CN104556051B - 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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- CN104556051B CN104556051B CN201410829785.3A CN201410829785A CN104556051B CN 104556051 B CN104556051 B CN 104556051B CN 201410829785 A CN201410829785 A CN 201410829785A CN 104556051 B CN104556051 B CN 104556051B
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- slag former
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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 element in polysilicon slag former, and regeneration slag former prepared by this method.
Background technology
Metallurgy method prepares solar-grade polysilicon, because its low cost, energy consumption are little, environmental friendliness the features such as, wide at present
General popularization and employing.In the technique of purification, the method for slag making melting is mainly utilized to remove the boron impurity in polysilicon, utilization
The method of directional solidification or pickling is removed metal impurities in polysilicon, is removed using the method for electronic torch melting or vacuum melting
Phosphorus impurities in polysilicon.
For in slag making smelting technology, the cost of slag former accounts for the 1/3 about of whole process costs, and current slag former
For expendable consumed product it is impossible to reuse.With the development of metallurgy method, the discarded slag former that slag making smelting technology produces is got over
Come more, define serious industrial refuse.
So, urgent at present a kind of method cheap, that free of contamination, energy consumption is little, to enable discarded slag former
Enough regenerations, while reducing new slag former use, reduce the industrial refuse that slag former produces, can reduce whole simultaneously
The cost of bar metallurgy-prepared polysilicon production line.
Content of the invention
For solving to adopt produce in the technique of boron impurity in slag making method of smelting removal polysilicon to discard in prior art
Slag former is many, forms industrial refuse, easily causes the problem of pollution, and the present invention provides a kind of cheap, free of contamination, energy consumption little
With metallurgy method remove polysilicon slag former in boron element method, so that the content of boron element is dropped to below the mark, can obtain again
Raw slag former.
Technical scheme is as follows：
A kind of method removing boron element in polysilicon slag former with metallurgy method, comprises the following steps：
1. by discarded polysilicon slag former and high-purity silicon material with 10～20:1 mass ratio mixing, is crushed to 20～40mm
Bulk, be placed in intermediate frequency furnace, melting under atmosphere, the power of intermediate frequency furnace risen to 100～300kW, by temperature
Degree is increased to more than 1800～2200 DEG C, stirs and is incubated 15～60min, makes boron back-diffusion to silicon；
2. step 1. in insulation terminate after, stop stirring, standing, continue second and be incubated, the time is 5～10min；
3. melt is poured onto in refractory container, cooling, one end of excision silicon material, remainder is and removes boron element
Polysilicon slag former.
Further, step 1. in broken graphite rod can be adopted using tungsten alloy hammer, described stirring, stirring can make slag making
Boron in agent quickly fully back-diffusion to silicon, the power of described intermediate frequency furnace is raised with the speed of 1～10kW/min, described
High-purity silicon material is 6N grade high-purity silicon material.
Further, step 3. described in refractory container material be alumina firebrick.
Another technical purpose of the present invention is to provide a kind of regeneration slag former, removes polysilicon slag making by above-mentioned metallurgy method
In agent, the method preparation of boron element, the polysilicon slag former removing boron element is crushed to the bulk of 1mm～5mm, encapsulates standby
With.Obtain final product described regeneration slag former.Described crushing can break machine using Hubei Province.
Beneficial effects of the present invention：
(1) present invention utilizes the back-diffusion behavior that boron element exists at silicon melt with slag melt interface, more than 1800
It is incubated at a temperature of DEG C, agitation slag agent enables the boron element in slag quickly sufficiently to diffuse in the middle of silicon melt, recycles silicon
The slag agent removing boron element is isolated by slag separation means, and after measured, the boron element in slag former can be reduced to 0.5 after treatment
～2ppmw, can reach the level of slag former, illustrate that the method for the present invention can effectively remove the impurity boron element in polysilicon；
(2) metallurgy method prepares the proposition of slag former renovation process in polysilicon link, slag former can be made to reuse, warp
Estimation, reduces the cost more than 5% of whole production line, and can save slag former cost more than 10%.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art that the present invention is more fully understood, but not with
Any mode limits the present invention.
Embodiment 1
Discarded polysilicon slag former and 6N grade high-purity silicon material are with 10:1 mass ratio mixing, is hammered into shape polysilicon with tungsten alloy
Slag former and 6N grade high-purity silicon material are crushed to the bulk of 20～40mm, are sufficiently mixed, are placed in the graphite crucible of intermediate frequency furnace,
Its power is increased to by 100kW with the speed of 1kW/min, after temperature rises to 1800 DEG C, is incubated 60min, keeps in whole process
Stirring, makes boron back-diffusion to silicon.After insulation terminates, stop stirring, static, carry out second insulation, the time is 10min, so
Afterwards melt is poured onto in the refractory container of alumina firebrick, cooling, one end of excision silicon material, remainder is and removes boron unit
The polysilicon slag former of element.It is broken crusher machine to 1mm bulk with Hubei Province, standby after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron element is 2ppmw.
