CN103265035A - 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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- CN103265035A CN103265035A CN2013102219682A CN201310221968A CN103265035A CN 103265035 A CN103265035 A CN 103265035A CN 2013102219682 A CN2013102219682 A CN 2013102219682A CN 201310221968 A CN201310221968 A CN 201310221968A CN 103265035 A CN103265035 A CN 103265035A
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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 realize in a kind of medium melting the method for white residue convection agitation.
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 always is the target that people pursue as satisfying the energy that requires like this.People are the utilizations of its heat effect to the use of sun power the earliest, but are difficult to satisfy fully the needs of modern society.Up to the discovery of photoresistance, the manufacturing of solar cell, people find sun power new utilize mode.Silicon is as the desirable feedstock of solar cell, impurity wherein mainly contains metallic impurity and nonmetallic impuritys such as B, P such as Fe, Al, Ca, and these impurity elements can reduce the silicon crystal grain compound degree of photo-generated carrier at the interface, and the compound degree of photo-generated carrier has determined the photoelectric transformation efficiency of solar cell, in the application facet of solar cell crucial effects is arranged so effectively remove these impurity.
The development of photovoltaic industry depends on the purification to the silicon raw material, comprises medium melting, directional freeze, electron beam purification and casting ingot process in the process that polysilicon is purified.Metallurgy method has development potentiality because possessing simple, the lower-cost advantage of technology.Require equipment the simplest with slag practice in all multi-methods, the easiest industrialization promotion.Thereby researching value and the application prospect of the tool reality of medium melting.
At present, both at home and abroad in the medium fusion process, no matter use light slag or heavy slag, wherein, the slag agent littler than the liquid-tight degree of silicon is light slag, the slag agent bigger than the liquid-tight degree of the silicon slag of namely attaching most importance to, liquid slag after the fusion and the relative position of silicon liquid are fixed, and the electromagnetic action by the heating in medium frequency stove stirs merely, and it is less to remove the boron reaction interface, the utilization ratio of slag agent is lower, and it is general to remove effect of boron.
Summary of the invention
The purpose of this invention is to provide in a kind of medium melting the method that realizes the white residue convection agitation, under the effect by external force not, by changing the density of slag agent, realize the convection agitation of silicon liquid and liquid slag.
Realize the method for white residue convection agitation in a kind of medium melting of the present invention, after the slag agent all is 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 the slag agent for use, preferably carry out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) adding slag agent conditioning agent earlier is light slag conditioning agent CaO, all fusings behind 10～20min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 5～15min, convection agitation finishes;
(3) add the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to again
2, all fusings behind 10～20min, opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 5～15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 3～5 times, namely finishes the medium melting.
When the weight slag is selected in the slag agent for use, preferably carry out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) add earlier the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to
2, all fusings behind 10～20min, liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 5～15min, convection agitation finishes;
(3) adding slag agent conditioning agent again is light slag conditioning agent CaO, all fusings behind 10～20min, and opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 5～15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 3～5 times, namely finishes the medium melting.
In the above process, the light each add-on of selecting for use of slag conditioning agent CaO and the mass ratio of slag agent are 1:20～1:40.The heavy slag conditioning agent SiO that selects for use
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 greater than the density of silicon liquid, and liquid slag is by convection into silicon liquid bottom from silicon liquid top; SiO
2Reduce the density of liquid slag, make the density of heavy slag less than the density of silicon liquid, liquid slag is by convection into silicon liquid top from silicon liquid bottom.
The invention has the advantages that: (1) by the induction stirring of medium-frequency induction furnace, has realized white residue convection agitation in the medium fusion process can effectively improving the utilization ratio of slag agent more than 30% by slag agent conditioning agent; (2) convection agitation can improve except the boron reaction interface, can make except effect of boron raising 15～25%.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1:
Light slag is selected in the slag agent for use, and the quality of slag agent is 100kg, and the medium melting is carried out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) adding slag agent conditioning agent earlier is light slag conditioning agent CaO2.5kg, all fusings behind the 10min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 10min, convection agitation finishes;
(3) add the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to again
23.5kg, all fusings behind the 10min, opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 10min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 5 times, namely finishes the medium melting.
The refined silicon that obtains after the medium melting takes multiple measurements it through ICP-MS and to average, and wherein B content is 0.25ppmw.
Embodiment 2:
Light slag is selected in the slag agent for use, and the quality of slag agent is 100kg, and the medium melting is carried out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) adding slag agent conditioning agent earlier is light slag conditioning agent CaO5kg, all fusings behind the 20min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 15min, convection agitation finishes;
(3) add the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to again
26kg, all fusings behind the 20min, opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 3 times, namely finishes the medium melting.
The refined silicon that obtains after the medium melting takes multiple measurements it through ICP-MS and to average, and wherein B content is 0.10ppmw.
