CN109292779A - A method of HIGH-PURITY SILICON/silicon alloy is produced with high scrap silicon slag refining - Google Patents

A method of HIGH-PURITY SILICON/silicon alloy is produced with high scrap silicon slag refining Download PDF

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CN109292779A
CN109292779A CN201811219039.7A CN201811219039A CN109292779A CN 109292779 A CN109292779 A CN 109292779A CN 201811219039 A CN201811219039 A CN 201811219039A CN 109292779 A CN109292779 A CN 109292779A
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silicon
melt
slag
alloy
high scrap
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邢鹏飞
孔剑
魏冬卉
庄艳歆
金星
冯忠宝
高波
尹华意
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Northeastern University China
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Northeastern University China
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/037Purification
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001Dry processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C28/00Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

A method of HIGH-PURITY SILICON/silicon alloy being produced with high scrap silicon slag refining, is used as raw material after sequentially including the following steps: (1) high scrap silicon drying;Prepare slag former;(2) smelting furnace is opened, raw material and slag former are put into smelting furnace and carry out slag refining, all forms melt after fusing;(3) after completing slag refining, melt is come out of the stove and pours into stratification in mold, or the stratification in smelting furnace, form HIGH-PURITY SILICON/silicon alloy after silicon melt/silicon alloy melt condensation.The method of the invention realizes the diamond wire cutting waste materials of crystalline silicon efficiently to recycle, and reduces pollution of the waste material to environment, realizes high melt and refining removal of impurities is combined into one.

Description

A method of HIGH-PURITY SILICON/silicon alloy is produced with high scrap silicon slag refining
Technical field
It is the invention belongs to field of material technology, in particular to a kind of to be closed with high scrap silicon slag refining production HIGH-PURITY SILICON/silicon The method of gold.
Background technique
Currently, the microtomy of solar energy crystalline silicon (crystalline silicon refers to polysilicon and monocrystalline silicon) be mainly Buddha's warrior attendant wire cutting or The cutting of person's silicon carbide, since the diameter of cutting wire and the thickness of required silicon wafer are not much different, have 35 in cutting process~ 40% crystalline silicon enters in slug in the form of a powder, forms crystalline silicon cutting waste material.It is quick with photovoltaic energy Development, it is anticipated that a large amount of cutting waste material will be generated, this not only has lost the expensive crystalline silicon of value, but also makes to environment At huge pollution, therefore being highly desirable invention can be to the method that this part waste material carries out effective recycling and reusing.
There are two types of high scrap silicon mainly includes:
The first high scrap silicon refers to the high scrap silicon that solar energy industry generates: generating when slicing silicon ingots including crystalline silicon Cutting waste material (including diamond cut generate waste material and silicon carbide cutting generate waste material), crystalline silicon ingot polishing when generate Polishing waste material, scale off after crystalline silicon ingot casting expect end to end, discarded crystal silicon chip, superseded solar battery sheet;Here Crystalline silicon refers to the general designation of polysilicon and monocrystalline silicon;The high scrap silicon main component generated in solar energy industry is elemental silicon, pure It spends very high, if it is possible to it be recycled, preparation high purity silicon ingot is re-used to, great economic benefit can be generated in this way;This Outside, moreover it is possible to reduce the cost of solar battery indirectly, this will play positive effect to the development for promoting photovoltaic industry;
Second high scrap silicon refers to the high scrap silicon that industrial silicon or high-silicon alloy are crushed or generate when cutting.If energy It is enough that the high scrap silicon in this part is recycled, it also can reduce environmental pollution, while great economic benefit can also be generated.
Summary of the invention
HIGH-PURITY SILICON/silicon alloy method is produced with high scrap silicon slag refining the purpose of the present invention is to propose to a kind of, is used Calcium based compound etc. is used as additive or slag former, is added in furnace after melting after it is mixed with high scrap silicon, then by silicon Liquid and clinker liquid separate after coming out of the stove, and obtain silicon after finally condensing.
