CN102321916B - Polysilicon production method and apparatus thereof - Google Patents
Polysilicon production method and apparatus thereof Download PDFInfo
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- CN102321916B CN102321916B CN201110278731.9A CN201110278731A CN102321916B CN 102321916 B CN102321916 B CN 102321916B CN 201110278731 A CN201110278731 A CN 201110278731A CN 102321916 B CN102321916 B CN 102321916B
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Abstract
The invention relates to the solar photovoltaic technical field, and discloses a polysilicon production method and an apparatus thereof. The production method provided by the invention comprises two processing lines that: processing line I: SiCl4 and H2 are formulated according to a certain molar ratio, such that silicon Si and hydrogen chloride HCl are produced; processing line II: SiHCl3 and H2 are formulated according to a certain molar ratio, such that Si, HCl, and SiCl4 are produced. Because the by-product SiCl4 is directly used as a production raw material, raw material cost of polysilicon production is reduced, and problems in polysilicon production by-product SiCl4 processing of high cost and high difficulty are solved. Therefore, production cost of polysilicon manufactures is effectively reduced. Also, when the diameter of a silicon rod reaches a preset threshold Do, the production is switched to the second processing line, such that power consumption of polysilicon production is effectively reduced, silicon rod growth diameter is effectively increased, and polysilicon production efficiency is improved.
Description
Technical field
The present invention relates to solar-photovoltaic technology field, particularly production of polysilicon technique.
Background technology
Polysilicon is the important raw and processed materials of semi-conductor, large-scale integrated circuit and solar energy industry, photovoltaic industrial market pull and golden eggs induction under, various places polysilicon project starts one after another, polysilicon industrial prospect is wide, development is swift and violent, has become the focus of investment in China.
At present, the technique of production polysilicon (is mainly trichlorosilane SiHCl with " improved Siemens "
3reduction method) be mainstream technology.SiHCl
3with hydrogen H
2be passed into according to a certain percentage in polysilicon CVD furnace, under the envrionment conditions of certain pressure and temperature, on conductive silicon core, carry out reduction reaction deposit spathic silicon.
But production of polysilicon easily pollutes, produce 1000 tons of polysilicons and will generate approximately 15000 tons of tetrachloro silicane SiCl
4, SiCl
4have poisoning toxicity, easily deliquescence generates silicic acid and hydrogenchloride, is not good at causing very large pollution to environment if process, and human body is also had to very large harm.How processing of SiC l
4become one of focal issue of polysilicon industry.Present stage, Some Enterprises SiCl
4produce white carbon black, its economic benefit is far below polysilicon, and market is also very limited to the demand of white carbon black; Separately there is part polysilicon enterprise to adopt hot hydride process processing of SiC l
4, but there is low conversion rate, the shortcoming such as energy consumption is high, facility investment is large.
That is to say above-mentioned processing of SiC l
4method investment high, income is low, causes SiCl
4disorderly disorderly arrange, caused serious environmental pollution.And production of polysilicon is also high energy consumption industrial chain, generate 1Kg polysilicon and need approximately 45～60Kw/h of power consumption, process 1Kg by product SiCl
4need power consumption 3～5Kw/h, wherein do not comprise the required energy consumptions such as other interchanger in technology chain.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing polysilicon and device thereof, to reduce raw materials cost, solve by product SiCl
4the problems such as processing costs is high, and intractability is large, and, effectively reduce production of polysilicon power consumption, effectively increase silicon rod growth diameter, improve production of polysilicon efficiency, make production of polysilicon technique there is the advantages such as high-level efficiency, low cost, less energy-consumption.
For solving the problems of the technologies described above, embodiments of the present invention provide a kind of method for preparing polysilicon, comprise following steps:
By SiCl
4and H
2obtain Si and HCl in first mole of default proportioning ratio reaction, the described Si obtaining is deposited on silicon core electrode, and the temperature of reacting required heats described silicon core electrode by startup and obtains;
When the diameter that is deposited into silicon rod as the Si on described silicon core electrode reaches default thresholding Do, stop described SiCl
4and H
2reaction, utilize the residual temperature of described silicon core electrode, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4, by SiHCl
3and H
2the Si that reaction obtains continues to be deposited on described silicon core electrode.
