CN102452651A - Process for removing boron impurities in silicon by using wet argon plasma - Google Patents
Process for removing boron impurities in silicon by using wet argon plasma Download PDFInfo
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- CN102452651A CN102452651A CN2010105240681A CN201010524068A CN102452651A CN 102452651 A CN102452651 A CN 102452651A CN 2010105240681 A CN2010105240681 A CN 2010105240681A CN 201010524068 A CN201010524068 A CN 201010524068A CN 102452651 A CN102452651 A CN 102452651A
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 70
- 239000010703 silicon Substances 0.000 title claims abstract description 70
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 57
- 229910052786 argon Inorganic materials 0.000 title claims abstract description 48
- 239000012535 impurity Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 27
- 230000008569 process Effects 0.000 title abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002210 silicon-based material Substances 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 238000003723 Smelting Methods 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims abstract description 4
- 238000009832 plasma treatment Methods 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 22
- 239000010453 quartz Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 241000209456 Plumbago Species 0.000 claims description 7
- 238000013467 fragmentation Methods 0.000 claims description 6
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- 238000004519 manufacturing process Methods 0.000 abstract description 7
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a process for removing boron impurities in polycrystalline silicon, which comprises the steps of melting high-purity silicon metal in a vacuum melting furnace, blowing by plasma beams formed by oxygen-containing wet argon to realize boron removal by oxidation, then stirring at high temperature for volatilization, descending a crucible and solidifying to realize ingot casting, wherein the purity of the obtained silicon material reaches the manufacturing standard of a solar cell. In the process, the smelting temperature is controlled to 1450-1550 ℃, the wet argon plasma treatment time is 2-5 hours, after the wet argon plasma is volatilized for 1-2 hours under the condition of heat preservation, the silicon liquid gradually descends along with the crucible to achieve cooling and solidification, and the obtained silicon ingot can be used for the subsequent production of the polycrystalline silicon solar cell after the flaw-piece is removed. The process has the characteristics of simplicity, high efficiency, low energy consumption, no pollution and the like, can effectively remove boron impurities in the silicon material, can reduce the boron concentration in the silicon to 0.05ppmwt at the lowest, and reduces the production cost of the solar-grade polysilicon.
Description
Technical field
The present invention relates to a kind of wet argon plasma and remove the technology of boron impurity in the silicon; Belong to the pyrometallurgy field; Relate generally to and utilize vacuum melting furnace to realize the fusing of high pure metal silicon; Adopt oxygen containing wet argon plasma flame to remove the technology of boron, reach further purification, to satisfy the silicon for solar cell requirement to high pure metal silicon.
Background technology
Flourish along with global new forms of energy industry; In order to solve the silicon material for solar cells problem; Each state has all dropped into strength and has carried out the research of the special-purpose polysilicon of solar cell; Being to solve quality problems on the one hand, is technology and the technological problems that solves industrialized mass production on the other hand, accomplishes low cost, high-quality, high efficiency suitability for industrialized production as far as possible.
At present, polycrystalline silicon used for solar battery mainly adopts chemical purification and two kinds of methods of physical purification to produce, and wherein chemical purification method mainly contains Siemens Method, silane decomposition, fluidized bed process etc.The physics method also is called as metallurgy method, is the physical properties of utilizing each impurity in the Pure Silicon Metal or impurity compound, directly smelts through metallurgical technology, adopts technologies such as high melt and directional freeze to remove impurity more.
Existing metallurgy method technology is primarily aimed at the less impurity of segregation coefficient and carries out directional freeze; Impurity to vp big (like phosphoric etc.) carries out vaporization at high temperature or electron beam melting, and adopts oxidation or slag making to remove to the boron impurity that more difficult fractional condensation and volatilization are removed more.Slag practice adopts CaO-SiO more
2Slag system contacts with molten silicon liquid, makes boron and slag former form compound or soluble solids, in process of setting, separates with silicon, reaches impurity-eliminating effect.Lot of domestic and foreign experts and scholars study this method, at CaO-SiO
2CaCl, CaF have been added on the basis of slag system
2, CrCl
3, material such as MgO, to improve the slag characteristic, improve impurity-eliminating effect, but that this method is removed effect of boron is limited, research work still rests on laboratory stage mostly.
