CN203440097U - Device for preparing polycrystalline silicon through coupling of electron-beam smelting technology and directional solidification technology - Google Patents
Device for preparing polycrystalline silicon through coupling of electron-beam smelting technology and directional solidification technology Download PDFInfo
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- CN203440097U CN203440097U CN201320531120.5U CN201320531120U CN203440097U CN 203440097 U CN203440097 U CN 203440097U CN 201320531120 U CN201320531120 U CN 201320531120U CN 203440097 U CN203440097 U CN 203440097U
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Abstract
The utility model relates to a device for preparing polycrystalline silicon through coupling of an electron-beam smelting technology and a directional solidification technology. The device comprises a furnace body, and is characterized in that an electron beam smelting component and a directional solidification component are arranged in the furnace body; the electron beam smelting component comprises a melting crucible with water cooling is arranged at the upper part in the furnace body; a concave melting tank is arranged on one side of the melting crucible; a flow guiding area inclining downwards is formed from a port of the melting tank and the other side of the melting crucible; the top, located above the melting crucible, of the furnace body is communicated with an electronic gun for melting and an electronic gun for smelting; the furnace body side wall located on one side of the melting tank of the melting crucible is communicated with a feeding mechanism; a discharging port of the feeding mechanism is located above the melting tank; the directional solidification component comprises a solidification crucible located at the lower part of the furnace body, and the solidification crucible is surrounded by a graphite heater and a heat preservation sleeve outwards sequentially; and a water-cooling ingot-pulling rotation mechanism communicated with the bottom of the furnace body is arranged at the bottom of the solidification crucible. According to the device, phosphorus impurity elements in silicon can be removed more efficiently; and at the same time, the total energy consumption in a production process is reduced.
Description
Technical field
The utility model belongs to polycrystalline silicon purifying field, is specifically related to the device that polysilicon is prepared in a kind of electron beam melting and directional solidification technique coupling.
Background technology
At present, China has become world energy sources production and consumption big country, but energy expenditure level is also very low per capita.Along with economical and social development, China's energy demand is by sustainable growth, for current energy shortage situation, deep thinking is all being carried out in countries in the world, and effort improves efficiency of energy utilization, promote the development and application of renewable energy source, reduce the dependence to Imported oil, strengthen energy security.
Solar energy power generating development in recent years as one of important development direction of renewable energy source is swift and violent, and its proportion is increasing.According to < < renewable energy source Long-and Medium-term Development planning > >, to the year two thousand twenty, China strives making solar electrical energy generation installed capacity to reach 1.8GW(gigawatt), will reach 600GW to the year two thousand fifty.Expect the year two thousand fifty, the electric power installation of Chinese renewable energy source will account for 25% of national electric power installation, and wherein photovoltaic generation installation will account for 5%.Before estimating the year two thousand thirty, the compound growth rate of Chinese sun power installed capacity will be up to more than 25%.
The development of photovoltaic industry depends on the purification to polycrystalline silicon raw material.The purifying technique of polycrystalline silicon raw material is several technique below main dependence at present: Siemens Method, silane thermal decomposition process, gas fluidized bed method and metallurgy method.Metallurgy method is prepared solar-grade polysilicon technology as the only way which must be passed of development low cost, eco-friendly solar-grade polysilicon technology of preparing, has obtained at present tremendous development, and has realized suitability for industrialized production.Metallurgy method purifying polycrystalline silicon refers to the physical metallurgy means that adopt, in the situation that silicon does not participate in chemical reaction occurs, remove successively the method for the various impurity elements (phosphorus, boron and metal) in silicon, it is not single preparation method, but a kind of Integration Method mainly utilizes saturated vapor pressure principle, segregation principle and oxidisability difference principle, adopts respectively different processing methodes, the impurity element of making a return journey in silica removal, thus be met the silicon material of solar energy polycrystalline silicon purity requirement.For example, utilize medium smelting technique to remove the boron impurity in silicon, utilize directional freeze to remove the metallic impurity in silicon, utilize electron beam melting technology to remove the phosphorus impurities in silicon, three kinds of melting technologies are integrated into an operational path, through three kinds of technological processs, thereby obtain solar-grade polysilicon.
