicking surface, obtains silicon rod；The preparation method makes the polycrystalline silicon growth generated on silicon rod or silicon core, improves yield, shortens the entire growth cycle of silicon rod；Meanwhile reducing power consumption, save the cost.
Description
Technical Field
The invention relates to the technical field of polycrystalline silicon production, in particular to a preparation method of polycrystalline silicon.
Background
Polycrystalline silicon is a raw material for preparing solar cells and is the basis of the photovoltaic industry all over the world. At present, most factories at home and abroad adopt trichlorosilane as a silicon source to produce polysilicon. Although the yield of the method is not low, the method separates dichlorosilane generated in the production process and treats the dichlorosilane as a byproduct. This not only complicates the process, but also wastes raw material industrial silicon, resulting in high production cost.
The dichlorosilane method has also been used earlier as a silicon source for producing semiconductor polysilicon. The method has high production rate, but because the silicon free radical is active and the reaction temperature is low, part of materials can generate homogeneous nucleation, namely, part of silicon does not grow on a silicon rod or a silicon core in a reduction furnace, but directly reacts in a cavity of the reduction furnace to generate silicon, and the silicon is gathered on a chassis and a furnace wall and cannot be recycled, so that the actual yield of the method is low.
Disclosure of Invention
In view of this, the present application provides a method for preparing polycrystalline silicon, which allows the generated polycrystalline silicon to grow on a silicon rod or a silicon core, improves the yield, and shortens the entire growth cycle of the silicon rod; meanwhile, the power consumption is reduced, and the cost is saved.
In order to solve the technical problems, the technical scheme provided by the invention is a preparation method of polycrystalline silicon, which comprises the following steps:
mixing dichlorosilane gas, trichlorosilane gas and hydrogen to obtain a mixture;
and (4) feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture, and generating polycrystalline silicon on the surface of the silicon core to obtain the silicon rod.
Preferably, the preparation method further comprises: heating and vaporizing dichlorosilane to obtain the dichlorosilane gas.
Preferably, in the process of heating and vaporizing the dichlorosilane, the heating and vaporizing temperature is 100-110 ℃.
Preferably, the preparation method further comprises: heating and vaporizing the trichlorosilane to obtain the trichlorosilane gas.
Preferably, in the process of heating and vaporizing trichlorosilane, the heating and vaporizing temperature is 100-110 ℃.
Preferably, the preparation method further comprises: the hydrogen is subjected to preheating treatment.
Preferably, in the preheating process, the preheating temperature is 90-100 ℃.
Preferably, the preparation method specifically comprises the following steps:
mixing dichlorosilane gas, trichlorosilane gas and hydrogen in a mixture to obtain a mixture;
and (3) feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture in the reduction furnace, and generating polycrystalline silicon on the surface of a silicon core in the reduction furnace to obtain the silicon rod.
Preferably, the temperature condition of the gas-phase chemical precipitation reaction is 1020-1120 ℃, the pressure condition is preferred, and the temperature condition of the gas-phase chemical precipitation reaction is 1020-1120 ℃, and the pressure condition is 0.45-0.5 MPa.
Preferably, the preparation method further comprises: and gradually reducing the content of the dichlorosilane gas in the mixture in the silicon rod growing process.
Preferably, the preparation method further comprises: the content of the dichlorosilane gas in the mixture is 10-15% in volume percentage at the initial growth stage of the silicon rod, and the content of the dichlorosilane gas in the mixture is 2% when the growth of the silicon rod is completed.
Preferably, the whole growth cycle of the silicon rod is within 100 hours.
Preferably, the molar ratio of the total content of the dichlorosilane gas and the trichlorosilane gas to the hydrogen content in the mixed gas is 1: 2-1: 10.