At present, be the method that oxidation removes boron by what generally adopt, and in industrial production, obtained using checking.The principle that oxidation removes boron is that boron is contacted with oxygen carrier, forms the oxide compound or the oxyhydroxide of boron, removes through the high melt volatilization again.It is numerous that existing oxidation removes the implementing process of boron, have nothing in common with each other, in physical purification technology with contain oxygen plasma to remove effect of boron the most obvious.This method improves the reaction efficiency and the rate of volatilization of boron mainly by the high reactivity and the high temperature of plasma flame, has reached and has well removed effect of boron.
As far back as 1996; Under the support of New Energy and Industrial Technology Development Organization (NEDO); Kawasaki, Japan system Inland Steel (Kawasaki Steel) develops the method for being produced solar energy level silicon by metalluragical silicon; In this method what remove that the boron step adopts is exactly the method that plasma removes boron, be to announce successful metallurgy method in the world the earliest.After this various countries researchist carries out the technical study of plasma purifying metalluragical silicon one after another, and constantly makes a breakthrough technically, makes the plasma impurity removal process become method of purification rapidly and efficiently gradually.The people such as C.Alemany of France utilize contains H
2And O
2The metalluragical silicon reaction of beam-plasma and molten state realized removing the effect of boron.Its result shows that the boron in the silicon is many with the volatilization of forms such as BOH, BO, and the mass concentration of B is reduced to 2ppmw from 15ppmw.More domestic researchists are also carrying out job family, and that mostly used atmosphere is is oxygenous, the plasma flame of hydrogen and water vapour, and used plasma generator adopts the direct current plasma producer more.
Though direct current plasma producer heating efficiency is higher, be prone to introduce impurity, in view of this, selected RF plasma reactor in the present invention for use, reach induced electricity and leave, avoid contaminating impurity.Simultaneously, select for use the water vapour of suitable proportioning and oxygen to add in the argon gas, under the situation that does not influence plasma flame, reach the best effect of boron that removes.
Summary of the invention
Technical problem to be solved by this invention provides the technology that a kind of wet argon plasma is removed boron impurity in the silicon, makes that the boron impurity total content is lower than 1ppmwt in the product.The present invention with high pure metal silicon in vacuum melting furnace after the fusion; Through containing the beam-plasma purging that the wet argon gas of oxygen forms; Realize that oxidation removes boron, after this descend through high-temperature stirring volatilization, crucible again and solidify the realization ingot casting that gained silicon material purity has reached the solar cell manufacturer's standard.
The technology that wet argon plasma provided by the invention is removed boron impurity in the silicon comprises the steps:
Step 1, select high pure metal silicon according to the fine fodder principle;
The overall purity of raw material is not less than 99.999%, and especially boron content is lower than 30ppmwt, and VA family constituent content is lower than 1ppmwt.
High pure metal silicon material places and carries out melting in the quartz crucible, and various materials in the stove (like quartz material, thermal field material, lagging material etc.) are high-purity material, and is wherein identical with step 1 to the requirement of boron and VA family constituent content.
Smelting furnace is vacuumized, after vacuum tightness reaches 10Pa, open heating system the silicon material is carried out preheating.After temperature of thermal field reaches 1535 ℃, the insulation material.Adopt resistance heat smelting furnace deposite metal silicon material, smelting temperature is 1450～1550 ℃, and its optimum temps is 1535 ℃.
Close lobe pump, utilize sliding vane rotary pump to keep rough vacuum in the stove, vacuum tightness is 10
2About Pa.