Method of the invention sequentially includes the following steps:
1, moisture removal is removed into the drying of high scrap silicon, as raw material;Prepare slag former;The wherein mass ratio of raw material and slag former For 100:(3~60);The slag former is calcium based compound, or is mixed compound;The mixed compound is magnesium One of based compound, sodium based compound and potassium based compound a variety of are mixed with calcium based compound;The calcium system Compound contains CaCO by mass percentage30~99%, CaCl20~30%, CaF20~30%, CaO 1~100%;It is described Magnesium based compound contain MgO 0~100%, MgCO by mass percentage30~100%, MgF20~30%, MgCl21~ 100%;The sodium based compound contains Na by mass percentage2CO31~100%, NaHCO30~99%, NaCl 0~ 30%, NaF 0~30%;The potassium based compound contains K by mass percentage2CO320~50%, KHCO315~30%, KCl 12~20%, KF 15~38%;Wherein the calcium based compound in mixed compound accounts for the 10~99% of gross mass;
2, smelting furnace is opened, raw material and slag former are put into smelting furnace and carry out slag refining, raw material and slag former are whole Melt is formed after fusing;The temperature of smelting furnace is controlled during slag refining at 1420 DEG C or more;
3, after completing slag refining, melt is come out of the stove and is poured into mold, the silicon melt in melt/silicon alloy melt and clinker Melt stratification in mold, then condensation solidification will be carried out respectively after silicon melt/silicon alloy melt and slag melt separation, HIGH-PURITY SILICON/silicon alloy is formed after middle silicon melt/silicon alloy melt condensation;Or after completing slag refining, whole melts are in melting Silicon melt/silicon alloy melt and slag melt stratification in furnace, then pour into respectively and condense solidification in different molds, wherein silicon HIGH-PURITY SILICON/silicon alloy is formed after melt/silicon alloy melt condensation.
There are two types of above-mentioned high scrap silicons: one is the high scrap silicons that solar energy industry generates, and select solar energy crystalline silicon The head scaled off after the polishing waste material that is generated when the cutting waste material that is generated when slicing silicon ingots, crystalline silicon ingot polishing, crystalline silicon ingot casting Tailing, discarded crystal silicon chip and/or superseded solar battery sheet;It is generated when the described solar energy crystalline silicon slicing silicon ingots Cutting waste material includes the waste material that diamond cut generates and the waste material that silicon carbide cutting generates;The crystalline silicon be polysilicon and The general designation of monocrystalline silicon;Another kind is the high scrap silicon generated when broken high-silicon alloy or cutting, and the high-silicon alloy is Si Mass percent >=50% alloy.
In the above method, when high scrap silicon is the high scrap silicon that solar energy industry generates, the pickling of high scrap silicon elder generation is gone Except impurity, then filtrate is washed to as neutrality, finally drying is used as raw material;The acid solution that pickling uses is mass concentration 5~30% Hydrochloric acid and/or sulfuric acid, the mass ratio of acid solution and high scrap silicon is (3~15) when pickling: 1.
In the above method, the adding manner of raw material and slag former are as follows: raw material and slag former are put into melting after mixing Furnace;Smelting furnace is placed into after raw material and slag former are either pressed into agglomerate after mixing;Either first raw material is suppressed At agglomerate, smelting furnace is put into after then again mixing agglomerate and slag former.
Above-mentioned smelting furnace is electric arc furnaces, mineral hot furnace, refining furnace, induction furnace, resistance furnace or plasma furnace.
The above method, when high scrap silicon is the high scrap silicon that solar energy industry generates, silicon melt and clinker when standing Melt layering forms HIGH-PURITY SILICON after silicon melt condensation, contains Si 99~99.999% by mass percentage;When high scrap silicon is silicon When the high scrap silicon generated when alloy breaks down or cutting, when standing, silicon alloy melt and slag melt are layered, and silicon alloy is molten Silicon alloy is formed after body condensation, contains Si >=50% by mass percentage.