Electron beam melting technology, as the important component part in metallurgy method technical process, can effectively remove the high saturated vapor pressure impurity in silicon, as phosphorus.Directional solidification technique is mainly applied segregation principle, the metallic impurity elements of the low segregation coefficient in silica removal of making a return journey.But at present, in metallurgy method technological process, electron beam melting technology and directional solidification technique are two independently links, generally by the silicon material after directional freeze, after fragmentation, cleaning process, resulting silicon material is put into electron beam equipment again and is carried out melting again, the phosphorus impurities of making a return journey in silica removal, or first carry out electron beam melting and carry out again directional freeze.But in this flow process, directional freeze relates to fusing and the process of setting of silicon material, directional freeze relates to fusing and the process of setting of silicon material equally, simultaneously, silicon material after back is processed, needs to carry out next step through fragmentation, cleaning, drying course again, has increased whole investment, meanwhile, the production efficiency of whole flow process is lower.
Utility model content
According to above the deficiencies in the prior art, the purpose of this utility model is the device that polysilicon is prepared in a kind of electron beam melting of proposition and directional solidification technique coupling, by by electron beam melting and the effective combination of directional freeze, remove more efficiently phosphorus impurities and metallic impurity in silicon, meanwhile, reduce the total energy consumption in production process.
The device of polysilicon is prepared in electron beam melting described in the utility model and directional solidification technique coupling, comprises body of heater, is provided with electron beam melting assembly and directional freeze assembly in body of heater, wherein:
Electron beam melting assembly comprises the fusion crucible with water-cooled that is positioned at body of heater internal upper part, and this fusion crucible one side is with spill melting pool, and melting pool mouth to the opposite side of fusion crucible is downward-sloping water conservancy diversion region; Lead at the body of heater top that is positioned at fusion crucible top electron beam gun and melting electron beam gun for fusing, and the sidewall of the furnace body that is positioned at melting pool one side of fusion crucible leads to feed mechanism, and the discharge port of this feed mechanism is positioned at above melting pool;
Directional freeze assembly comprises the solidification crucible that is positioned at lower portion of furnace body, solidification crucible outwards surrounds successively and is provided with graphite heater and insulation sleeve, solidification crucible bottom is provided with the water-cooled of leading to bottom of furnace body and draws ingot rotating mechanism, wherein, this solidification crucible is positioned at the below of the mouth that comes down in torrents in water conservancy diversion region, and under the mouth that comes down in torrents, corresponding insulation sleeve place, position offers through hole.
Wherein, fusion crucible is preferably the copper crucible with water-cooled.Adopting copper crucible is the thermal conductivity that fully takes into account copper product self excellence, thereby preventing that beam energy is too high causes damage to fusion crucible.
Solidification crucible is preferably quartz crucible.For solidification crucible itself, can adopt plumbago crucible, also can adopt quartz crucible, but plumbago crucible foreign matter content is higher, can again to silicon material, pollute, if at plumbago crucible surface spraying coating, can increase production cost.
In water conservancy diversion region, preferably offer diversion groove, increase diversion groove and can make silicon liquid flow direction more concentrated, be convenient to melting with electron beam gun to its electron beam melting.
Working process of the present utility model is as follows: electron beam melting furnace is vacuumized, then by feed mechanism, in the fusion crucible with water-cooled, continue feeding, by fusing, with electron beam gun, silicon material is melted, when ever-increasing silicon liquid reaches fusion crucible mouth, mode by water conservancy diversion flow into the solidification crucible in electron beam melting furnace, wherein, silicon liquid carries out electron beam melting by melting with electron beam gun in water conservancy diversion region, in solidification crucible, by water-cooled, draws ingot rotating mechanism to carry out directional freeze.