compared with the prior art, the detailed description of the application is as follows:
the invention provides a preparation method of polycrystalline silicon, which is characterized in that dichlorosilane gas, trichlorosilane gas and hydrogen are mixed to obtain a mixture; namely, the independent control and independent feeding of the dichlorosilane gas are realized. Thereby realizing the control of the content of dichlorosilane gas in the mixture in the silicon rod growing process. Furthermore, the content of dichlorosilane gas in the mixture is gradually reduced in the silicon rod growth process, the content of dichlorosilane gas in the mixture at the initial growth stage of the silicon rod is 10-15% in terms of volume percentage, and the content of dichlorosilane gas in the mixture is 2% when the silicon rod growth is completed. Firstly, the deposition temperature of dichlorosilane is lower than that of trichlorosilane, dichlorosilane gas, trichlorosilane gas and hydrogen are used as raw materials, and compared with the method only adopting trichlorosilane, the method can reduce the power consumption in the gas phase chemical deposition process, thereby reducing the production cost; secondly, the content of the dichlorosilane gas in the mixture is gradually reduced from 10-15% of the silicon rod in the initial growth stage to 2%, the reaction can be effectively accelerated by adopting 10-15% of the dichlorosilane gas in the initial growth stage, the energy consumption is reduced, and meanwhile, the dichlorosilane gas with the content is a gas-phase chemical deposition raw material, so that the phenomenon that the dichlorosilane reacts violently to generate powder can be avoided; the content of dichlorosilane gas in the mixture is gradually reduced, so that trichlorosilane reacts to generate silicon, hydrogen chloride, hydrogen, silicon tetrachloride and dichlorosilane, dichlorosilane reacts to generate silicon and hydrogen chloride, and the dichlorosilane reaches a dynamic balance in a reduction furnace, so that the dichlorosilane gas is further effectively accelerated to react, the power consumption is reduced, and meanwhile, the dichlorosilane is prevented from generating powder through violent reaction. Thereby realizing the purposes of reducing power consumption, saving cost, growing the generated polysilicon on the silicon rod or the silicon core, improving yield and shortening the whole growth period of the silicon rod.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of a method for preparing polysilicon according to the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to specific embodiments.
Example 1
As shown in figure 1 of the drawings, in which,
a method for preparing polycrystalline silicon comprises the following steps:
heating and vaporizing dichlorosilane at 100-110 ℃ to obtain dichlorosilane gas; the preparation method further comprises the following steps: heating and vaporizing trichlorosilane at 100-110 ℃ to obtain trichlorosilane gas;
mixing dichlorosilane gas, trichlorosilane gas and hydrogen in a mixture to obtain a mixture; the hydrogen is preheated, and the preheating temperature is 90-100 ℃;
feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture in the reduction furnace, and generating polycrystalline silicon on the surface of a silicon core in the reduction furnace to obtain a silicon rod; the temperature condition of the gas phase chemical precipitation reaction is 1020-1120 ℃, and the pressure condition is 0.45-0.5 MPa.
Wherein,
the molar ratio of the total content of the dichlorosilane gas and the trichlorosilane gas to the hydrogen content in the mixed gas is 1: 2-1: 10.
the preparation method further comprises the following steps: controlling the air input of the dichlorosilane gas, and gradually reducing the content of the dichlorosilane gas in the mixture in the silicon rod growing process; according to the volume percentage, the content of the dichlorosilane gas in the mixture is 10% at the initial growth stage of the silicon rod, and the content of the dichlorosilane gas in the mixture is 2% when the growth of the silicon rod is completed.
According to the preparation method of the polycrystalline silicon, the generated polycrystalline silicon grows on the silicon rod or the silicon core, the primary conversion rate is more than 15%, the whole growth cycle of the silicon rod is within 100 hours, and the average power consumption of the generated polycrystalline silicon per kilogram is 48 degrees (calculated by a polycrystalline silicon reduction furnace of 24 pairs of electric shock rods).
Example 2
The difference between this example and example 1 is only that the content of dichlorosilane gas in the mixture during the initial growth of the silicon rods is 12% by volume.
According to the preparation method of the polycrystalline silicon, the generated polycrystalline silicon grows on the silicon rod or the silicon core, the primary conversion rate is more than 16%, the whole growth cycle of the silicon rod is within 100 hours, and the average power consumption of the generated polycrystalline silicon per kilogram is 47 degrees (calculated by a 24-pair electric shock rod polycrystalline silicon reduction furnace).
Example 3
The difference between this example and example 1 is only that the content of dichlorosilane gas in the mixture during the initial growth of the silicon rods is 15% by volume.
According to the preparation method of the polycrystalline silicon, the generated polycrystalline silicon grows on the silicon rod or the silicon core, the primary conversion rate is more than 17%, the whole growth cycle of the silicon rod is within 100 hours, and the average power consumption of the generated polycrystalline silicon per kilogram is 46 degrees (calculated by a polycrystalline silicon reduction furnace of 24 pairs of electric shock rods).
Comparative example 1
A method for preparing polycrystalline silicon comprises the following steps:
heating and vaporizing dichlorosilane at 100-110 ℃ to obtain dichlorosilane gas; the preparation method further comprises the following steps: heating and vaporizing trichlorosilane at 100-110 ℃ to obtain trichlorosilane gas;
mixing dichlorosilane gas, trichlorosilane gas and hydrogen in a mixture to obtain a mixture; the hydrogen is preheated, and the preheating temperature is 90-100 ℃;
feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture in the reduction furnace, and generating polycrystalline silicon on the surface of a silicon core in the reduction furnace to obtain a silicon rod; the temperature condition of the gas phase chemical precipitation reaction is 1020-1120 ℃, and the pressure condition is 0.45-0.5 MPa.