Embodiments of the present invention also provide a kind of polycrystalline silicon producing device, comprise: the first process pipe, the second process pipe, reactor for polycrystalline silicon, the silicon rod that comprises silicon core electrode;
Described the first process pipe and described the second process pipe are connected to respectively described reactor for polycrystalline silicon, described in comprise silicon core electrode silicon rod be positioned at described reactor for polycrystalline silicon;
Described the first process pipe is by SiCl
4and H
2be delivered in described reactor for polycrystalline silicon and react in first mole of default proportioning ratio, obtain Si and HCl, the described Si obtaining is deposited on silicon core electrode, reaches default thresholding Do until the Si on described silicon core electrode is deposited into the diameter of silicon rod, wherein, SiCl
4and H
2the required temperature of reaction provided by the described silicon core electrode starting after heating;
Described the second process pipe is in the time that the diameter of described silicon rod reaches default thresholding Do, by SiHCl
3and H
2be delivered in described reactor for polycrystalline silicon in second mole of default proportioning ratio, utilize the residual temperature of described silicon core electrode to react, obtain Si, HCl and SiCl
4, by SiHCl
3and H
2the Si that reaction obtains continues to be deposited on described silicon core electrode.
Embodiment of the present invention in terms of existing technologies, in production of polysilicon technique, comprises two processing lines, processing line I:SiCl
4and H
2by certain mole of proportioning, generate silicon Si and hydrogenchloride HCl; Processing line II:SiHCl
3and H
2by certain mole of proportioning, generate Si, HCl and SiCl
4.Owing to directly utilizing by product SiCl
4as raw materials for production, reduce production of polysilicon raw materials cost, solved production of polysilicon by product SiCl simultaneously
4the problems such as processing costs is high, and difficulty is large, further effectively reduce the production cost of production of polysilicon producer.And, when the diameter that is deposited into silicon rod as the Si on described silicon core electrode reaches default thresholding Do, stop described SiCl
4and H
2reaction, utilize the residual temperature of described silicon core electrode, by SiHCl
3and H
2obtain Si+HCl+SiCl in second mole of default proportioning ratio reaction
4, effectively reduce production of polysilicon power consumption, further, effectively increase silicon rod growth diameter, improve production of polysilicon efficiency.
In addition, the value of default thresholding Do be when the outer end temperature of silicon rod be SiCl
4and H
2react required temperature, and silicon core electrode is while being the ultimate value being fused by high temperature, the diameter of this silicon rod.While heating due to silicon core electrode, the temperature of silicon rod distributes according to certain rules, and the regularity of distribution is for from silicon core electrode center, outside silicon rod temperature reduces gradually.Along with the increase of silicon rod diameter, be assurance SiCl
4and H
2temperature of reaction, silicon core temperature also needs to increase gradually, thereby easily causes fusible core, and the bad phenomenon such as silicon rod fracture occur.Therefore, take the outer end temperature of silicon rod as SiCl
4and H
2react required temperature, and silicon core electrode is while being the ultimate value being fused by high temperature, the diameter of this silicon rod, as the value of Do, has been realized the reasonable switching of two kinds of generating process of Si, has further guaranteed the efficient and low energy low consumption of production of polysilicon.
In addition, SiCl
4and H
2by being connected to the first process pipe of the reactor for polycrystalline silicon that is provided with described silicon rod, enter reactor for polycrystalline silicon, react; SiHCl
3and H
2by being connected to the second process pipe of this reactor for polycrystalline silicon, enter reactor for polycrystalline silicon, react.Carry out SiCl at needs
4and H
2reaction time, open the first valve arranging on the first process pipe, close the second valve arranging on the second process pipe, carry out SiHCl at needs
3and H
2reaction time, close the first valve arranging on the first process pipe, open the second valve arranging on the second process pipe, realize simply, be conducive to apply.