Embodiment 2
Discarded polysilicon slag former and 6N grade high-purity silicon material are with 15:1 mass ratio mixing, is hammered into shape polysilicon with tungsten alloy
Slag former and 6N grade high-purity silicon material are crushed to the bulk of 30mm～40mm, are sufficiently mixed, are placed in the graphite crucible of intermediate frequency furnace
In, its power is increased to by 200kW with the speed of 5kW/min, after temperature rises to 2000 DEG C, is incubated 40min, protects in whole process
Hold stirring, make boron back-diffusion to silicon.After insulation terminates, stop stirring, static, carry out second insulation, the time is 7min, so
Afterwards melt is poured onto in the refractory container of alumina firebrick, cooling, one end of excision silicon material, remainder is and removes boron unit
The polysilicon slag former of element.It is broken crusher machine to the bulk of 3mm with Hubei Province, standby after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron element is 1.8ppmw.
Embodiment 3
Discarded polysilicon slag former and 6N grade high-purity silicon material are with 20:1 mass ratio mixing, is hammered into shape polysilicon with tungsten alloy
Slag former and 6N grade high-purity silicon material are crushed to the bulk of 20mm～40mm, are sufficiently mixed, are placed in the graphite crucible of intermediate frequency furnace
In, its power is increased to by 300kW with the speed of 10kW/min, after temperature rises to 2200 DEG C, is incubated 15min, in whole process
It is kept stirring for, make boron back-diffusion to silicon.After insulation terminates, stop stirring, static, carry out second insulation, the time is 5min,
Then melt is poured onto in the refractory container of alumina firebrick, cooling, one end of excision silicon material, remainder as removes boron
The polysilicon slag former of element.It is broken crusher machine to the bulk of 5mm with Hubei Province, standby after encapsulation.
Through measuring, in the regeneration slag former prepared in this way, the content of boron element is 0.5ppmw.
Claims (5)
1. a kind of method removing boron element in polysilicon slag former with metallurgy method, comprises the following steps：
1. by discarded polysilicon slag former and high-purity silicon material with 10～20:1 mass ratio mixing, is crushed to the block of 20～40mm
Shape, is placed in intermediate frequency furnace, and the power of intermediate frequency furnace is risen to 100～300kW by melting under atmosphere, by temperature liter
Up to 2200 DEG C, stir and be incubated 15～60min, make boron back-diffusion to silicon；
2. step 1. in insulation terminate after, stop stirring, standing, continue second and be incubated, the time is 5～10min；
3. melt is poured onto in refractory container, cooling, one end of excision silicon material, remainder is the polycrystalline removing boron element
Silicon slag former.
2. metallurgy method according to claim 1 remove boron element in polysilicon slag former method it is characterised in that：Step
The power of intermediate frequency furnace described in 1. is raised with the speed of 1～10kW/min.
3. metallurgy method according to claim 1 remove boron element in polysilicon slag former method it is characterised in that：Step
1. high-purity silicon material described in is 6N grade high-purity silicon material.
4. metallurgy method according to claim 1 remove boron element in polysilicon slag former method it is characterised in that：Step
The material of refractory container described in 3. is alumina firebrick.
5. the metallurgy method described in Claims 1 to 4 any one removes the method preparation of boron element in polysilicon slag former
Regeneration slag former it is characterised in that：The polysilicon slag former removing boron element is crushed to the bulk of 1mm～5mm, encapsulates standby
With.
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| NO318092B1 (en) * | 2002-05-22 | 2005-01-31 | Elkem Materials | Calcium-silicate-based slag, process for the preparation of calcium-silicate-based slag, and application for slag treatment of molten silicon |
| CN103072993B (en) * | 2013-02-04 | 2014-07-09 | 福建兴朝阳硅材料股份有限公司 | Method for removing boron in polycrystalline silicon |
| CN103073001B (en) * | 2013-02-26 | 2015-12-02 | 昆明理工大学 | A kind of method adopting high alkalinity refining agent to remove boron impurities in metallurgical grade silicon |
| CN103342363B (en) * | 2013-06-19 | 2015-08-19 | 青岛隆盛晶硅科技有限公司 | Slag former and the using method thereof of white residue separation is convenient to during polycrystalline silicon medium melting |
| CN103754882B (en) * | 2013-12-27 | 2015-07-08 | 福建兴朝阳硅材料股份有限公司 | Purifying method of slag-making agent with boron removal |
| CN103964677B (en) * | 2014-04-17 | 2016-03-30 | 江苏盎华光伏工程技术研究中心有限公司 | Fused silica crucible fragment renovation process after polycrystalline silicon ingot casting |
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