CN101948113B - Method and equipment for preparing polycrystalline silicon through physical phosphorous removal - Google Patents
Method and equipment for preparing polycrystalline silicon through physical phosphorous removal Download PDFInfo
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- CN101948113B CN101948113B CN201010286544.0A CN201010286544A CN101948113B CN 101948113 B CN101948113 B CN 101948113B CN 201010286544 A CN201010286544 A CN 201010286544A CN 101948113 B CN101948113 B CN 101948113B
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Abstract
The invention discloses a method and equipment for preparing polycrystalline silicon through physical phosphorous removal, and a method and equipment for reducing phosphorus content of metallurgical silicon by a physical method. In the method, phosphorous is removed from the metallurgical silicon in a specific environment by mainly using the physical characteristics of phosphorous so that the metallurgical silicon meets the requirement of solar silicon. Meanwhile, the invention also discloses the equipment which is provided with a micropore stirring tray and matched with the method. The method and the equipment have the advantages of simple process, high efficiency, energy conservation and the environmental protection, and are suitable for popularization.
Description
Technical field
The present invention relates to method for manufacturing polycrystalline silicon, be specially a kind of physical property of phosphorus of utilizing by the method and apparatus of a kind of preparing polycrystalline silicon through physical phosphorous removal of phosphorus removal.
Background technology
Along with the global Energy Consumption amount improves constantly, conventional non-regeneration energy can not meet the demand and supply of most countries.According to the analysis of world energy sources authoritative institution, according to fossil energy reserves and the recovery rate verified at present, to calculate, the Global Oil residue can be exploited the time limit only 40 years, and the Sweet natural gas residue can be adopted the time limit 60 years, and the coal residue can be adopted the time limit 120 years.On the other hand, the exploitation of the disposable energy and application are also major reasons that causes ecological damage and global environmental pollution.Therefore, the application of renewable new forms of energy is prerequisites of the permanent development of the mankind, is also the basic method of our sustainable development.
New forms of energy photovoltaic generation industry, as renewable and clean energy resource, because of its have safe and reliable, noiseless, pollution-free, restriction less, the not available advantage of other conventional energy resourcess such as failure rate is low, easy maintenance, resource be wide, being recognized is important new forms of energy of 21 century, be widely used in generate electricity by way of merging two or more grid systems, the aspects such as civilian power generation, communal facility and integrated energy-saving building, the crystalline silicon photovoltaic power generation system occupies the main status in new forms of energy photovoltaic generation market at present.Along with application and the silicon chip processing technology of polycrystalline silicon purifying technology are further ripe, the raising of photoelectric transformation efficiency and the development of other Technologies, comprise that the renewable energy source of new forms of energy photovoltaic generation fully likely completes from supplementing the role transforming of the energy to conventional energy resources.
As the basic product of photovoltaic generation industry-High Purity Polycrystalline silicon materials, the progress of its production technology is the important step that can the photovoltaic generation industry promotion and application development.The reliability that how to reduce cost for solar power generation, environmental contamination reduction, reduction production energy consumption, raising production safety is the important topic of theCourse of PV Industry.Worldwide production high purity polycrystalline silicon material is mainly used siemens's chemical manufacturing process at present, but, along with increase and the impact of Present Global financial crisis the requirement of environment protection, safety in the whole world, the market requirement is the HIGH-PURITY SILICON material of low price more.New in the case low cost more environmental protection high purity polycrystalline silicon production technology is continually developed and is obtained successfully in the whole world, particularly the Physical high purity polycrystalline silicon production technology of low-cost environmental-protecting is achieved success and obtains effectively using checking in the utilization field in some developed countries (Japan, the U.S., Germany, Canada), for the production of Physical high purity polycrystalline silicon provides huge development space; The 6N HIGH-PURITY SILICON material of the Physical production of low-cost environmental-protecting applies in a large number solar cell and manufactures photovoltaic industry, with lower cost of electricity-generating, advances the sun power clean electric power generation to be widely used.
In metallurgical grade silicon, trace impurity almost contains all elements in the periodic table of elements, characteristic difference due to each family's element, impurity element in silicon will be removed one by one and be reached requirement, its technology controlling and process is very complicated and strict, and the difficulty faced in purification process is a lot.At first must analyze grasp to the chemical property of each impurity element in silicon, suit the remedy to the case, try out, the prior mutual pollution that will prevent impurity element in purification process.