Accompanying drawing explanation
Fig. 1 is according to the process flow sheet of first embodiment of the invention method for preparing polysilicon;
Fig. 2 is according to the production of polysilicon process schematic representation in first embodiment of the invention;
Fig. 3 is according to the temperature schematic layout pattern on silicon rod in first embodiment of the invention.
Embodiment
The first embodiment of the present invention relates to a kind of method for preparing polysilicon.Idiographic flow as shown in Figure 1.
In step 110, by SiCl
4and H
2obtain Si and HCl in first mole of default proportioning ratio reaction, the described Si obtaining is deposited on silicon core electrode, and the temperature of reacting required heats described silicon core electrode by startup and obtains.
Specifically, silicon core electrode is started heating and/or is started heating by high-voltage power supply by reference power supply, and SiCl is provided
4and H
2react needed temperature, SiCl
4and H
2the temperature of reacting required is 1200 ℃.The span of first mole of proportioning ratio is: 1: 2 to 1: 5, the material that wherein proportional quantity is 1 was SiCl
4, it is H that proportional quantity is greater than 1 material
2.
In the present embodiment, SiCl
4and H
2the first process pipe 2 that is provided with the reactor for polycrystalline silicon 7 (being polysilicon CVD furnace) of silicon rod 6 by being connected to, enters reactor for polycrystalline silicon, as shown in Figure 2.Start heating and/or high-voltage power supply starts heating when silicon core electrode 1 (silicon core electrode 1 is included in silicon rod 6) is heated to approximately 1200 ℃, SiCl by normal power supplies
4and H
2there is following chemical reaction:
(wherein T
1approximately 1200 ℃ of temperature)
The Si generating in polysilicon CVD furnace deposits on silicon core electrode 1.
It should be noted that, in present embodiment, be connected to second process pipe 4 that also has of reactor for polycrystalline silicon, as shown in Figure 2, for by SiHCl
3and H
2be delivered to reactor for polycrystalline silicon, but in this step, still do not need SiHCl
3and H
2be delivered in reactor for polycrystalline silicon and react, specifically can be by the first valve 3 being set respectively on the first process pipe 2 and the second process pipe 4 and the second valve 5 is realized.That is to say, in this step, open the first valve 3 arranging on the first process pipe 2, close the second valve 5 arranging on the second process pipe 4, make SiCl
4and H
2within 1: 2～1: 5, enter in polysilicon CVD furnace and react by mole proportioning, generate Si.
Then,, in step 120, judge whether the diameter of silicon rod reaches default thresholding Do.Due to SiCl
4and H
2the Si generating deposits on silicon core electrode 1, and therefore the diameter of silicon rod will increase gradually.In this step, judge whether the diameter of silicon rod reaches default thresholding Do, if reached, enter step 130, if not yet reached, get back to step 110, proceed SiCl
4and H
2reaction.
In step 130, stop described SiCl
4and H
2reaction, utilize the residual temperature of described silicon core electrode, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4, by SiHCl
3and H
2the Si that reaction obtains continues to be deposited on described silicon core electrode.
Wherein, the span of second mole of proportioning ratio is: 1: 2 to 1: 5, the material that wherein proportional quantity is 1 was SiHCl
3, it is H that proportional quantity is greater than 1 material
2, SiHCl
3and H
2react required temperature and be less than described SiCl
4and H
2react required temperature.
Specifically, when the diameter that is deposited into silicon rod as the Si on silicon core electrode reaches default thresholding Do, enter into this step.The value of this Do is that the outer end temperature when silicon rod is SiCl
4and H
2react required temperature, and silicon core electrode is while being the ultimate value being fused by high temperature, the diameter of this silicon rod, about 50mm.
In this step, by closing the first valve 3 arranging on the first process pipe 2, stop SiCl
4and H
2reaction, open the second valve 5 arranging on the second process pipe 4, by SiHCl
3and H
2be delivered to reactor for polycrystalline silicon in second mole of default proportioning ratio, now the residual temperature of silicon core electrode is about 1100 ℃, SiHCl
3and H
2to there is following chemical reaction:
The Si generating in polysilicon CVD furnace continues deposition on silicon core electrode 1.
