CN104556051A - Method for removing boron element in polysilicon slag former with metallurgy method and prepared regenerated slag former - Google Patents
Method for removing boron element in polysilicon slag former with metallurgy method and prepared regenerated slag former Download PDFInfo
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- CN104556051A CN104556051A CN201410829785.3A CN201410829785A CN104556051A CN 104556051 A CN104556051 A CN 104556051A CN 201410829785 A CN201410829785 A CN 201410829785A CN 104556051 A CN104556051 A CN 104556051A
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Abstract
The invention relates to a method for removing boron element in a polysilicon slag former with a metallurgy method. The method comprises the following steps: after mixing the waste polysilicon slag former with a high-purity silicon material, smelting in a medium-frequency induction furnace, stirring at the temperature of 1800-2200 DEG C and carrying out heat preservation for 15-60 min, so that boron is back-diffused into silicon, then standing for 5-10 min, pouring a melt into a refractory container, cooling, and cutting one end of the silicon material, so that the remaining part is the polysilicon slag former with removed boron element. According to the method, the impurity boron element in the polysilicon can be effectively removed, so that the impurity boron element is reduced to be 0.5-2 ppmw, the level of the slag former can be reached, and the recycling of the slag former can reduce more than 5% of the cost of the whole production line and can save more than 10% of the cost of the slag former.
Description
Technical field
The present invention relates to the method removing boron in polysilicon slag former, and regeneration slag former prepared by this method.
Background technology
Metallurgy method prepares solar-grade polysilicon, due to features such as its cost is low, energy consumption is little, environmental friendliness, is promoted widely and adopts at present.In the technique of purifying, mainly utilize the boron impurity in the method for slag making melting removal polysilicon, utilize the method for directional freeze or pickling to remove the metallic impurity in polysilicon, the phosphorus impurities utilized in the method removal polysilicon of electron beam melting or vacuum melting.
For in slag making melting technology, the cost of slag former accounts for about 1/3 of whole process costs, and slag former is expendable consumed product at present, can not reuse.Along with the development of metallurgy method, the discarded slag former that slag making melting technology produces gets more and more, and defines serious industrial refuse.
So, urgent a kind of that occur cheapness, that free of contamination, energy consumption is little method, enables the slag former regeneration of discarding at present, while reducing new slag former use, reduce the industrial refuse that slag former produces, the cost of whole piece metallurgy-prepared polysilicon production line can be reduced simultaneously.
Summary of the invention
Adopt the discarded slag former produced in the technique of boron impurity in slag making melting method removal polysilicon many for solving in prior art, form industrial refuse, the problem easily polluted, a kind of that the invention provides cheapness, that free of contamination, energy consumption the is little method removing boron in polysilicon slag former with metallurgy method, the content of boron is dropped to below the mark, regeneration slag former can be obtained.
Technical scheme of the present invention is as follows:
Remove a method for boron in polysilicon slag former with metallurgy method, comprise the following steps:
1. discarded polysilicon slag former is mixed with the mass ratio of 10 ~ 20:1 with HIGH-PURITY SILICON material, be crushed to the bulk of 20 ~ 40mm, be placed in medium-frequency induction furnace, melting under atmosphere, the power of medium-frequency induction furnace is risen to 100 ~ 300kW, temperature is increased to more than 1800 ~ 2200 DEG C, stirs and be incubated 15 ~ 60min, make boron back diffusion in silicon;
2. step 1. in insulation terminate after, stop stir, leave standstill, continue second time insulation, the time is 5 ~ 10min;
3. be poured onto in refractory container by melt, cooling, one end of excision silicon material, rest part is the polysilicon slag former removing boron.
Further, step 1. middle fragmentation can adopt tungstenalloy to hammer into shape, and described stirring can adopt graphite rod, stirs and the quick fully back diffusion of the boron in slag former can be made in silicon, the power of described medium-frequency induction furnace raises with the speed of 1 ~ 10kW/min, and described HIGH-PURITY SILICON material is 6N grade high-purity silicon material.
Further, step 3. described in the material of refractory container be alumina firebrick.
Another technical purpose of the present invention is to provide a kind of regeneration slag former, and prepared by the method being removed boron in polysilicon slag former by above-mentioned metallurgy method, the polysilicon slag former removing boron is crushed to the bulk of 1mm ~ 5mm, for subsequent use after encapsulation.Obtain described regeneration slag former.Described fragmentation can adopt Hubei Province to break machine.
Beneficial effect of the present invention:
(1) the present invention utilizes the back diffusion behavior that boron exists at silicon melt and slag melt interface place, be incubated at the temperature more than 1800 DEG C, stirring slag agent enables the boron in slag diffuse to fully fast in the middle of silicon melt, the slag agent of removing boron is isolated by recycling white residue separation means, after measured, boron in slag former can be reduced to 0.5 ~ 2ppmw after treatment, the level of slag former can be reached, illustrate that method of the present invention effectively can remove the boron impurities element in polysilicon;
(2) metallurgy method prepares the proposition of slag former renovation process in polysilicon link, and slag former can be made to reuse, and through estimation, reduces the cost more than 5% of whole production line, and can save slag former cost more than 10%.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
Discarded polysilicon slag former mixes with the mass ratio of 10:1 with 6N grade high-purity silicon material, with tungstenalloy hammer, polysilicon slag former and 6N grade high-purity silicon material are crushed to the bulk of 20 ~ 40mm, abundant mixing, be placed in the plumbago crucible of medium-frequency induction furnace, with the speed of 1kW/min, its power is increased to 100kW, after temperature rises to 1800 DEG C, insulation 60min, keep in whole process stirring, make boron back diffusion in silicon.After insulation terminates, stop stirring, static, carry out second time insulation, the time is 10min, is then poured onto in the refractory container of alumina firebrick by melt, cooling, and one end of excision silicon material, rest part is the polysilicon slag former removing boron.It is broken crusher machine with Hubei Province block to 1mm, for subsequent use after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron is 2ppmw.
