CN101481112B - Direct oxidation refining purification method for industrial silicon melt - Google Patents
Direct oxidation refining purification method for industrial silicon melt Download PDFInfo
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- CN101481112B CN101481112B CN2009100940783A CN200910094078A CN101481112B CN 101481112 B CN101481112 B CN 101481112B CN 2009100940783 A CN2009100940783 A CN 2009100940783A CN 200910094078 A CN200910094078 A CN 200910094078A CN 101481112 B CN101481112 B CN 101481112B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 73
- 239000010703 silicon Substances 0.000 title claims abstract description 73
- 238000007670 refining Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 230000003647 oxidation Effects 0.000 title claims description 6
- 238000007254 oxidation reaction Methods 0.000 title claims description 6
- 238000000746 purification Methods 0.000 title 1
- 239000012535 impurity Substances 0.000 claims abstract description 34
- 229910052796 boron Inorganic materials 0.000 claims abstract description 16
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 11
- 239000008247 solid mixture Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 10
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- 241000209456 Plumbago Species 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- -1 boron oxide compound Chemical class 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 9
- XUKUURHRXDUEBC-SXOMAYOGSA-N (3s,5r)-7-[2-(4-fluorophenyl)-3-phenyl-4-(phenylcarbamoyl)-5-propan-2-ylpyrrol-1-yl]-3,5-dihydroxyheptanoic acid Chemical compound C=1C=CC=CC=1C1=C(C=2C=CC(F)=CC=2)N(CC[C@@H](O)C[C@H](O)CC(O)=O)C(C(C)C)=C1C(=O)NC1=CC=CC=C1 XUKUURHRXDUEBC-SXOMAYOGSA-N 0.000 abstract description 5
- 238000007664 blowing Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract 2
- 229910002804 graphite Inorganic materials 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 19
- 229910052742 iron Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 229910004762 CaSiO Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a directly oxidizing refining and purifying method for industrial silicon melt, which comprises the following steps: adding melt state industrial silicon into a graphite crucible of a heating converting furnace through a pouring box, keeping the temperature of the silicon melt between 1450 and 1600 DEG C by adopting the intermediate sensing heating way, blowing the gas-solid mixture of compressed air and SiO2-CaO slag oxidant powder into the silicon melt to be oxidized and refined, removing most part of metallic impurity Al, Ca, Ti and the like and a small amount of impurity element B; and then closing the compressed air, blowing oxidized gas H2O steam, removing the residual metallic impurity and non-metallic impurity B; and finally, blowing H2 to remove the impurity element P in silicon. The invention achieves the purposes of reducing metallic impurity in the silicon to be less than 1.0 ppmw, reducing the non-metallic impurities B and P respectively to be less than 0.2 ppmw and 0.5 ppmw, and increasing the t electric resistivity to be larger than 2.5 Omega*cm.
Description
One, technical field
The present invention relates to the method that a kind of industrial silicon melt direct oxidation refining is purified, belong to metallurgical method purifying industrial silicon materials technical field.
Two, background technology
Mainly contain metallic impurity such as Fe, Al, Ca and B, P, nonmetallic impuritys such as C, O in the industrial silicon (MG-Si), purity is generally more than 98%, and the total content of impurity is usually above 10000ppm; The purity requirement of solar energy level silicon (SoG-Si) is 5N～7N, in order to ensure desired photoelectric transformation efficiency, content of impurities is no more than 50ppmw in the silicon, and metallic impurity such as Fe, Al, Ca are below the 5.0ppmw usually, B, P impurity are lower than 1.0ppmw, and C, O etc. is below the 5.0ppmw.For solar energy level silicon is used widely, must adopt low-cost and large batch of production technique.
2007, global solar photovoltaic product reached 4000MW, expect the year two thousand twenty after, will reach 18GW every year.At present, the solar level silicon materials do not form independently supply system, 90% derives from the waste material of electronic-grade silicon and the material end to end of silicon single crystal, can not satisfy the demand of solar cell industry fast development far away, and raw material supply has become the bottleneck of restriction photovoltaic industry development.The improvement Siemens Method is the production main method of solar cell silicon raw material, and output accounts for 78% of Gross World Product, but this technology is the U.S., Japan and the monopolization of major company of German a few family always, and China is carried out blockade on new techniques.Directional solidification method and high-temperature vacuum method of evaporation can effectively be removed segregation coefficient is little in the metallurgical grade silicon impurity element Fe, Al, Cu etc. and Volatile Elements P, but work hardly with not volatile impurity element to segregation coefficient is big, especially to impurity element B important in the silicon powerless (its segregation coefficient to silicon is 0.8).More external researchists begin to develop the method that other prepare solar energy level silicon.