Be not difficult to find, in the present embodiment, in the early stage of production of polysilicon, when silicon rod diameter≤Do (the about 50mm of Do) of depositing on silicon core electrode, open the first valve 3 arranging on the first process pipe 2, close the second valve 5 arranging on the second process pipe 4.SiCl
4and H
2enter polysilicon CVD furnace by certain mole of proportioning (1: 2～1: 5), be heated to certain temperature by silicon core electrode, approximately 1200 ℃ of this temperature, SiCl
4and H
2there is chemical reaction.And while heating due to silicon core electrode, the temperature of silicon core electrode distributes according to certain rules, this rule is for from silicon core electrode center, outside silicon rod temperature reduces gradually, because the temperature of silicon core electrode 1 is far above silicon rod 6 outer end temperature, as shown in Figure 3.That is to say, for guaranteeing that reaction continues, and needs to guarantee that silicon rod temperature is T
1silicon rod diameter is along with Do increases, and the temperature of silicon core electrode 1 increases gradually, in the time that the temperature of silicon core electrode 1 reaches a ultimate value (this ultimate value is the value that silicon core electrode 1 is fused by high temperature), easily cause fusible core, the bad phenomenon such as silicon rod fracture occur.Therefore, before there is the bad phenomenon such as fusible core, silicon rod fracture, switch process pipeline, stop SiCl
4and H
2reaction, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4.React required temperature T
2lower than temperature T
1, can utilize the silicon rod temperature of former growth directly to reach desired reaction temperature, effectively reduce production of polysilicon power consumption, be also conducive to silicon rod growth diameter simultaneously and increase.That is to say, in the later stage of production of polysilicon, when the silicon rod diameter depositing on silicon core electrode is more than or equal to Do (the about 50mm of Do), close the first valve 3 arranging on the first process pipe 2, open the second valve 5 arranging on the second process pipe 4, by SiHCl
3and H
2within 1: 2～1: 5, enter polysilicon CVD furnace by mole proportioning, if now silicon rod 6 outer end temperature are greater than 1100 ℃, can suitably turn down silicon core electrode 1 temperature to guarantee SiHCl
3and H
2there is chemical reaction, and continue deposition on silicon core electrode 1.
As can be seen here, in present embodiment, directly utilized by product SiCl
4as raw materials for production, reduce production of polysilicon raw materials cost, solved production of polysilicon by product SiCl simultaneously
4the problems such as processing costs is high, and difficulty is large, further effectively reduce the production cost of production of polysilicon producer.And, when the diameter that is deposited into silicon rod as the Si on described silicon core electrode reaches default thresholding Do, stop described SiCl
4and H
2reaction, utilize the residual temperature of described silicon core electrode, by SiHCl
3and H
2obtain Si+HCl+SiCl in second mole of default proportioning ratio reaction
4, effectively reduce production of polysilicon power consumption, further, effectively increase silicon rod growth diameter, improve production of polysilicon efficiency.
And, take the outer end temperature of silicon rod as SiCl
4and H
2react required temperature, and silicon core electrode is while being the ultimate value being fused by high temperature, the diameter (about 50mm) of this silicon rod, as the value of Do, has been realized the reasonable switching of two kinds of generating process of Si, has further guaranteed the efficient and low energy low consumption of production of polysilicon.In addition the value that, it will be understood by those skilled in the art that Do also can, on the basis of 50mm, slightly be adjusted.
The second embodiment of the present invention relates to a kind of polycrystalline silicon producing device.This polycrystalline silicon producing device comprises: the first process pipe 2, the second process pipe 4, reactor for polycrystalline silicon 7, the silicon rod 6 that comprises silicon core electrode 1, as shown in Figure 2, the first process pipe 2 and the second process pipe 4 are connected to respectively reactor for polycrystalline silicon 7, and silicon rod 6 is positioned at reactor for polycrystalline silicon 7.