The method of various countries' production polysilicon mainly contains chemical method and metallurgy method in the world at present.And chemical method mainly be take Siemens Method as main; Metallurgy method is mainly the physical purification technology, also claims Physical.Both key distinctions are that chemical method changes the chemical composition of silicon in technological process, finally be reduced into silicon through a series of chemical reaction, and Physical keep the components unchanged of silicon in production process, by a series of impurity elimination, purify and form.
Siemens's chemical method mainly utilizes metallurgical grade silicon to be reacted with anhydrous hydrogen chloride and generates trichlorosilane (SiHCl
3), then obtaining the electronic-grade trichlorosilane by distillation, the trichlorosilane after purification is heated to 1100 ℃ and carries out VCD reaction generation high purity polycrystalline silicon in hydrogen reduction furnace.
The removal of Physical purification techniques impurity element can be divided into two classes: a class is the removal of metallic impurity elements, and mainly take Fe, Al, Ca trigram element is representative; Another kind of is the removal of non-metallic element, is mainly that two elements of P and B are representative.The requirement of solar-grade polysilicon is that total impurities content<1ppm is 6N, particularly very strict to the content requirement of P and B element, (B<0.4ppm, P<0.7ppm), in the purifying technique process, two kinds of elements of P and B, due to the singularity of its chemical property, reach the solar-grade polysilicon requirement and bring very big difficulty to technique.Use in the world at present the very little of this technology of Physical technological breakthrough.
Summary of the invention
The technical problem that the present invention will solve is, a kind of equipment of preparing polycrystalline silicon through physical phosphorous removal is provided, and this equipment utilization Physical purification techniques obtains solar-grade polysilicon.
For this technical problem, technical solution provided by the invention is, a kind of equipment of preparing polycrystalline silicon through physical phosphorous removal is provided, by agitator arm, elevating lever, the connecting fiber mouth, stir pallet, drive unit, crucible and refining furnace form, described elevating lever connects the bell of refining furnace, and can drive and move up and down on bell by drive unit, described drive unit is arranged on bell near the elevating lever place, described elevating lever is connected by the connecting fiber mouth with agitator arm, connect and stir pallet in the lower end of agitator arm, making to stir pallet is suspended in the middle of crucible, described stirring pallet is circular, a plurality of 1～2mm micropores distribute on the pallet face.
Another technical problem to be solved by this invention is that a kind of method of utilizing equipment of the present invention to prepare polysilicon is provided.
For this technical problem, technical solution of the present invention is, a kind of method for preparing polysilicon is provided, utilize the flow characteristics that silicon liquid is good, the crucible that Pure Silicon Metal is housed is arranged in airtight high temperature refining furnace, under certain furnace pressure, the heat fused Pure Silicon Metal is to liquid state, utilize the stirring pallet to make silicon liquid form interior flowing, continue to change silicon liquid surface diffusion area simultaneously, make the phosphorus of silicon liquid inside constantly by silicon liquid surface, continue steam raising, and the phosphorus of gasification is constantly cemented out, the content of phosphorus is reduced to below 0.7ppm, meet the solar-grade polysilicon requirement, its concrete steps are as follows:
1) select high-test metal silicon, its granularity requirements is at 1～3 centimetre, and cleans and dry with deionized water, Pure Silicon Metal evenly put in crucible, and charged crucible is arranged in the high temperature refining furnace;
2) crucible is slowly heated up and is heated to silicon running down state, holding temperature to 1450～1550 degree, open the furnace inner environment gas ventilator and maintain the negative pressure state of furnace pressure at 1000～3000 handkerchiefs;
3) descend and stir pallet to silicon liquid, because silicon liquid flowing property is good, dephosphorization prepares the equipment of polysilicon when stirring, and it is relatively mobile that silicon liquid forms silicon liquid inside by the pallet micropore, makes silicon liquid surface form ripple simultaneously, make the phosphorus of silicon liquid inside constantly evaporate gasification, and constantly displace furnace inner environment gas, and make phosphorus constantly out replaced, maintain this state operation and stop after three hours stirring, directed cooling under the high purity inert gas environment, complete dephosphorization work.
During operation, fill with silicon liquid in crucible, drive unit drives stirring pallet above-below direction by agitator arm and repeatedly moves, and is stirred, and its agitation stroke is set in apart from silicon liquid bottom 5cm, apart from silicon liquid surface 10cm.