Embodiment 3:
Heavy slag is selected in the slag agent for use, and the quality of slag agent is 100kg, and the medium melting is carried out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) add earlier the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to
24.5kg, all fusings behind the 15min, liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 7min, convection agitation finishes;
(3) adding slag agent conditioning agent again is light slag conditioning agent CaO3.5kg, all fusings behind the 15min, and opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 7min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 4 times, namely finishes the medium melting.
The refined silicon that obtains after the medium melting takes multiple measurements it through ICP-MS and to average, and wherein B content is 0.15ppmw.
Embodiment 4:
Heavy slag is selected in the slag agent for use, and the quality of slag agent is 100kg, and the medium melting is carried out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) add earlier the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to
25kg, all fusings behind the 15min, liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 15min, convection agitation finishes;
(3) adding slag agent conditioning agent again is light slag conditioning agent CaO4kg, all fusings behind the 15min, and opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 4 times, namely finishes the medium melting.
The refined silicon that obtains after the medium melting takes multiple measurements it through ICP-MS and to average, and wherein B content is 0.20ppmw.
Claims (5)
1. realize the method for white residue convection agitation in the medium melting, it is characterized in that when the slag agent all is molten to silicon liquid after that add slag agent conditioning agent, the density of change liquid slag realizes the convection agitation of slag agent and silicon liquid with this.
2. realize the method for white residue convection agitation in the medium melting according to claim 1, it is characterized in that when light slag is selected in the slag agent for use, carrying out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) adding slag agent conditioning agent earlier is light slag conditioning agent CaO, all fusings behind 10～20min, and liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 5～15min, convection agitation finishes;
(3) add the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to again
2, all fusings behind 10～20min, opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 5～15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 3～5 times, namely finishes the medium melting.
3. realize the method for white residue convection agitation in the medium melting according to claim 1, it is characterized in that when the weight slag is selected in the slag agent for use, carrying out according to following steps:
(1) the slag agent becomes liquid slag after all being molten to silicon liquid;
(2) add earlier the slag agent conditioning agent slag conditioning agent SiO that attaches most importance to
2, all fusings behind 10～20min, liquid slag density is through changing, and with silicon liquid generation convection agitation, behind 5～15min, convection agitation finishes;
(3) adding slag agent conditioning agent again is light slag conditioning agent CaO, all fusings behind 10～20min, and opposition stream through changing, takes place with silicon liquid and stirs in liquid slag density again, behind 5～15min, opposes that the stream stirring finishes;
(4) repeating step (2)～(3) is 3～5 times, namely finishes the medium melting.
4. according to the method that realizes the white residue convection agitation in claim 2 or the 3 described medium meltings, the mass ratio that it is characterized in that light slag conditioning agent CaO and slag agent is 1:20～1:40.
5. according to the method that realizes the white residue convection agitation in claim 2 or the 3 described medium meltings, it is characterized in that heavy slag conditioning agent SiO
2With the mass ratio of slag agent be 1:15～1:30.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115468419A (en) * | 2022-08-11 | 2022-12-13 | 商南中剑实业有限责任公司 | Device and method for removing boron impurities in metallurgical-grade silicon in ore-smelting furnace |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555015A (en) * | 2009-05-19 | 2009-10-14 | 厦门大学 | Purifying method and device for removing boron from polysilicon |
| CN101628718A (en) * | 2008-07-16 | 2010-01-20 | 佳科太阳能硅(厦门)有限公司 | Method for removing impurity of phosphorus from metallurgical grade silicon |
| CN102259865A (en) * | 2011-06-01 | 2011-11-30 | 宁夏银星多晶硅有限责任公司 | Slag washing process for removing boron from metallurgical polycrystalline silicon |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628718A (en) * | 2008-07-16 | 2010-01-20 | 佳科太阳能硅(厦门)有限公司 | Method for removing impurity of phosphorus from metallurgical grade silicon |
| CN101555015A (en) * | 2009-05-19 | 2009-10-14 | 厦门大学 | Purifying method and device for removing boron from polysilicon |
| CN102259865A (en) * | 2011-06-01 | 2011-11-30 | 宁夏银星多晶硅有限责任公司 | Slag washing process for removing boron from metallurgical polycrystalline silicon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115468419A (en) * | 2022-08-11 | 2022-12-13 | 商南中剑实业有限责任公司 | Device and method for removing boron impurities in metallurgical-grade silicon in ore-smelting furnace |
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Effective date of registration: 20171124 Address after: Pudong Town Jimo city Shandong province 266234 city of Qingdao Ren Jia Tun Cun Ren Jia Tun Lu Patentee after: QINGDAO NEW ENERGY SOLUTIONS INC. (NESI) Address before: 1 road 266000 in Shandong province Qingdao city Laoshan District No. 1 Keyuan latitude B block 7 layer B4-2 Patentee before: Qingdao Changsheng Dongfang Industry Group Co., Ltd. |
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