The first process pipe 2 is by SiCl
4and H
2be delivered in reactor for polycrystalline silicon 7 and react that (span of first mole of proportioning ratio is: 1: 2 to 1: 5, the material that wherein proportional quantity is 1 was SiCl in first mole of default proportioning ratio
4, it is H that proportional quantity is greater than 1 material
2), obtain Si and HCl, the described Si obtaining is deposited on silicon core electrode 1, reaches default thresholding Do until the Si on silicon core electrode 1 is deposited into the diameter of silicon rod, wherein, the value of Do be when the outer end temperature of described silicon rod be SiCl
4and H
2react required temperature, and described silicon core electrode is while being the ultimate value being fused by high temperature, the diameter of described silicon rod.SiCl
4and H
2the required temperature of reaction provide (SiCl by the silicon core electrode 1 starting after heating
4and H
2the temperature of reacting required is 1200 ℃), such as silicon core electrode 1 is with power input, this power input is connected with reference power supply and/or high-voltage power supply, makes this silicon core electrode 1 to be started heating by reference power supply and/or high-voltage power supply.The second process pipe 4 is in the time that the diameter of silicon rod 6 reaches default thresholding Do, by SiHCl
3and H
2be delivered in second mole of default proportioning ratio that in reactor for polycrystalline silicon 7, (span of second mole of proportioning ratio is: 1: 2 to 1: 5, the material that wherein proportional quantity is 1 was SiHCl
3, it is H that proportional quantity is greater than 1 material
2), utilize the residual temperature of silicon core electrode 1 to react (SiHCl
3and H
2react required temperature and be less than described SiCl
4and H
2react required temperature), obtain Si, HCl and SiCl
4, by SiHCl
3and H
2the Si that reaction obtains continues to be deposited on silicon core electrode 1.
Specifically, the first process pipe 2 is provided with the first valve 3, the second process pipes 4 and is provided with the second valve 5.In the early stage of production of polysilicon, when silicon rod diameter≤Do (the about 50mm of Do) of depositing on silicon core electrode, open the first valve 3 arranging on the first process pipe 2, close the second valve 5 arranging on the second process pipe 4.SiCl
4and H
2within 1: 2～1: 5, enter polysilicon CVD furnace by certain mole of proportioning, be heated to certain temperature by silicon core electrode, approximately 1200 ℃ of this temperature, SiCl
4and H
2there is chemical reaction.And while heating due to silicon core electrode, the temperature of silicon core electrode distributes according to certain rules, this rule is for from silicon core electrode center, outside silicon rod temperature reduces gradually, because the temperature of silicon core electrode 1 is far above silicon rod 6 outer end temperature, as shown in Figure 3.That is to say, for guaranteeing that reaction continues, and needs to guarantee that silicon rod temperature is T
1silicon rod diameter is along with Do increases, and the temperature of silicon core electrode 1 increases gradually, in the time that the temperature of silicon core electrode 1 reaches a ultimate value (this ultimate value is the value that silicon core electrode 1 is fused by high temperature), easily cause fusible core, the bad phenomenon such as silicon rod fracture occur.Therefore, before there is the bad phenomenon such as fusible core, silicon rod fracture, switch process pipeline, stop SiCl
4and H
2reaction, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4.React required temperature T
2lower than temperature T
1, can utilize the silicon rod temperature of former growth directly to reach desired reaction temperature, effectively reduce production of polysilicon power consumption, be also conducive to silicon rod growth diameter simultaneously and increase.That is to say, in the later stage of production of polysilicon, when the silicon rod diameter depositing on silicon core electrode is more than or equal to Do (the about 50mm of Do), close the first valve 3 arranging on the first process pipe 2, open the second valve 5 arranging on the second process pipe 4, by SiHCl
3and H
2within 1: 2～1: 5, enter polysilicon CVD furnace by mole proportioning, if now silicon rod 6 outer end temperature are greater than 1100 ℃, can suitably turn down silicon core electrode 1 temperature to guarantee SiHCl
3and H
2there is chemical reaction, and continue deposition on silicon core electrode 1.