Specifically according to following steps, carry out:
(1) get the raw materials ready: the silicon material after electron beam melting and directional freeze are purified is put into solidification crucible inner bottom part as solidifying bed material; The silicon material for the treatment of electron beam melting and directional freeze is put into feed mechanism, and put into fusion crucible bottom as fusing bed material;
(2) pre-treatment: open cooling water circulation to electron beam melting furnace, fusion crucible and water-cooled ingot pulling mechanism, to vacuumizing processing in electron beam melting furnace, be evacuated to below 0.005Pa, and fusing is vacuumized to processing with electron beam gun and melting with electron beam gun, be evacuated to below 0.0005Pa, then carry out preheating, heater current is set to 800mA, after preheating 15min, close preheating button;
(3) purify: open the graphite heater of solidification crucible periphery, the bed material that solidifies in solidification crucible is melted, open electron beam gun and melting electron beam gun for fusing, setting power is 250kw, open the electron beam transmitting of electron beam gun for fusing, controlled melting distributes by the beam energy of electron beam gun, make the fusing bed material in fusion crucible be fused into silicon liquid, then start feed mechanism, continue to add silicon material in fusion crucible, when the silicon liquid liquid level of fusing formation rises to fusion crucible mouth, enter water conservancy diversion region, now open the electron beam transmitting of electron beam gun for melting, controlling melting distributes by the beam energy of electron beam gun, silicon liquid in water conservancy diversion region is carried out to electron beam melting purification, finally by flowing into after water conservancy diversion in solidification crucible, the cold drawn ingot rotating mechanism of open water when silicon liquid flows into solidification crucible, thus solidification crucible rotation is moved downward away from graphite heater, realize the directional freeze of silicon liquid, when solidification crucible reaches after bearing capacity, close feed mechanism, close electron beam gun and melting electron beam gun for fusing, silicon liquid in solidification crucible all solidifies long crystalline substance finish after, close water-cooled and draw ingot rotating mechanism, close graphite heater power supply, through cooling to below 200 ℃, close vacuum system, to blow-on after inflation in electron beam melting furnace, take out solidification crucible, thus the silicon ingot after obtaining electron beam melting and directional freeze and purifying.
Wherein, in the unit time in step (3), the long crystalline substance that solidifies in solidification crucible is measured preferably consistent with the feeding amount of feed mechanism.
In the utility model, broken traditional electron beam melting pattern, in the melting pool of fusion crucible, only melt and preliminary electron beam melting, and in water conservancy diversion region, carry out concentrated electron beam melting, because silicon liquid can spread in water conservancy diversion region, fall apart, specific surface area increases, so electron beam melting better effects if, because water conservancy diversion region is downward-sloping structure, the silicon liquid after melting is purified flows in solidification crucible.In addition, the utility model well combines electron beam melting and directional freeze, and both can be completed in a stove, has omitted the process of once solidifying, and does not also need to carry out fragmentation, cleaning, drying course again.
The utility model has the advantage of: (1) and the melting of conditional electronic bundle and directional solidification processes to than, this device is coupled electron beam continuous smelting process and directional freeze process effectively, thereby realized the object that realizes two kinds of production technique on same equipment, energy expenditure while having greatly reduced independent production, total energy consumption reduces over 35%, production efficiency can improve 40% left and right, simultaneously, reduced fragmentation, cleaned and dried link, input and the floor space of saving relevant device.(2) after this device improves, electron beam melting and directional freeze refining effect are better, the silicon ingot phosphorus content that obtains of purifying lower than 0.000035%, total metal contents in soil is lower than 0.0001%.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
In figure: 1, body of heater 2, fusion crucible 3, electron beam gun 4 for fusing, for melting, electron beam gun 5, feed mechanism 6, solidification crucible 7, water-cooled are drawn ingot rotating mechanism 8, graphite heater 9, are incubated sleeve.
Embodiment
Below in conjunction with drawings and Examples, the utility model is described further.
Embodiment 1:
As shown in Figure 1, the device of polysilicon is prepared in electron beam melting and directional solidification technique coupling, comprises body of heater 1, is provided with electron beam melting assembly and directional freeze assembly in body of heater 1, wherein:
Electron beam melting assembly comprises the fusion crucible 2 with water-cooled that is positioned at body of heater 1 internal upper part, and these fusion crucible 2 one sides are with spill melting pool, and melting pool mouth to the opposite side of fusion crucible 2 is downward-sloping water conservancy diversion region; Lead at body of heater 1 top that is positioned at fusion crucible 2 tops electron beam gun 3 and electron beam gun 4 melting for for fusing, and body of heater 1 sidewall that is positioned at melting pool one side of fusion crucible 2 leads to feed mechanism 5, and the discharge port of this feed mechanism 5 is positioned at above melting pool;
Directional freeze assembly comprises the solidification crucible 6 that is positioned at body of heater 1 bottom, solidification crucible 6 outwards surrounds successively and is provided with graphite heater 8 and insulation sleeve 9, solidification crucible 6 bottoms are provided with the water-cooled of leading to body of heater 1 bottom and draw ingot rotating mechanism 7, wherein, this solidification crucible 6 is positioned at the below of the mouth that comes down in torrents in water conservancy diversion region, and under the mouth that comes down in torrents, corresponding insulation sleeve 9 places, position offer through hole.