People's (patent No. was authorized on March 2nd, 066523,2003) such as Japan FujiwaraH utilize SiO
2Content is higher than 45% slag and carries out the refining of metallurgical grade silicon, in order to obtain the slag of different melting points or viscosity, adds the used Al of similar refining steel in right amount
2O
3, MgO, BaO, CaF
2Deng additive, boron content is reduced to 1.6ppm from 7ppm.J.Diet publishes thesis (1988:599) on " Proc.8th E.C.Photovoltaic Solar Energy Conf. ", utilizes metallurgical grade silicon and the CaSiO of Fe4500ppm, Al600ppm, Cu185ppm, P18ppm, Ca150ppm, P45ppm
3Fe, Al, Cu and Ca content in the silicon all can be reduced to below the 1ppm, B, P content ease down to below the 1ppm, add CaSiO
3Slag refining meeting reduces Al in the silicon, B content, and Ca content raises, but by vacuum-evaporation and directional freeze refining, Fe, Cu, P, Ca content all can be reduced to the solar energy level silicon standard.
Sharp Corporation (patent No. 200580023743.X, in May, 2007 open) utilize contain can with water vapour and Ar (or the Ar and the H of impurity element reaction in the silicon
2) mixed gas contacts with molten silicon and react, and is blown into high-purity Si O by gas blow pipe in melt simultaneously
2Powder is when carrier gas is (Ar+4%H
2)+60%H
2O, slag are 45%SiO
2During+55%CaO, can make that boron content is reduced to 1.2ppm by 10ppm in the silicon.French and the Canadian Alemany C of joint laboratory " the Refining ofmetallurgical-grade silicon by inductive plasma " (2002 that on " Sol.Energy Mater.Sol.Cells ", publish thesis, 72 (1-4): 41-48), carry out blowing refining Deng the employing flame passes, this method all has good removal efficient to many impurity in the silicon, especially very obvious to the removal of elements such as Al, Ca, Fe, B, but the removal effect to element P is relatively poor, and this is because P is easy and Si forms nonvolatile Si
2P, SiP phase when having more Ca in the melt, also can be combined into stable compound Ca
4(PO
4)
2(OH).
Three, summary of the invention
The method that the object of the present invention is to provide a kind of industrial silicon melt direct oxidation refining to purify, it is raw material that this method adopts the silicon melt of emitting in the electric furnace, directly joins in the heating converting furnace, successively is blown into pressurized air and SiO in the heating converting furnace
2Gas-solid mixture, H that-CaO base composite oxidate is formed
2O steam and H
2Make that metallic impurity are reduced to below the 1.0ppmw in the silicon, nonmetallic impurity B, P are reduced to below the 0.5ppmw, resistivity reaches more than the 2.5 Ω cm, thereby directly directly prepare foreign matter contents such as Al, Ca, Ti, B, P from industrial silicon melt, reach that metallic impurity are reduced to below the 1.0ppmw in the silicon, nonmetallic impurity B and P are reduced to 0.2ppmw respectively and below the 0.5ppmw, resistivity reaches 2.5 Ω cm the above object.The HIGH-PURITY SILICON that meets the solar energy level silicon requirement.
