CN103265035B - Method for realizing convection agitation of silicon slag in medium smelting - Google Patents
Method for realizing convection agitation of silicon slag in medium smelting Download PDFInfo
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- CN103265035B CN103265035B CN201310221968.2A CN201310221968A CN103265035B CN 103265035 B CN103265035 B CN 103265035B CN 201310221968 A CN201310221968 A CN 201310221968A CN 103265035 B CN103265035 B CN 103265035B
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Abstract
The invention belongs to the field of smelting of polysilicon medium, and particularly relates to a method for realizing convection agitation of a silicon slag in medium smelting. The method is characterized in that a slag agent regulator is added to change the density of a liquid slag after a slag agent is completely melted into silicon liquid, so as to realize convection agitation of the slag agent and the silicon liquid. The method has the advantages that (1) the convection agitation of the silicon slag in the medium smelting process is realized by using the slag agent regulator under the condition of not using electromagnetic agitation of a medium-frequency induction furnace; and the utilization rate of the slag agent can be effectively improved by over 30%; and (2) a boron-removal reaction interface can be improved by the convection agitation; and the boron-removal effect can be improved by 15-25%.
Description
Technical field
The invention belongs to polycrystalline silicon medium melting field, be specifically related to a kind of method realizing convection agitation of silicon slag in medium melting.
Background technology
World today's energy dilemma and environmental pollution pressure are also deposited, and people are badly in need of cleaning, safety, continuable new forms of energy.Sun power, as meeting the energy required like this, always is the target that people pursue.People are the utilizations of its heat effect to the use of sun power the earliest, but are difficult to the needs meeting modern society completely.Until the discovery of photoresistance, the manufacture of solar cell, the Land use systems that people find sun power new.Silicon is as the most desirable feedstock of solar cell, impurity wherein mainly contains the nonmetallic impuritys such as metallic impurity and B, P such as Fe, Al, Ca, and these impurity elements can reduce the Compound Degree of silicon crystal grain interface photo-generated carrier, and the Compound Degree of photo-generated carrier determines the photoelectric transformation efficiency of solar cell, removing these impurity so effective has vital effect in the application aspect of solar cell.
The development of solar photovoltaic industry depends on the purification to silicon raw material, comprises medium melting, directional freeze, electron beam purification and casting ingot process in the process of polycrystalline silicon purifying.Metallurgy method has development potentiality because possessing simple, the lower-cost advantage of technique.Require that equipment is the simplest with slag practice in all multi-methods, the easiest industrialization promotion.Thus the researching value of medium melting most reality and application prospect.
At present, in domestic and international medium fusion process, no matter use light slag or heavy slag, wherein, the slag agent less than the liquid-tight degree of silicon is light slag, namely the slag agent larger than the liquid-tight degree of silicon attach most importance to slag, the relative position of the liquid slag after melting and silicon liquid is fixed, and the simple electromagnetic action by intermediate-frequency heating furnace stirs, except boron reaction interface is less, the utilization ratio of slag agent is lower, except effect of boron is general.
Summary of the invention
The object of this invention is to provide a kind of method realizing convection agitation of silicon slag in medium melting, not by under the effect of external force, by changing the density of slag agent, realizing the convection agitation of silicon liquid and liquid slag.
Realize the method for convection agitation of silicon slag in a kind of medium melting of the present invention, after slag agent is all molten to silicon liquid, add slag agent conditioning agent, change the density of liquid slag, realize the convection agitation of slag agent and silicon liquid with this.
Wherein, when light slag is selected in slag agent, preferably carry out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first adding slag agent conditioning agent is light slag conditioning agent CaO, all melts after 10 ~ 20min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, after 5 ~ 15min, convection agitation terminates;
(3) add slag agent conditioning agent again to attach most importance to slag conditioning agent SiO
2, all melt after 10 ~ 20min, liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 5 ~ 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 3 ~ 5 times, namely completes medium melting.
When heavy slag is selected in slag agent, preferably carry out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first add slag agent conditioning agent to attach most importance to slag conditioning agent SiO
2, all melt after 10 ~ 20min, liquid slag density is through changing, and with silicon liquid generation convection agitation, after 5 ~ 15min, convection agitation terminates;
(3) adding slag agent conditioning agent is again light slag conditioning agent CaO, all melts after 10 ~ 20min, and liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 5 ~ 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 3 ~ 5 times, namely completes medium melting.
In above process, each add-on of light slag conditioning agent CaO selected and the mass ratio of slag agent are 1:20 ~ 1:40.The heavy slag conditioning agent SiO selected
2the mass ratio of each add-on and slag agent is 1:15 ~ 1:30.