Beneficial effect:
The present invention utilizes the flow characteristics that silicon liquid is good, and process is simple, and efficiency is high, and energy-conserving and environment-protective simultaneously, can make the content of phosphorus be reduced to below 0.7PPm, meets the solar-grade polysilicon requirement.
The accompanying drawing explanation
The equipment drawing that Fig. 1 is preferred embodiment of the present invention.
Embodiment
Below give an actual example and describe the present invention.
At the equipment of a kind of preparing polycrystalline silicon through physical phosphorous removal as shown in figure mono-, by agitator arm 5, elevating lever 1, connecting fiber mouth 4, stirring pallet 6, drive unit 2, crucible 8 and refining furnace, formed.Wherein, elevating lever 1 connects the bell of refining furnace, and driven by drive unit 2, on bell, move up and down, described drive unit 2 is arranged on close elevating lever 1 place on bell, and described elevating lever 1 is connected by connecting fiber mouth 4 with agitator arm 5, the lower end of agitator arm 5 connects stirs pallet 6, make to stir pallet 6 and be suspended in the middle of crucible 8, described stirring pallet 6 is circular, and a plurality of 1～2mm micropores distribute on the pallet face of stirring pallet 6.
Embodiment mono-:
Select 20 kilograms of the Pure Silicon Metals of pre-treatment phosphorus content 3ppm, it is crushed to granularity at 2 centimetres.Then clean in the hot water of 100 ℃ with deionized water, after cleaning, be filtered dry and put into baking oven, Temperature Setting is dried the silicon material 160 ℃ of left and right.Silicon material after drying is positioned in crucible 8 equably, and is fixed in refining furnace, cover bell 3 and make in stove to keep sealed state.
Increase gradually power the silicon material is heated, until in crucible, the silicon material is to the fine melt state, the temperature that records silicon liquid 7 is 1550 ℃, and it is temperature-resistant in stove that temperature power keeps.Be filled with rare gas element in stove, make in stove form negative pressure state (pressure setting is at 3000 handkerchiefs) and maintain.The decline dephosphorization prepares the equipment of polysilicon to silicon liquid 7, dephosphorization prepares the equipment above-below direction mobile stirring repeatedly of polysilicon, the agitation stroke that stirs pallet 6 is set in apart from 5 centimetres of silicon liquid 7 bottoms and apart between 10 centimetres, silicon liquid 7 surface, stir and slowly carry out, the ambassador's silicon liquid 7 that prevents from moving splashes.Under whipping appts constantly stirs, the phosphorus in silicon liquid 7 constantly evaporates gasification, and by the rare gas element be filled with, it is cemented out, and stirs after three hours and stops stirring, directed cooling under the high purity inert gas environment.
The peak power that the equipment of a kind of preparing polycrystalline silicon through physical phosphorous removal in the present embodiment is used is 50KW, and after purifying, in silicon, phosphorus content can be down to 0.5pmm, meets the solar-grade polysilicon requirement.
Embodiment bis-:
Select 20 kilograms of the Pure Silicon Metals of pre-treatment phosphorus content 2ppm, it is crushed to granularity at 1 centimetre.Then clean in the hot water of 100 ℃ with deionized water, after cleaning, be filtered dry and put into baking oven, Temperature Setting is dried the silicon material 160 ℃ of left and right.Silicon material after drying is positioned in crucible 8 equably, and is fixed in refining furnace, cover bell 3 and make in stove to keep sealed state.
Increase gradually power the silicon material is heated, until in crucible, the silicon material is to the fine melt state, the temperature that records silicon liquid is 1500 ℃, and it is temperature-resistant in stove that temperature power keeps.Be filled with rare gas element in stove, make in stove form negative pressure state (pressure setting is at 2000 handkerchiefs) and maintain.The decline dephosphorization prepares the equipment of polysilicon to silicon liquid 7, dephosphorization prepares the equipment above-below direction mobile stirring repeatedly of polysilicon, agitation stroke is set in apart from 5 centimetres of silicon liquid 7 bottoms and apart between 10 centimetres, silicon liquid 7 surface, stirs and slowly carries out, and the ambassador's silicon liquid 7 that prevents from moving splashes.Under whipping appts constantly stirs, the phosphorus in silicon liquid constantly evaporates gasification, and by the rare gas element be filled with, it is cemented out, and stirs after three hours and stops stirring, directed cooling under the high purity inert gas environment.