With the glass source bottle of argon gas through being filled with water, form wet argon gas, feed plasma generator ionization again, form plasma flame at the spout place.Behind plasma igniting, slowly add oxygen, form oxygen containing wet argon plasma flame.The volume ratio of argon gas, water vapour and oxygen is 30: 1: 1.5 in the used mixed gas.
Through crucible lift device, plumbago crucible is risen to the place apart from plasma spout 5～6cm, with wet argon plasma flame silicon liquid surface is purged, purge time was controlled at 2～5 hours.
After wet argon plasma processing, open lobe pump, improve vacuum tightness in the stove, reach about 10Pa, silicon liquid is incubated melting, temperature is controlled at 1530～1550 ℃ is fully volatilized lower-boiling impurity.
Through the slow decline of crucible, realize silicon liquid directional freeze from bottom to top, dropping speed of the crucible is 5～10mm/min.
Embodiment subsequently will prove, the wet argon plasma of the present invention removes that boron impurity content is lower than 1ppmwt in the technology gained polycrystal silicon ingot product of boron impurity in the silicon, can be used for the polysilicon solar cell subsequent production.That technology of the present invention has is simple efficient, less energy-consumption, characteristics such as pollution-free, can effectively remove the boron impurity in the silicon material, minimumly can boron concentration in the silicon be reduced to 0.05ppmwt, and reduces the production cost that solar level is tasted with discrimination silicon more.
Description of drawings
Fig. 1 removes the process flow sheet of boron impurity in the silicon for the present invention.
Fig. 2 is the structural representation that wet argon plasma of the present invention removes the boron device.
Wherein: 1 is plasma generator; 2, melting bell; 3, thermal field; 4, plumbago crucible; 5, graphite crucible holder; 6, water-cooled pallet; 7, water inlet; 8, water outlet; 9, silicon liquid; 10, quartz crucible; 11, plasma gas; 12, ruhmkorff coil; 13, high frequency electric source; 14, Sheath Gas (argon gas); 15, Central Gas (mixed gas).
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, further set forth the present invention.These embodiment are interpreted as only being used to the present invention is described and are not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can do various changes or modification to the present invention, and these equivalences change and modify and fall into claim of the present invention institute restricted portion equally.
Embodiment 1
As shown in Figure 1, use wet argon plasma as shown in Figure 2 to remove the boron device, be that the high pure metal silicon of 27ppmwt is after fragmentation, in ten inches non-transparent quartz crucibles 10 of the standard of evenly packing into 3Kg boron concentration.Quartz crucible 10 is placed in the plumbago crucible 4 of vacuum melting furnace, vacuumize and carry out high temperature melting at 1450 ℃ after reaching 10Pa.After treating that the silicon material melts fully, close lobe pump, only utilize rotary-vane vaccum pump to keep the vacuum tightness of 400Pa in the stove.In plasma generator 1, feed moisture argon gas 14 and 15, after igniting forms plasma flame, aerating oxygen progressively, the plasma flame of formation mixed atmosphere.Utilize lifting device rising bushing position to apart from plasma spout 5cm place, silicon liquid 9 surfaces are purged.
Purge after 2 hours, close plasma generator 1, stop air feed, open lobe pump simultaneously, be evacuated to 10Pa.Crucible is fallen into thermal field 3 middle parts, insulation volatilization 1 hour.Afterwards, keep the 9 upper end fusions of silicon liquid, the quartz crucible 4 that slowly descends makes it break away from thermal field 3 and cooling from bottom to top gradually, and fall off rate was 5mm/min, accomplished the directional freeze process through 6 hours.After treating to cool off fully, take out silicon ingot and obtain polycrystal silicon ingot with the mechanically cutting flaw-piece.
Detect through sampling, the purity of present embodiment gained silicon material reaches 99.9997%, and wherein the concentration of boron is reduced to 0.05ppmwt.