Above-mentioned HIGH-PURITY SILICON is come out and cooled down after directional solidification using solidification is oriented in directional solidification furnace to room temperature Silicon ingot is obtained, the both ends end to end of silicon ingot are cut off respectively, the resection length at both ends accounts for silicon ingot total length 20~30% end to end, remaining Part is the polysilicon of solar level, contains Si >=99.9999% by mass percentage.
In the above method, the rate of recovery of elemental silicon is 45~98% in high scrap silicon.
The principle of the invention lies in: using calcium based compound as slag former, or use the mixing containing calcium based compound Compound melts together with cutting waste material under the high temperature conditions as slag former;Melt clinker liquid and mesh during standing Standard liquid body (silicon melt/silicon alloy melt) layering, casting when can make target component (HIGH-PURITY SILICON/silicon alloy) and other at (including silica) is divided to be smoothly detached.
Of the invention the high efficiente callback for realizing high scrap silicon utilizes compared with prior art, not only turns waste into wealth, but also Reduce pollution of the waste material to environment, realizes high melt and refining removal of impurities process is combined into one;This method have process it is short, The advantages that low energy consumption, simple and easy, it is easy to accomplish industrialized production.
Detailed description of the invention
Fig. 1 is being shown in the embodiment of the present invention with high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method flow It is intended to.
Specific embodiment
The present invention is described in detail below in conjunction with specific example.
High scrap silicon in the embodiment of the present invention contains Si 60~90% by mass percentage, contains SiO25~30%.
Pickling time is 1~2h in the embodiment of the present invention.
The CaCO used in the embodiment of the present invention3、CaCl2、CaF2It is commercially available pulverulent reagent product with CaO.
MgO, the MgCO used in the embodiment of the present invention3、MgF2And MgCl2For commercially available pulverulent reagent product.
The Na used in the embodiment of the present invention2CO3、NaHCO3, NaCl and NaF be commercially available pulverulent reagent product.
The K used in the embodiment of the present invention2CO3、KHCO3, KCl and KF be commercially available pulverulent reagent product.
Embodiment 1
The cutting waste material generated when the high scrap silicon used is solar energy crystalline silicon slicing silicon ingots;Solar energy crystalline silicon silicon ingot The cutting waste material generated when slice is the waste material that diamond cut generates and the waste material that silicon carbide cutting generates;High scrap silicon is dried It is dry to remove moisture removal, as raw material;
Prepare slag former;The mass ratio of raw material and slag former is 100:20;Slag former is calcium based compound, by quality percentage Than containing CaCO32%, CaCl233%, CaF215%, CaO 50%;
Smelting furnace is opened, raw material and slag former are put into smelting furnace and carry out slag refining, it is whole to raw material and slag former Melt is formed after fusing;The temperature of smelting furnace is controlled during slag refining at 1480~1500 DEG C;Wherein raw material and slag former Adding manner are as follows: raw material and slag former are put into smelting furnace after mixing;
The smelting furnace of use is resistance furnace;
After completing slag refining, melt is come out of the stove and is poured into mold, the silicon melt and slag melt in melt are in mold Stratification, then condensation solidification will be carried out respectively after silicon melt and slag melt separation, it is wherein formed after silicon melt condensation high-purity Silicon contains Si 99.971% by mass percentage;
The silicon rate of recovery is 54%.