The present invention realizes according to the following steps:
1, reinforced: as the industrial silicon melt of Al content 1000～2000ppmw, Ca content 50～500ppmw, Ti content 100～200ppmw, B content 10～50ppmw, P content 20～80ppmw in the electric furnace to be joined by tundish in the plumbago crucible of heating converting furnace, adopt the Frequency Induction Heating mode to make the industrial silicon melt temperature be controlled at 1450～1600 ℃;
2, refining:
(1) removes metallic impurity: in silicon melt, be blown into by pressurized air and 50～70 weight %SiO
2The gas-solid mixture of forming with 30～50 weight %CaO carries out refining, gas-solid volume ratio is 20～50: 1, gas-solid mixture flow rate 5～15L/min removes higher metal element A l, Ca, Ti, Na, the Mg of content in the silicon, and metallic element is oxidized to corresponding oxide compound Al
2O
3, CaO, TiO
2, Na
2O, MgO and with the SiO that adds
2-CaO forms compound multicomponent slag phase, and impurity element B and P generate B respectively simultaneously
2O
3, P
2O
5Enter in the slag or generation gaseous boron oxide compound BO, B
2Volatilizations such as O are removed, and refining time 1～2h, foreign matter content are reduced to Al 50～10ppmw, Ca20～5ppmw, Ti10～1ppmw, B10～5ppmw, P content 20～10ppmw respectively, and slag is removed from molten silicon surface;
(2) removal of impurity element boron: the closes compression air is blown into rare gas element and 5～20 volume %H
2The mixed gas of O steam, gas flow are 5～20L/min, and the control melt temperature is at 1500～1600 ℃, system pressure is 10000～90000Pa, and duration of blast is 1～2h, at this moment, metals content impurity is reduced to below the 1.0ppmw in the silicon, and impurity element boron is oxidized to BHO
2, HBO, BH
2Gaseous compound and volatilizing, boron content is reduced to below the 0.2ppmw;
(3) removal of impurity element phosphor: stop H
2The O steam is blown into rare gas element and 10%～30 volume %H
2Mixed gas, gas flow 5～20L/min, melt temperature still are controlled at 1500～1600 ℃, system pressure 10000～90000Pa keeps duration of blast 1～2h, phosphorus content is reduced to below the 0.5ppmw;
3, condensation ingot casting: plumbago crucible is slowly tilted, silicon after the refining poured in the vacuum cyrsytalliser cool off from bottom to up, rate of cooling is controlled at 0.2～1mm/min, keep system pressure 0.001～0.1Pa, remove in the melt remaining gas, waiting to reduce to must silicon ingot after taking out and excise 1/3 head and 1/10 afterbody after the room temperature and promptly get refining.
Advantage of comparing with known technology and positively effect: to the clearance height of metallic impurity elements in the silicon and nonmetallic impurity B, P, reach that metallic impurity are reduced to below the 1.0ppmw in the silicon, nonmetallic impurity B and P are reduced to 0.2ppmw respectively and below the 0.5ppmw, resistivity reaches more than the 2.5 Ω cm, meets the solar energy level silicon requirement; Technical process is simplified, less investment, and cost is low, and can realize cleaner production substantially.
Four, embodiment
Embodiment 1: the molten state industrial silicon 5kg more than the purity 98wt% is joined by tundish in the plumbago crucible of heating converting furnace, adopt Frequency Induction Heating to make the silicon melt temperature remain on 1450～1500 ℃.At first, in silicon melt, be blown into by pressurized air and 55 weight %SiO
2The gas-solid mixture that-45 weight %CaO form, gas-solid volume ratio is 40: 1, and gas-solid mixture flow rate 10L/min removes silicon metallic element such as Al, Ca, Ti, Na, Mg, and refining time 1h removes slag from molten silicon surface; Closes compression air then is blown into the mixed gas of Ar and 10 volume % water vapour in melt, gas flow 10L/min, and temperature is controlled at 1550 ℃, and system pressure 90000Pa, duration of blast are 1.5h; Change and become to be blown into Ar+ (10 volume %) H
2Mixed gas, gas flow 10L/min, melt temperature still are controlled at 1500～1550 ℃, system pressure 90000Pa keeps duration of blast 1h; After refining finishes, silicon after the refining is poured in the crystallizer from last to cooling off, keep system pressure 0.1Pa, rate of cooling is controlled at 0.8mm/min, fully remove gas remaining in the melt, wait to reduce to and take out and excise 1/3 head and 1/10 afterbody after the room temperature and promptly get silicon ingot after the refining, Al≤1.0ppmw, Ca≤0.3ppmw, Ti≤0.5ppmw, Na≤0.1ppmw, Mg≤0.2ppmw, below other metals content impurities 0.1ppmw, B≤0.2ppmw, P≤0.3ppmw, resistivity 〉=2.5 Ω cm.
Embodiment 2: molten state industrial silicon 5kg is joined by tundish in the plumbago crucible of heating converting furnace, adopt Frequency Induction Heating to make the silicon melt temperature remain on 1450～1500 ℃.At first, in silicon melt, be blown into by pressurized air and 60%SiO
2The gas-solid mixture that-40%CaO forms, gas-solid volume ratio is 30: 1 gas-solid mixture flow rate 15L/min, removes silicon metallic element such as Al, Ca, Ti, Na, Mg etc., refining time 1h removes slag from molten silicon surface; The closes compression air is blown into Ar-(15% volume) H in melt then
2The mixed gas of O, gas flow 10L/min, temperature is controlled at 1550 ℃, system pressure 90000Pa, duration of blast 1.5h; Change and become to be blown into Ar+ (20% volume) H
2Mixed gas, gas flow 10L/min, melt temperature still are controlled at 1550 ℃, system pressure 90000Pa keeps duration of blast 1.5h; After refining finishes, silicon after the refining is poured in the crystallizer from last to cooling off, keep system pressure 0.1Pa, rate of cooling is controlled at 0.8mm/min, fully remove gas remaining in the melt, wait to reduce to and take out and excise 1/3 head and 1/10 afterbody after the room temperature and promptly get silicon ingot after the refining, Al≤0.5ppmw, Ca≤0.2ppmw, Ti≤0.2ppmw, Na≤0.1ppmw, Mg≤0.1ppmw, below other metals content impurities 0.1ppmw, B≤0.2ppmw, P≤0.2ppmw, resistivity 〉=3.5 Ω cm.