Embodiment 2
Discarded polysilicon slag former mixes with the mass ratio of 15:1 with 6N grade high-purity silicon material, with tungstenalloy hammer, polysilicon slag former and 6N grade high-purity silicon material are crushed to the bulk of 30mm ~ 40mm, abundant mixing, be placed in the plumbago crucible of medium-frequency induction furnace, with the speed of 5kW/min, its power is increased to 200kW, after temperature rises to 2000 DEG C, insulation 40min, keep in whole process stirring, make boron back diffusion in silicon.After insulation terminates, stop stirring, static, carry out second time insulation, the time is 7min, is then poured onto in the refractory container of alumina firebrick by melt, cooling, and one end of excision silicon material, rest part is the polysilicon slag former removing boron.It is broken the bulk of crusher machine to 3mm with Hubei Province, for subsequent use after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron is 1.8ppmw.
Embodiment 3
Discarded polysilicon slag former mixes with the mass ratio of 20:1 with 6N grade high-purity silicon material, with tungstenalloy hammer, polysilicon slag former and 6N grade high-purity silicon material are crushed to the bulk of 20mm ~ 40mm, abundant mixing, be placed in the plumbago crucible of medium-frequency induction furnace, with the speed of 10kW/min, its power is increased to 300kW, after temperature rises to 2200 DEG C, insulation 15min, keep in whole process stirring, make boron back diffusion in silicon.After insulation terminates, stop stirring, static, carry out second time insulation, the time is 5min, is then poured onto in the refractory container of alumina firebrick by melt, cooling, and one end of excision silicon material, rest part is the polysilicon slag former removing boron.It is broken the bulk of crusher machine to 5mm with Hubei Province, for subsequent use after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron is 0.5ppmw.
Claims (5)
1. remove a method for boron in polysilicon slag former with metallurgy method, comprise the following steps:
1. discarded polysilicon slag former is mixed with the mass ratio of 10 ~ 20:1 with HIGH-PURITY SILICON material, be crushed to the bulk of 20 ~ 40mm, be placed in medium-frequency induction furnace, melting under atmosphere, the power of medium-frequency induction furnace is risen to 100 ~ 300kW, temperature is increased to more than 1800 ~ 2200 DEG C, stirs and be incubated 15 ~ 60min, make boron back diffusion in silicon;
2. step 1. in insulation terminate after, stop stir, leave standstill, continue second time insulation, the time is 5 ~ 10min;
3. be poured onto in refractory container by melt, cooling, one end of excision silicon material, rest part is the polysilicon slag former removing boron.
2. metallurgy method according to claim 1 removes the method for boron in polysilicon slag former, it is characterized in that: step 1. described in the power of medium-frequency induction furnace raise with the speed of 1 ~ 10kW/min.
3. metallurgy method according to claim 1 removes the method for boron in polysilicon slag former, it is characterized in that: step 1. described in HIGH-PURITY SILICON material be 6N grade high-purity silicon material.
4. metallurgy method according to claim 1 removes the method for boron in polysilicon slag former, it is characterized in that: step 3. described in the material of refractory container be alumina firebrick.
5. regeneration slag former prepared by the method removing boron in polysilicon slag former by the metallurgy method described in Claims 1 to 4 any one, is characterized in that: the bulk polysilicon slag former removing boron being crushed to 1mm ~ 5mm, for subsequent use after encapsulation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106185948A (en) * | 2016-07-11 | 2016-12-07 | 厦门大学 | A kind of industrial silicon slag making dephosphorization process |
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| CN103754882A (en) * | 2013-12-27 | 2014-04-30 | 福建兴朝阳硅材料股份有限公司 | Purifying method of slag-making agent with boron removal |
| CN103964677A (en) * | 2014-04-17 | 2014-08-06 | 江苏盎华光伏工程技术研究中心有限公司 | Method for regenerating fused quartz crucible through fused quartz crucible fragments after polycrystalline silicon ingoting |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2003097528A1 (en) * | 2002-05-22 | 2003-11-27 | Elkem Asa | A calcium-silicate based slag for treatment of molten silicon |
| CN103072993A (en) * | 2013-02-04 | 2013-05-01 | 福建兴朝阳硅材料股份有限公司 | Method for removing boron in polycrystalline silicon |
| CN103073001A (en) * | 2013-02-26 | 2013-05-01 | 昆明理工大学 | Method for removing impurity boron of metallurgical silicon by high-basicity refining agent |
| CN103342363A (en) * | 2013-06-19 | 2013-10-09 | 青岛隆盛晶硅科技有限公司 | Slag-forming agent convenient for silicon slag separation in medium smelting of polycrystalline silicon, and application method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106185948A (en) * | 2016-07-11 | 2016-12-07 | 厦门大学 | A kind of industrial silicon slag making dephosphorization process |
| CN106185948B (en) * | 2016-07-11 | 2018-12-11 | 厦门大学 | A kind of industrial silicon slag making dephosphorization process |
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