Embodiment 2
Process is as shown in Figure 1;
With embodiment 1, difference is method:
(1) the polishing waste material generated when the high scrap silicon used is crystalline silicon ingot polishing;The pickling of high scrap silicon elder generation is removed Impurity, then filtrate is washed to as neutrality, finally drying is used as raw material;The acid solution that pickling uses is the hydrochloric acid of mass concentration 5%, acid The mass ratio of acid solution and high scrap silicon is 15:1 when washing;
(2) prepare slag former;Wherein the mass ratio of raw material and slag former is 100:3;Slag former is mixed compound, by magnesium Based compound is mixed with calcium based compound;Calcium based compound contains CaCO by mass percentage389%, CaCl25%, CaF2 4%, CaO 2%;Magnesium based compound contains MgO 50%, MgCO by mass percentage315%, MgF220%, MgCl215%; Wherein the calcium based compound in mixed compound accounts for the 60% of gross mass;
(3) temperature of smelting furnace is controlled during slag refining at 1460~1490 DEG C;The addition side of raw material and slag former Formula are as follows: place into smelting furnace after raw material and slag former are pressed into agglomerate after mixing;The smelting furnace of use is induction furnace;
(4) after completing slag refining, then whole melts silicon melt and slag melt stratification in smelting furnace are distinguished It pours into and condenses solidification in different molds, wherein form HIGH-PURITY SILICON after silicon melt condensation, contain Si 99.992% by mass percentage;
The silicon rate of recovery is 83%;
By HIGH-PURITY SILICON using solidification is oriented in directional solidification furnace, is come out and cooled down after directional solidification to room temperature and obtained Silicon ingot cuts off at the both ends end to end of silicon ingot respectively, and the resection length at both ends accounts for silicon ingot total length 20% end to end, and remainder is too The polysilicon of positive energy level contains Si 99.9999% by mass percentage.
Embodiment 3
(1) the high scrap silicon used for crystalline silicon ingot casting after the material end to end that scales off;The pickling of high scrap silicon elder generation is gone to clean Matter, then filtrate is washed to as neutrality, finally drying is used as raw material;The acid solution that pickling uses is the sulfuric acid of mass concentration 30%, acid The mass ratio of acid solution and high scrap silicon is 3:1 when washing;
(2) prepare slag former;The mass ratio of raw material and slag former is 100:60;Slag former is mixed compound, by sodium system Compound is mixed with calcium based compound;Calcium based compound contains CaCO by mass percentage359%, CaF25%, CaO 36%;Sodium based compound contains Na by mass percentage2CO350%, NaHCO315%, NaCl 20%, NaF 15%;Hybridization The calcium based compound closed in object accounts for the 40% of gross mass;
(3) temperature of smelting furnace is controlled during slag refining at 1420~1470 DEG C;The addition side of raw material and slag former Formula are as follows: first press raw materials into agglomerate, be put into smelting furnace after then again mixing agglomerate and slag former;The smelting furnace of use is electricity Arc furnace;
(4) HIGH-PURITY SILICON contains Si 99.983% by mass percentage;
The silicon rate of recovery is 61%;
By HIGH-PURITY SILICON using solidification is oriented in directional solidification furnace, is come out and cooled down after directional solidification to room temperature and obtained Silicon ingot cuts off at the both ends end to end of silicon ingot respectively, and the resection length at both ends accounts for silicon ingot total length 25% end to end, and remainder is too The polysilicon of positive energy level contains Si 99.9999% by mass percentage.
Embodiment 4
Process is as shown in Figure 1;
With embodiment 1, difference is method:
(1) the high scrap silicon used is discarded crystal silicon chip and superseded solar battery sheet;High scrap silicon is first sour It washes away except impurity, then is washed to filtrate as neutrality, finally drying is used as raw material;The acid solution that pickling uses is mass concentration 10% Hydrochloric acid and 10% the mass mixings acid such as sulfuric acid, the mass ratio of acid solution and high scrap silicon is 5:1 when pickling;
(2) prepare slag former;The mass ratio of raw material and slag former is 100:15;Slag former is mixed compound, by potassium system Compound is mixed with calcium based compound;Calcium based compound contains CaCO by mass percentage374%, CaCl210%, CaO 16%;Potassium based compound contains K by mass percentage2CO350%, KHCO315%, KCl 20%, KF 15%;Mixed compound In calcium based compound account for the 50% of gross mass;
(3) temperature of smelting furnace is controlled during slag refining at 1470~1510 DEG C;The smelting furnace of use is plasma Body furnace;
(4) after completing slag refining, then whole melts silicon melt and slag melt stratification in smelting furnace are distinguished It pours into and condenses solidification in different molds, wherein form HIGH-PURITY SILICON after silicon melt condensation, contain Si 99.890% by mass percentage;
The silicon rate of recovery is 85%;
By HIGH-PURITY SILICON using solidification is oriented in directional solidification furnace, is come out and cooled down after directional solidification to room temperature and obtained Silicon ingot cuts off at the both ends end to end of silicon ingot respectively, and the resection length at both ends accounts for silicon ingot total length 30% end to end, and remainder is too The polysilicon of positive energy level contains Si 99.9999% by mass percentage.