Wherein, fusion crucible 2 is the copper crucible with water-cooled.Adopting copper crucible is the thermal conductivity that fully takes into account copper product self excellence, thereby preventing that beam energy is too high causes damage to fusion crucible 2.
Solidification crucible 6 is quartz crucible.Own for solidification crucible 6, can adopt plumbago crucible, also can adopt quartz crucible, but plumbago crucible foreign matter content is higher, can again to silicon material, pollute, if at plumbago crucible surface spraying coating, can increase production cost.
Water conservancy diversion offers diversion groove in region, increases diversion groove and can make silicon liquid flow direction more concentrated, is convenient to melting and uses electron beam gun 4 to its electron beam melting.
Embodiment 2:
Device described in employing embodiment 1, carries out electron beam melting and polysilicon is prepared in directional solidification technique coupling, according to following steps, carries out:
(1) get the raw materials ready: 500kg phosphorus, metal content are respectively to 0.005%, 0.5% silicon material, utilize cleaning equipment to clean, remove surperficial dust, oil stain, put into drying baker, at 80 ℃ of temperature, dry; Solidification crucible 6 is put into graphite heater 8, and the outer placing graphite sleeve 9 of graphite heater 8 is incubated; Silicon material after drying is put into respectively to feed mechanism 5 and fusion crucible 2, wherein, in fusion crucible 2, put 5kg, as melting bed material, the silicon material after electron beam melting and directional freeze are purified is put into solidification crucible 6 inner bottom parts as solidifying bed material simultaneously;
(2) pre-treatment: device is closed to stove, to electron beam melting furnace, fusion crucible 2 and water-cooled, draw ingot rotating mechanism 7 to open cooling water circulation, the vacuum system of unlocking electronic bundle smelting furnace, first utilize vacuum system mechanical pump and the lobe pump of electron beam melting furnace that vacuum in stove is evacuated to below 10Pa, then start diffusion pump, vacuum in stove is evacuated to below 0.005Pa.Meanwhile, start fusing and with electron beam gun 3 and melting, use mechanical pump, lobe pump and the molecular pump of the vacuum system of electron beam gun 4, fusing is evacuated to below 0.0005Pa by electron beam gun 4 vacuum with electron beam gun 3 and melting, then carry out preheating, heater current is set to 800mA, after preheating 15min, close preheating button;
(3) purify: open the power supply of graphite heater 8, slowly increase power to 100kw, the bed material that solidifies in solidification crucible 6 is melted, open to melt and use electron beam gun 3 and electron beam gun 4 for melting, setting power is 250kw, slowly increase power to 250kw, open the electron beam transmitting of electron beam gun 3 for fusing, controlled melting distributes by the beam energy of electron beam gun 3, make the fusing bed material in fusion crucible 2 be fused into silicon liquid, after fusing 10min, then start feed mechanism 5, according to the filler speed of 2.5kg/min, continue to add silicon material in fusion crucible 2, when the silicon liquid liquid level of fusing formation rises to melting pool mouth, enter the diversion groove in water conservancy diversion region, now open the electron beam transmitting of electron beam gun 4 for melting, controlling melting distributes by the beam energy of electron beam gun 4, silicon liquid in water conservancy diversion region is carried out to electron beam melting purification, thereby effectively remove the volatile impunty elements such as phosphorus in silicon liquid, finally by flowing into after water conservancy diversion in solidification crucible 6, the cold drawn ingot rotating mechanism 7 of open water when silicon liquid flows into solidification crucible 6, thereby solidification crucible 6 rotations are moved downward away from graphite heater 8, lowering speed is 1mm/min, speed of rotation is 1r/min, thereby the brilliant amount of length of solidifying in guarantor unit's time in solidification crucible 6 is consistent with the feeding amount of feed mechanism 5, realize the directional freeze of silicon liquid, when solidification crucible 6 reaches after bearing capacity, close feed mechanism 5, silicon material stops carrying, and silicon liquid stops flowing, and closes electron beam gun 3 and electron beam gun 4 melting for for fusing, and the interior remaining silicon liquid of fusion crucible 2 solidifies the rear fusing bed material use as producing next time, silicon liquid in solidification crucible 6 all solidifies long crystalline substance finish after, close water-cooled and draw ingot rotating mechanism 7, close graphite heater 8 power supplys, through 3h, cool to 100 ℃, close vacuum system, to blow-on after inflation in electron beam melting furnace, take out solidification crucible 6, thus the silicon ingot after obtaining electron beam melting and directional freeze and purifying.After testing, the phosphorus content of the silicon ingot obtaining is 0.000028%, and total metals content impurity is 0.00008%.