Be not difficult to find, carry out SiCl at needs
4and H
2reaction time, open the first valve arranging on the first process pipe, close the second valve arranging on the second process pipe, carry out SiHCl at needs
3and H
2reaction time, close the first valve arranging on the first process pipe, open the second valve arranging on the second process pipe, realize simply, be conducive to apply.
In addition, in actual applications, also can, directly by the control of the opening for feed to the first process pipe and the second process pipe, realize the switching of two kinds of Si generating process.
The respective embodiments described above are to realize specific embodiments of the invention, and in actual applications, can do various changes to it in the form and details, and without departing from the spirit and scope of the present invention.
Claims (8)
1. a method for preparing polysilicon, is characterized in that, comprises following steps:
By SiCl
4and H
2obtain Si and HCl in first mole of default proportioning ratio reaction, the described Si obtaining is deposited on silicon core electrode, and the temperature of reacting required heats described silicon core electrode by startup and obtains;
When the diameter that is deposited into silicon rod as the Si on described silicon core electrode reaches default thresholding Do, stop described SiCl
4and H
2reaction, utilize the residual temperature of described silicon core electrode, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4, by SiHCl
3and H
2the Si that reaction obtains continues to be deposited on described silicon core electrode.
2. method for preparing polysilicon according to claim 1, is characterized in that, the value of described Do is that the outer end temperature when described silicon rod is SiCl
4and H
2react required temperature, and described silicon core electrode is while being the ultimate value being fused by high temperature, the diameter of described silicon rod.
3. method for preparing polysilicon according to claim 2, is characterized in that, the value of described Do is 50mm.
4. method for preparing polysilicon according to claim 1, is characterized in that, the span of described first mole of proportioning ratio is: 1:2 to 1:5, the material that wherein proportional quantity is 1 is SiCl
4, it is H that proportional quantity is greater than 1 material
2;
Described SiCl
4and H
2the temperature of reacting required is 1200 ℃.
5. method for preparing polysilicon according to claim 1, is characterized in that, the span of described second mole of proportioning ratio is: 1:2 to 1:5, the material that wherein proportional quantity is 1 is SiHCl
3, it is H that proportional quantity is greater than 1 material
2;
Described SiHCl
3and H
2react required temperature and be less than described SiCl
4and H
2react required temperature.
6. according to the method for preparing polysilicon described in any one in claim 1 to 5, it is characterized in that,
Described silicon core electrode is started heating and/or is started heating by high-voltage power supply by reference power supply.
7. according to the method for preparing polysilicon described in any one in claim 1 to 5, it is characterized in that described SiCl
4and H
2by being connected to the first process pipe of the reactor for polycrystalline silicon that is provided with described silicon rod, enter described reactor for polycrystalline silicon, react;
Described SiHCl
3and H
2by being connected to the second process pipe of described reactor for polycrystalline silicon, enter described reactor for polycrystalline silicon, react.
8. method for preparing polysilicon according to claim 7, it is characterized in that, when the diameter that is deposited into silicon rod as the Si on described silicon core electrode reaches default thresholding Do, by closing the first valve arranging on described the first process pipe, open the second valve arranging on described the second process pipe, stop described SiCl
4and H
2reaction, by SiHCl
3and H
2obtain Si, HCl and SiCl in second mole of default proportioning ratio reaction
4.
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723371A (en) * | 2008-10-29 | 2010-06-09 | 卓越诚信集团有限公司 | Method for generating polycrystalline silicon by recycling by-products |
| CN101723370A (en) * | 2008-10-13 | 2010-06-09 | 刘雅铭 | Polysilicon production method without silicon tetrachloride emission |
| CN202369401U (en) * | 2011-09-19 | 2012-08-08 | 上海森松新能源设备有限公司 | Polysilicon production device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723370A (en) * | 2008-10-13 | 2010-06-09 | 刘雅铭 | Polysilicon production method without silicon tetrachloride emission |
| CN101723371A (en) * | 2008-10-29 | 2010-06-09 | 卓越诚信集团有限公司 | Method for generating polycrystalline silicon by recycling by-products |
| CN202369401U (en) * | 2011-09-19 | 2012-08-08 | 上海森松新能源设备有限公司 | Polysilicon production device |
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