The device of solar-grade polysilicon is prepared in electron beam serialization melting
Technical field
The utility model belongs to polycrystalline silicon purifying field, is specifically related to the device that solar-grade polysilicon is prepared in a kind of electron beam serialization melting.
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.But at present, typical electron beam melting technique is single stove melting, in smelting pot, add raw material, under vacuum condition, utilize electron beam to carry out melting, in fusion process, remove the phosphorus impurities in silicon, after melting certain hour, close electron beam, carry out solidifying of silicon material, cooling after, low-phosphorous polycrystalline silicon ingot casting is taken out in blow-on.Or employing Dumpage type melting method, utilize charging mechanism to add certain mass silicon raw material in smelting pot, utilize electron beam melting, after melting completes, silicon liquid is poured in solidification crucible, after toppling over, smelting pot is resetted, re-use charging mechanism and add raw material in smelting pot, again carry out melting, toppling process, repeatedly carry out repeatedly, after solidification crucible is filled with, stop fusion process, carry out cooling, finally be met the polycrystalline silicon ingot casting of purity requirement, this remains the method for a kind of electron beam list stove melting in fact.Due to current this technique, relate to silicon material interpolation, topple over, the process such as fusing repeatedly, reduced production efficiency, cause a large amount of power losses simultaneously.
Utility model content
According to above the deficiencies in the prior art, the utility model proposes the device that solar-grade polysilicon is prepared in a kind of electron beam serialization melting, can remove more efficiently the phosphorus impurities element in silicon, meanwhile, reduce the total energy consumption in production process.
The device of solar-grade polysilicon is prepared in electron beam serialization melting described in the utility model, comprise body of heater, body of heater internal upper part is provided with the fusion crucible of water-cooled, 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; Mouthful bottom of furnace body of below that comes down in torrents in water conservancy diversion region is provided with solidification crucible.
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 the copper crucible with water-cooled.For solidification crucible itself, can adopt plumbago crucible, also can adopt quartz crucible, but when casting, easily broken, utilize the copper crucible with water-cooled, its cooling power is stronger, cooling time is shorter, simultaneously can Reusability, and holistic cost is lower.And it is not fragile.
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, in water conservancy diversion region, by melting, with electron beam gun, carry out electron beam melting, after solidification crucible reaches bearing capacity, stop feed mechanism feeding, close electron beam gun and melting electron beam gun for fusing, silicon ingot in solidification crucible is taken out.
Specifically according to following steps, carry out:
(1) get the raw materials ready: the silicon material after electron beam melting is purified is put into solidification crucible inner bottom part as solidifying bed material; The silicon material for the treatment of electron beam melting 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 and fusion crucible, 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;
(3) melting is purified: 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, after solidification crucible reaches bearing capacity, stop feed mechanism feeding, close electron beam gun and melting electron beam gun for fusing, through cooling to below 200 ℃, close vacuum system, to blow-on after inflation in electron beam melting furnace, take out the silicon ingot in solidification crucible.
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 loose in water conservancy diversion region, specific surface area increases, so electron beam melting better effects if, because water conservancy diversion region is downward-sloping structure, silicon liquid after melting is purified flows in solidification crucible, in solidification crucible, pile up, generally select the solidification crucible of large-size, facilitate once electron beam melting technology to reach larger single furnace output.
The utility model has the advantage of: compare with conditional electronic bundle melting technology, this device has been realized the object of serialization melting polysilicon, in fusion process, realize the object of serialization dephosphorization, and electron beam melting refining effect is better, the silicon ingot phosphorus content obtaining is lower than 0.000035%.Adopt this device, production efficiency can improve 20% left and right, and the energy expenditure in whole production process reduces more than 20%.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
In figure: 1, body of heater 2, fusion crucible 3, fusing electron beam gun 4, electron beam gun 5, feed mechanism 6, solidification crucible for melting.
Embodiment
Below in conjunction with drawings and Examples, the utility model is described further.
Embodiment 1:
As shown in Figure 1, the device of solar-grade polysilicon is prepared in electron beam serialization melting, comprises body of heater 1, and body of heater 1 internal upper part is provided with the fusion crucible 2 of water-cooled, 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; Mouthful body of heater 1 bottom of below of coming down in torrents in water conservancy diversion region is provided with solidification crucible 6.
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 the copper crucible with water-cooled.Own for solidification crucible 6, can adopt plumbago crucible, also can adopt quartz crucible, but when casting, easily broken, utilize the copper crucible with water-cooled, its cooling power is stronger, cooling time is shorter, simultaneously can Reusability, and holistic cost is lower.And it is not fragile.
Water conservancy diversion offers diversion groove in region, increases diversion groove and can make silicon liquid flow direction more concentrated, and meanwhile, silicon liquid is more shallow in diversion trench, and specific surface area increases, so electron beam melting better effects if, 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 serialization melting and prepares solar-grade polysilicon, according to following steps, carries out:
(1) get the raw materials ready: the silicon material that is 0.005% by 500kg phosphorus content, utilize cleaning equipment to clean, remove surperficial dust, oil stain, put into drying baker, at 80 ℃ of temperature, dry.Silicon material after drying is put into respectively to hopper and the fusion crucible 2 of feed mechanism 5, wherein, in fusion crucible 2, put 5kg, as fusing bed material, simultaneously putting into the silicon material after electron beam melting is purified of 10kg in solidification crucible 6, as solidifying bed material;
(2) pre-treatment: device is closed to stove, to electron beam melting furnace, fusion crucible 2 and solidification crucible 6, 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;
(3) melting is purified: 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, finally by flowing into after water conservancy diversion in solidification crucible 6, after solidification crucible 6 reaches bearing capacity, stop feed mechanism 5 feedings, close to melt and use electron beam gun 3 and electron beam gun 4 for melting, through cooling to 200 ℃, close vacuum system, to blow-on after inflation in electron beam melting furnace, take out the silicon ingot in solidification crucible 6, thereby obtain the silicon ingot after electron beam melting is purified.The phosphorus content of the silicon ingot obtaining after testing, is 0.000028%.