Claims (4)
1. a device for polysilicon is prepared in electron beam melting and directional solidification technique coupling, comprises body of heater, it is characterized in that being provided with electron beam melting assembly and directional freeze assembly in body of heater, wherein:
Electron beam melting assembly comprises the fusion crucible with water-cooled that is positioned at body of heater internal upper part, and this fusion crucible one side is with spill melting pool, and melting pool mouth to the opposite side of fusion crucible is downward-sloping water conservancy diversion region; Lead at the body of heater top that is positioned at fusion crucible top electron beam gun and melting electron beam gun for fusing, and the sidewall of the furnace body that is positioned at melting pool one side of fusion crucible leads to feed mechanism, and the discharge port of this feed mechanism is positioned at above melting pool;
Directional freeze assembly comprises the solidification crucible that is positioned at lower portion of furnace body, solidification crucible outwards surrounds successively and is provided with graphite heater and insulation sleeve, solidification crucible bottom is provided with the water-cooled of leading to bottom of furnace body and draws ingot rotating mechanism, wherein, this solidification crucible is positioned at the below of the mouth that comes down in torrents in water conservancy diversion region, and under the mouth that comes down in torrents, corresponding insulation sleeve place, position offers through hole.
2. the device of polysilicon is prepared in electron beam melting according to claim 1 and directional solidification technique coupling, it is characterized in that fusion crucible is the copper crucible with water-cooled.
3. the device of polysilicon is prepared in electron beam melting according to claim 1 and directional solidification technique coupling, it is characterized in that solidification crucible is quartz crucible.
4. the device of polysilicon is prepared in electron beam melting according to claim 1 and directional solidification technique coupling, it is characterized in that offering diversion groove in water conservancy diversion region.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420380A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology |
| CN104178810A (en) * | 2014-09-01 | 2014-12-03 | 大连理工大学 | Electron-beam melting device and method for preparing boron mother alloy by using same |
| CN104195637A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Electric beam melting device and method for preparing boron master alloy |
| CN104445903A (en) * | 2014-11-25 | 2015-03-25 | 大连理工大学 | Electric beam melting and directional solidification combined device for polycrystalline silicon powder and method |
| CN104178810B (en) * | 2014-09-01 | 2017-01-04 | 大连理工大学 | A kind of electron beam melting apparatus and utilize the method that this device prepares boron foundry alloy |
| CN109112618A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification growth device and method of solar energy polycrystalline silicon |
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2013
- 2013-08-28 CN CN201320531120.5U patent/CN203440097U/en not_active Withdrawn - After Issue
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420380A (en) * | 2013-08-28 | 2013-12-04 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology |
| CN103420380B (en) * | 2013-08-28 | 2015-06-03 | 青岛隆盛晶硅科技有限公司 | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology |
| CN104178810A (en) * | 2014-09-01 | 2014-12-03 | 大连理工大学 | Electron-beam melting device and method for preparing boron mother alloy by using same |
| CN104195637A (en) * | 2014-09-01 | 2014-12-10 | 大连理工大学 | Electric beam melting device and method for preparing boron master alloy |
| CN104178810B (en) * | 2014-09-01 | 2017-01-04 | 大连理工大学 | A kind of electron beam melting apparatus and utilize the method that this device prepares boron foundry alloy |
| CN104195637B (en) * | 2014-09-01 | 2017-02-15 | 大连理工大学 | Electric beam melting device and method for preparing boron master alloy |
| CN104445903A (en) * | 2014-11-25 | 2015-03-25 | 大连理工大学 | Electric beam melting and directional solidification combined device for polycrystalline silicon powder and method |
| CN104445903B (en) * | 2014-11-25 | 2017-04-12 | 大连理工大学 | Electric beam melting and directional solidification combined device for polycrystalline silicon powder and method |
| CN109112618A (en) * | 2017-06-23 | 2019-01-01 | 镇江仁德新能源科技有限公司 | A kind of directional solidification growth device and method of solar energy polycrystalline silicon |
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