CaO can increase the density of liquid slag, makes the density of light slag be greater than the density of silicon liquid, and liquid slag is by convection into bottom silicon liquid from silicon liquid top; SiO
2reduce the density of liquid slag, make the density of heavy slag be less than the density of silicon liquid, liquid slag is by convection into silicon liquid top bottom silicon liquid.
The invention has the advantages that: (1), in the induction stirring not by medium-frequency induction furnace, achieves the convection agitation of silicon slag in medium fusion process by slag agent conditioning agent, effectively can improve the utilization ratio more than 30% of slag agent; (2) convection agitation can improve except boron reaction interface, can make except effect of boron improves 15 ~ 25%.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
Light slag is selected in slag agent, and the quality of slag agent is 100kg, and medium melting is carried out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first adding slag agent conditioning agent is light slag conditioning agent CaO2.5kg, all melts after 10min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, after 10min, convection agitation terminates;
(3) add slag agent conditioning agent again to attach most importance to slag conditioning agent SiO
2all melt after 3.5kg, 10min, liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 10min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 5 times, namely completes medium melting.
The refined silicon obtained after medium melting, to take multiple measurements it through ICP-MS and average, wherein B content is 0.25ppmw.
Embodiment 2:
Light slag is selected in slag agent, and the quality of slag agent is 100kg, and medium melting is carried out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first adding slag agent conditioning agent is light slag conditioning agent CaO5kg, all melts after 20min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, after 15min, convection agitation terminates;
(3) add slag agent conditioning agent again to attach most importance to slag conditioning agent SiO
2all melt after 6kg, 20min, liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 3 times, namely completes medium melting.
The refined silicon obtained after medium melting, to take multiple measurements it through ICP-MS and average, wherein B content is 0.10ppmw.
Embodiment 3:
Heavy slag is selected in slag agent, and the quality of slag agent is 100kg, and medium melting is carried out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first add slag agent conditioning agent to attach most importance to slag conditioning agent SiO
2all melt after 4.5kg, 15min, liquid slag density is through changing, and with silicon liquid generation convection agitation, after 7min, convection agitation terminates;
(3) adding slag agent conditioning agent is again light slag conditioning agent CaO3.5kg, all melts after 15min, and liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 7min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 4 times, namely completes medium melting.
The refined silicon obtained after medium melting, to take multiple measurements it through ICP-MS and average, wherein B content is 0.15ppmw.
Embodiment 4:
Heavy slag is selected in slag agent, and the quality of slag agent is 100kg, and medium melting is carried out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first add slag agent conditioning agent to attach most importance to slag conditioning agent SiO
2all melt after 5kg, 15min, liquid slag density is through changing, and with silicon liquid generation convection agitation, after 15min, convection agitation terminates;
(3) adding slag agent conditioning agent is again light slag conditioning agent CaO4kg, all melts after 15min, and liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 4 times, namely completes medium melting.
The refined silicon obtained after medium melting, to take multiple measurements it through ICP-MS and average, wherein B content is 0.20ppmw.
Claims (2)
1. realize a method for convection agitation of silicon slag in medium melting, it is characterized in that, when light slag is selected in slag agent, carry out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first adding slag agent conditioning agent is light slag conditioning agent CaO, and the mass ratio of described light slag conditioning agent CaO and slag agent is 1:20 ~ 1:40, all melts after 10 ~ 20min, liquid slag density is through changing, with silicon liquid generation convection agitation, after 5 ~ 15min, convection agitation terminates;
(3) add slag agent conditioning agent again to attach most importance to slag conditioning agent SiO
2, described heavy slag conditioning agent SiO
2be 1:15 ~ 1:30 with the mass ratio of slag agent, all melt after 10 ~ 20min, liquid slag density is again through changing, and with silicon liquid, anti-convection agitation occurs, after 5 ~ 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 3 ~ 5 times, namely completes medium melting.
2. realize a method for convection agitation of silicon slag in medium melting, it is characterized in that, when heavy slag is selected in slag agent, carry out according to following steps:
(1) slag agent becomes liquid slag after being all molten to silicon liquid;
(2) first add slag agent conditioning agent to attach most importance to slag conditioning agent SiO
2, described heavy slag conditioning agent SiO
2be 1:15 ~ 1:30 with the mass ratio of slag agent, all melt after 10 ~ 20min, liquid slag density is through changing, and with silicon liquid generation convection agitation, after 5 ~ 15min, convection agitation terminates;
(3) adding slag agent conditioning agent is again light slag conditioning agent CaO, the mass ratio of described light slag conditioning agent CaO and slag agent is 1:20 ~ 1:40, all melt after 10 ~ 20min, liquid slag density is again through changing, anti-convection agitation is there is with silicon liquid, after 5 ~ 15min, anti-convection agitation terminates;
(4) repeating step (2) ~ (3) 3 ~ 5 times, namely completes medium melting.
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