The peak power that the equipment of a kind of preparing polycrystalline silicon through physical phosphorous removal in the present embodiment is used is 50KW, and after purifying, in silicon, phosphorus content can be down to 0.4pmm, meets the solar-grade polysilicon requirement.
Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (2)
1. the equipment of a preparing polycrystalline silicon through physical phosphorous removal, it is characterized in that, by agitator arm, elevating lever, connecting fiber mouth, stirring pallet, drive unit, crucible and refining furnace, formed, described elevating lever connects the bell of refining furnace, and can drive and move up and down on bell by drive unit, described drive unit is arranged on bell near the elevating lever place, described elevating lever is connected by the connecting fiber mouth with agitator arm, connect and stir pallet in the lower end of agitator arm, making to stir pallet is suspended in the middle of crucible, described stirring pallet is circular, and a plurality of 1～2mm micropores distribute on the pallet face.
2. a method of utilizing equipment claimed in claim 1 to prepare polysilicon, it is characterized in that, utilize the flow characteristics that silicon liquid is good, the crucible that Pure Silicon Metal is housed is arranged in airtight high temperature refining furnace, under certain furnace pressure, the heat fused Pure Silicon Metal is to liquid state, utilize the stirring pallet to make silicon liquid form interior flowing, continue to change silicon liquid surface diffusion area simultaneously, make the phosphorus of silicon liquid inside constantly by silicon liquid surface, continue steam raising, and the phosphorus of gasification is constantly cemented out, the content of phosphorus is reduced to below 0.7ppm, meet the solar-grade polysilicon requirement,
Its concrete steps are as follows:
1) select high-test metal silicon, its granularity requirements is at 1～3 centimetre, and cleans and dry with deionized water, Pure Silicon Metal evenly put in crucible, and charged crucible is arranged in the high temperature refining furnace;
2) crucible is slowly heated up and is heated to silicon running down state, holding temperature to 1450～1550 degree, open the furnace inner environment gas ventilator and maintain the negative pressure state of furnace pressure at 1000～3000 handkerchiefs;
3) descend and stir pallet to silicon liquid, because silicon liquid flowing property is good, dephosphorization prepares the equipment of polysilicon when stirring, and it is relatively mobile that silicon liquid forms silicon liquid inside by the pallet micropore, makes silicon liquid surface form ripple simultaneously, make the phosphorus of silicon liquid inside constantly evaporate gasification, and constantly displace furnace inner environment gas, and make phosphorus constantly out replaced, maintain this state operation and stop after three hours stirring, directed cooling under the high purity inert gas environment, complete dephosphorization work.
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| CN201010286544.0A CN101948113B (en) | 2010-09-19 | 2010-09-19 | Method and equipment for preparing polycrystalline silicon through physical phosphorous removal |
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| CN201010286544.0A CN101948113B (en) | 2010-09-19 | 2010-09-19 | Method and equipment for preparing polycrystalline silicon through physical phosphorous removal |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5182091A (en) * | 1990-05-30 | 1993-01-26 | Kawasaki Steel Corporation | Method and apparatus for purifying silicon |
| JP2905353B2 (en) * | 1993-02-04 | 1999-06-14 | 川崎製鉄株式会社 | Purification method of metallic silicon |
| CN101343063A (en) * | 2008-08-13 | 2009-01-14 | 厦门大学 | Purification apparatus and method for solar energy level polysilicon |
| CN101628718A (en) * | 2008-07-16 | 2010-01-20 | 佳科太阳能硅(厦门)有限公司 | Method for removing impurity of phosphorus from metallurgical grade silicon |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201295600Y (en) * | 2008-10-30 | 2009-08-26 | 北京爱博生生物技术有限公司 | Blending device |
| CN101748481B (en) * | 2008-12-11 | 2013-08-21 | 浙江昱辉阳光能源有限公司 | Method for purifying polycrystalline silicon material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5182091A (en) * | 1990-05-30 | 1993-01-26 | Kawasaki Steel Corporation | Method and apparatus for purifying silicon |
| JP2905353B2 (en) * | 1993-02-04 | 1999-06-14 | 川崎製鉄株式会社 | Purification method of metallic silicon |
| CN101628718A (en) * | 2008-07-16 | 2010-01-20 | 佳科太阳能硅(厦门)有限公司 | Method for removing impurity of phosphorus from metallurgical grade silicon |
| CN101343063A (en) * | 2008-08-13 | 2009-01-14 | 厦门大学 | Purification apparatus and method for solar energy level polysilicon |
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