Claims (2)
1. the industrial silicon melt direct oxidation refining method of purifying is characterized in that: it realizes according to the following steps,
1) reinforced: as the industrial silicon melt raw material of Al content 1000～2000ppmw, Ca content 50～500ppmw, Ti content 100～200ppmw, B content 10～50ppmw, P content 20～80ppmw in the electric furnace to be joined by tundish in the plumbago crucible of heating converting furnace, adopt the Frequency Induction Heating mode to make the industrial silicon melt temperature be controlled at 1450～1600 ℃;
2) refining:
(1) removes metallic impurity: in silicon melt, be blown into by pressurized air and 50～70 weight %SiO
2The gas-solid mixture of forming with 30～50 weight %CaO carries out refining, gas-solid volume ratio is 20～50: 1, gas-solid mixture flow rate 5～15L/min removes higher metal element A l, Ca, Ti, Na, the Mg of content in the silicon, and metallic element is oxidized to corresponding oxide compound Al
2O
3, CaO, TiO
2, Na
2O, MgO and with the SiO that adds
2-CaO forms compound multicomponent slag phase, and impurity element B and P generate B respectively simultaneously
2O
3, P
2O
5Enter in the slag or generation gaseous boron oxide compound BO, B
2The O volatilization is removed, and refining time 1～2h, foreign matter content are reduced to Al 50～10ppmw, Ca20～5ppmw, Ti10～1ppmw, B10～5ppmw, P content 20～10ppmw respectively, and slag is removed from molten silicon surface;
(2) removal of impurity element boron: the closes compression air is blown into rare gas element and 5～20 volume %H
2The mixed gas of O steam, gas flow are 5～20L/min, and the control melt temperature is at 1500～1600 ℃, system pressure is 10000～90000Pa, and duration of blast is 1～2h, at this moment, metals content impurity is reduced to below the 1.0ppmw in the silicon, and impurity element boron is oxidized to HBO
2, HBO, BH
2Gaseous compound and volatilizing, boron content is reduced to below the 0.2ppmw;
(3) removal of impurity element phosphor: stop H
2The O steam is blown into rare gas element and 10%～30 volume %H
2Mixed gas, gas flow 5～20L/min, melt temperature still are controlled at 1500～1600 ℃, system pressure 10000～90000Pa keeps duration of blast 1～2h, phosphorus content is reduced to below the 0.5ppmw;
3) condensation ingot casting: plumbago crucible is slowly tilted, silicon after the refining poured in the vacuum cyrsytalliser cool off from bottom to up, rate of cooling is controlled at 0.2～1mm/min, keep system pressure 0.001～0.1Pa, remove in the melt remaining gas, wait to reduce to the silicon ingot that takes out and excise after the room temperature after 1/3 head and 1/10 afterbody promptly get refining.
2. the method that industrial silicon melt direct oxidation refining according to claim 1 is purified, it is characterized in that: the purity of described industrial silicon melt raw material is more than the 98wt%.
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| CN101481112B true CN101481112B (en) | 2010-11-10 |
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| CN102583389A (en) * | 2012-03-05 | 2012-07-18 | 昆明理工大学 | Method for purifying industrial silicon through external refining |
| CN103058199B (en) * | 2013-01-21 | 2015-06-03 | 昆明理工大学 | Method for external refining purification of industrial silicon |
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| WO2020221439A1 (en) * | 2019-04-30 | 2020-11-05 | Wacker Chemie Ag | Process for refining crude molten silicon by means of a particulate mediator |
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| CN112028031A (en) * | 2020-08-04 | 2020-12-04 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing sodium sulfide by melting reduction of industrial sodium sulfate |
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2009
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|---|---|---|---|---|
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| CN101481112A (en) | 2009-07-15 |
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