Embodiment 5
With embodiment 1, difference is method:
(1) the high scrap silicon that the high scrap silicon used generates when being crushed for high-silicon alloy;Drying goes moisture removal as raw material;
(2) prepare slag former;Wherein the mass ratio of raw material and slag former is 100:22;Slag former is mixed compound, by Magnesium based compound, sodium based compound, potassium based compound and calcium based compound mix;Calcium based compound contains by mass percentage CaCO355%, CaCl22%, CaF22%, CaO 41%;Magnesium based compound contains MgO 20%, MgCO by mass percentage3 30%, MgF212%, MgCl238%;Sodium based compound contains Na by mass percentage2CO320%, NaHCO330%, NaCl 12%, NaF 38%;Potassium based compound contains K by mass percentage2CO320~50%, KHCO315~30%, KCl 12~ 20%, KF 16~20%;Calcium based compound in mixed compound accounts for the 55% of gross mass, magnesium based compound, sodium based compound The 15% of gross mass is respectively accounted for potassium based compound;
(3) temperature of smelting furnace is controlled during slag refining at 1450~1500 DEG C;Wherein raw material and slag former plus Enter mode are as follows: place into smelting furnace after raw material and slag former are pressed into agglomerate after mixing;The smelting furnace of use is mine heat Furnace;
(4) after completing slag refining, melt is come out of the stove and is poured into mold, the silicon alloy melt and slag melt in melt exist Stratification in mold, then condensation solidification will be carried out respectively after silicon alloy melt and slag melt separation, wherein silicon alloy melt Silicon alloy is formed after condensation, contains Si 62% by mass percentage;
The silicon rate of recovery is 70%.
Embodiment 6
With embodiment 1, difference is method:
(1) the high scrap silicon generated when the high scrap silicon used is high-silicon alloy cutting;Drying goes moisture removal as raw material;
(2) prepare slag former;Wherein the mass ratio of raw material and slag former is 100:33;Slag former is mixed compound, by Magnesium based compound, sodium based compound and calcium based compound mix;Calcium based compound contains CaCO by mass percentage369%, CaCl27%, CaF21%, CaO 23%;Magnesium based compound contains MgO 30%, MgCO by mass percentage320%, MgF2 15%, MgCl235%;Sodium based compound contains Na by mass percentage2CO320%, NaHCO330%, NaCl 12%, NaF 38%;Calcium based compound in mixed compound accounts for the 56% of gross mass, and magnesium based compound and sodium based compound respectively account for gross mass 22%;
(3) temperature of smelting furnace is controlled during slag refining at 1430~1480 DEG C;Wherein raw material and slag former plus Enter mode are as follows: first press raw materials into agglomerate, be put into smelting furnace after then again mixing agglomerate and slag former;The smelting furnace of use It is refining furnace;
(4) after completing slag refining, whole melts silicon alloy melt and slag melt stratification in smelting furnace, then It pours into respectively and condenses solidification in different molds, wherein form silicon alloy after the condensation of silicon alloy melt, contain Si by mass percentage 59%;
The silicon rate of recovery is 81%.