Wherein,
the molar ratio of the total content of the dichlorosilane gas and the trichlorosilane gas to the hydrogen content in the mixed gas is 1: 2-1: 10. the content of the dichlorosilane gas in the mixture is less than 4 percent by volume percentage.
According to the preparation method of the polycrystalline silicon, a large amount of silicon powder is generated in the later growth stage of the silicon rod.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. A method for preparing polycrystalline silicon, comprising:
mixing dichlorosilane gas, trichlorosilane gas and hydrogen to obtain a mixture;
and (4) feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture, and generating polycrystalline silicon on the surface of the silicon core to obtain the silicon rod.
2. The method of manufacturing according to claim 1, further comprising: heating and vaporizing dichlorosilane to obtain the dichlorosilane gas.
3. The method of manufacturing according to claim 1, further comprising: heating and vaporizing the trichlorosilane to obtain the trichlorosilane gas.
4. The method of manufacturing according to claim 1, further comprising: the hydrogen is subjected to preheating treatment.
5. The preparation method according to claim 1, wherein the preparation method specifically comprises:
mixing dichlorosilane gas, trichlorosilane gas and hydrogen in a mixture to obtain a mixture;
and (3) feeding the mixture into a reduction furnace, carrying out gas-phase chemical precipitation reaction on the third mixture in the reduction furnace, and generating polycrystalline silicon on the surface of a silicon core in the reduction furnace to obtain the silicon rod.
6. The preparation method according to claim 1, wherein the gas phase chemical precipitation reaction temperature condition is 1020-1120 ℃ and the pressure condition is 0.45-0.5 MPa.
7. The method of manufacturing according to claim 1, further comprising: and gradually reducing the content of the dichlorosilane gas in the mixture in the silicon rod growing process.
8. The method of manufacturing according to claim 7, further comprising: the content of the dichlorosilane gas in the mixture is 10-15% in volume percentage at the initial growth stage of the silicon rod, and the content of the dichlorosilane gas in the mixture is 2% when the growth of the silicon rod is completed.
9. The preparation method according to claim 1, wherein the entire growth cycle of the silicon rod is within 100 hours.
10. The preparation method according to claim 1, wherein the molar ratio of the total content of the dichlorosilane gas and the trichlorosilane gas to the hydrogen content in the mixed gas is 1: 2-1: 10.
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| CN201811075034.1A CN108840340A (en) | 2018-09-14 | 2018-09-14 | A kind of preparation method of polysilicon |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007047210A1 (en) * | 2007-10-02 | 2009-04-09 | Wacker Chemie Ag | Polycrystalline silicon and process for its preparation |
| CN102642834A (en) * | 2012-05-10 | 2012-08-22 | 雅安永旺硅业有限公司 | Method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon |
| CN102674358A (en) * | 2011-03-08 | 2012-09-19 | 内蒙古盾安光伏科技有限公司 | Method and system for producing polysilicon |
| CN107720755A (en) * | 2017-11-02 | 2018-02-23 | 成都蜀菱科技发展有限公司 | A kind of production of polysilicon raw material and method for preparing polysilicon |
| CN207347177U (en) * | 2017-10-25 | 2018-05-11 | 新疆合晶能源科技有限公司 | Polycrystalline silicon production system |
-
2018
- 2018-09-14 CN CN201811075034.1A patent/CN108840340A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007047210A1 (en) * | 2007-10-02 | 2009-04-09 | Wacker Chemie Ag | Polycrystalline silicon and process for its preparation |
| CN102674358A (en) * | 2011-03-08 | 2012-09-19 | 内蒙古盾安光伏科技有限公司 | Method and system for producing polysilicon |
| CN102642834A (en) * | 2012-05-10 | 2012-08-22 | 雅安永旺硅业有限公司 | Method adopting trichlorosilane and dichlorosilane mixed raw materials to produce polycrystalline silicon |
| CN207347177U (en) * | 2017-10-25 | 2018-05-11 | 新疆合晶能源科技有限公司 | Polycrystalline silicon production system |
| CN107720755A (en) * | 2017-11-02 | 2018-02-23 | 成都蜀菱科技发展有限公司 | A kind of production of polysilicon raw material and method for preparing polysilicon |
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