As shown in Figure 1, use wet argon plasma as shown in Figure 2 to remove the boron device, be that the high pure metal silicon of 26ppmwt is after fragmentation, in ten inches non-transparent quartz crucibles 10 of the standard of evenly packing into 5Kg boron concentration.Quartz crucible 10 is placed in the plumbago crucible 4 of vacuum melting furnace, vacuumize and carry out high temperature melting at 1535 ℃ after reaching 10Pa.After treating that the silicon material melts fully, close lobe pump, only utilize rotary-vane vaccum pump to keep the vacuum tightness of 400Pa in the stove.In plasma generator 1, feed moisture argon gas 14 and 15, after igniting forms plasma flame 11, aerating oxygen progressively, the plasma flame of formation mixed atmosphere.Utilize lifting device rising bushing position to apart from plasma spout 5cm place, silicon liquid 9 surfaces are purged.
Purge after 3 hours, close plasma generator 1, stop air feed, open lobe pump simultaneously, be evacuated to 10Pa.Crucible is fallen into the thermal field middle part, insulation volatilization 1. hours.Afterwards, keep the 9 upper end fusions of silicon liquid, the quartz crucible 10 that slowly descends makes it break away from thermal field 3 and cooling from bottom to top gradually, and fall off rate was 10mm/min, accomplished the directional freeze process through 5 hours.After treating to cool off fully, take out silicon ingot and obtain polycrystal silicon ingot with the mechanically cutting flaw-piece.
Detect through sampling, the purity of present embodiment gained silicon material reaches 99.9995%, and wherein the concentration of boron is reduced to 0.07ppmwt.
Embodiment 3:
As shown in Figure 1, use wet argon plasma as shown in Figure 2 to remove the boron device, be that the high pure metal silicon of 27ppmwt is after fragmentation, in ten inches non-transparent quartz crucibles 10 of the standard of evenly packing into 10Kg boron concentration.Quartz crucible 10 is placed in the plumbago crucible 4 of vacuum melting furnace, vacuumize and carry out high temperature melting at 1550 ℃ after reaching 10Pa.After treating that the silicon material melts fully, close lobe pump, only utilize rotary-vane vaccum pump to keep the vacuum tightness of 400Pa in the stove.In plasma generator 1, feed moisture argon gas 14 and 15, after igniting forms plasma flame 11, aerating oxygen progressively, the plasma flame of formation mixed atmosphere.Utilize lifting device rising bushing position to apart from plasma spout 5cm place, silicon liquid 9 surfaces are purged.
Purge after 5 hours, close plasma generator 1, stop air feed, open lobe pump simultaneously, be evacuated to 10Pa.Crucible is fallen into thermal field 3 middle parts, insulation volatilization 2 hours.Afterwards, keep the 9 upper end fusions of silicon liquid, the quartz crucible 10 that slowly descends makes it break away from thermal field 3 and cooling from bottom to top gradually, and fall off rate was 10mm/min, accomplished the directional freeze process through 8 hours.After treating to cool off fully, take out silicon ingot and obtain polycrystal silicon ingot with the mechanically cutting flaw-piece.
Detect through sampling, the purity of present embodiment gained silicon material reaches 99.9994%, and wherein the concentration of boron is reduced to 0.13ppmwt.
Claims (10)
1. a wet argon plasma is removed the technology of boron impurity in the silicon, and it may further comprise the steps:
Step 1, select high pure metal silicon according to the fine fodder principle, its purity is not less than 99.999%;
Step 2, high pure metal silicon is carried out fragmentation;
Step 3, the metal silico briquette is placed in the quartz crucible, in vacuum melting furnace, carry out vacuum melting;
Step 4, form oxygen containing wet argon plasma flame, silicon liquid surface is purged through RF plasma reactor;
Step 5, the silicon liquid after plasma treatment at high temperature are incubated volatilization;
Step 6, the slow quartz crucible that descends make the slow cooling from bottom to top of silicon liquid, realize directional freeze and ingot casting;
Step 7, the gained silicon ingot is removed flaw-piece, obtain polycrystal silicon ingot.
2. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon, it is characterized in that in the described step 1, in the high pure metal silicon, boron content is lower than 30ppmwt, and VA family constituent content is lower than 1ppmwt.
3. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon, it is characterized in that in the described step 3, the metal silico briquette after the fragmentation places in the plumbago crucible of vacuum melting furnace; Vacuumize, after vacuum tightness reached 10Pa, opening resistor hot melt furnace carried out preheating to the silicon material, reached 1450～1550 ℃ until the thermal field smelting temperature, the insulation material.
4. wet argon plasma according to claim 3 is removed the technology of boron impurity in the silicon, it is characterized in that the thermal field smelting temperature is 1535 ℃.
5. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon; It is characterized in that, in the described step 4, utilize sliding vane rotary pump to keep rough vacuum in the smelting furnace; With the glass source bottle of argon gas through being filled with water; Form wet argon gas, feed plasma generator ionization again, form plasma flame at the spout place; Behind plasma igniting, slowly add oxygen, form oxygen containing wet argon plasma flame; Through crucible lift device, plumbago crucible is risen to the place apart from plasma spout 5～6cm, with wet argon plasma flame silicon liquid surface is purged, purge time is 2～5 hours.
6. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon, it is characterized in that, in the described step 5; After wet argon plasma processing; Open lobe pump, improve vacuum tightness in the smelting furnace, reach 1-20Pa; Silicon liquid is incubated melting, and temperature is controlled at 1530～1550 ℃ is fully volatilized lower-boiling impurity.
7. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon, it is characterized in that in the described step 6, dropping speed of the crucible is 5～10mm/min.
8. wet argon plasma according to claim 1 is removed the technology of boron impurity in the silicon, it is characterized in that, in the described step 7, removes quartz, silicon material surface oxide layer and the impurity coacervating of adhesion.
9. remove the technology of boron impurity in the silicon according to claim 1 or 4 described wet argon plasmas; It is characterized in that; In the described step 3, high pure metal silicon material places and carries out melting in the quartz crucible, and quartz material, thermal field material and lagging material in the vacuum melting furnace are high-purity material; Boron content is lower than 30ppmwt, and VA family constituent content is lower than 1ppmwt.
10. wet argon plasma according to claim 5 is removed the technology of boron impurity in the silicon; It is characterized in that; The volume ratio of argon gas and water vapour is 30: 1 in the used wet argon gas, and after forming plasma flame, the oxygen that the back adds and the volume ratio of used argon gas are 1: 20; The plasma flame that final mountain argon gas, water vapour and oxygen mixture volume ionization form, wherein the volume ratio of argon gas, water vapour and oxygen is 30: 1: 1.5 in the mixed gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815704A (en) * | 2012-09-18 | 2012-12-12 | 复旦大学 | Method for preparing solar grade polysilicon by recycling silicon cut wastes |
| CN110006841A (en) * | 2019-04-11 | 2019-07-12 | 内蒙古神舟硅业有限责任公司 | O, C in a kind of granulated polycrystalline silicon, III, the detection method of group Ⅴ element |
| CN115872408A (en) * | 2022-10-19 | 2023-03-31 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
-
2010
- 2010-10-28 CN CN2010105240681A patent/CN102452651A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815704A (en) * | 2012-09-18 | 2012-12-12 | 复旦大学 | Method for preparing solar grade polysilicon by recycling silicon cut wastes |
| CN110006841A (en) * | 2019-04-11 | 2019-07-12 | 内蒙古神舟硅业有限责任公司 | O, C in a kind of granulated polycrystalline silicon, III, the detection method of group Ⅴ element |
| CN110006841B (en) * | 2019-04-11 | 2022-12-06 | 内蒙古神舟硅业有限责任公司 | Method for detecting O, C, III and V group elements in granular polycrystalline silicon |
| CN115872408A (en) * | 2022-10-19 | 2023-03-31 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
| CN115872408B (en) * | 2022-10-19 | 2023-08-11 | 北京理工大学 | Quartz sand purification method based on thermal plasma jet |
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Application publication date: 20120516 |