Claims (7)

1. a kind of produce HIGH-PURITY SILICON/silicon alloy method with high scrap silicon slag refining, it is characterised in that sequentially include the following steps:
(1) moisture removal is removed into the drying of high scrap silicon, as raw material;Prepare slag former;Wherein the mass ratio of raw material and slag former is 100:(3~60);The slag former is calcium based compound, or is mixed compound;The mixed compound is magnesium system One of compound, sodium based compound and potassium based compound a variety of are mixed with calcium based compound;The calcium system It closes object and contains CaCO by mass percentage30~99%, CaCl20~30%, CaF20~30%, CaO 1~100%;Described Magnesium based compound contains MgO 0~100%, MgCO by mass percentage30~100%, MgF20~30%, MgCl21~ 100%;The sodium based compound contains Na by mass percentage2CO31~100%, NaHCO30~99%, NaCl 0~ 30%, NaF 0~30%;The potassium based compound contains K by mass percentage2CO320~50%, KHCO315~30%, KCl 12~20%, KF 15~38%;Wherein the calcium based compound in mixed compound accounts for the 10~99% of gross mass;
(2) smelting furnace is opened, raw material and slag former are put into smelting furnace and carry out slag refining, raw material and slag former all melt After form melt;The temperature of smelting furnace is controlled during slag refining at 1420 DEG C or more;
(3) after completing slag refining, melt is come out of the stove and is poured into mold, the silicon melt in melt/silicon alloy melt and clinker are molten Body stratification in mold, then condensation solidification will be carried out respectively after silicon melt/silicon alloy melt and slag melt separation, wherein HIGH-PURITY SILICON/silicon alloy is formed after silicon melt/silicon alloy melt condensation;Or after completing slag refining, whole melts are in smelting furnace Then interior silicon melt/silicon alloy melt and slag melt stratification pour into respectively and condense solidification in different molds, wherein silicon is molten HIGH-PURITY SILICON/silicon alloy is formed after body/silicon alloy melt condensation.
2. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method, feature according to claim 1 Be there are two types of the high scrap silicons: one is the high scrap silicons that solar energy industry generates, and select solar energy crystalline silicon silicon ingot The material end to end that is scaled off after the polishing waste material that is generated when the cutting waste material that is generated when slice, crystalline silicon ingot polishing, crystalline silicon ingot casting, Discarded crystal silicon chip and/or superseded solar battery sheet;The cutting generated when the described solar energy crystalline silicon slicing silicon ingots Waste material includes the waste material that diamond cut generates and the waste material that silicon carbide cutting generates;The crystalline silicon is polysilicon and monocrystalline The general designation of silicon;Another kind is the high scrap silicon generated when broken high-silicon alloy or cutting, and the high-silicon alloy is the matter of Si Measure the alloy of percentage >=50%.
3. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method according to claims 1 and 2, It is characterized in that the pickling of high scrap silicon elder generation is removed impurity, then water when high scrap silicon is the high scrap silicon that solar energy industry generates Filtrate is washed till as neutrality, finally drying is used as raw material;The acid solution that pickling uses is the hydrochloric acid of mass concentration 5~30% and/or sulphur Acid, the mass ratio of acid solution and high scrap silicon is (3~15) when pickling: 1.
4. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method, feature according to claim 1 It is in step (2), the adding manner of raw material and slag former are as follows: raw material and slag former are put into smelting furnace after mixing;Or Person is to place into smelting furnace after raw material and slag former are pressed into agglomerate after mixing;The either first group of pressing raw materials into Block is put into smelting furnace after then again mixing agglomerate and slag former.
5. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method, feature according to claim 1 It is that the smelting furnace is electric arc furnaces, mineral hot furnace, refining furnace, induction furnace, resistance furnace or plasma furnace.
6. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method according to claims 1 and 2, It is characterized in that, when high scrap silicon is the high scrap silicon that solar energy industry generates, silicon melt and slag melt are layered when standing, HIGH-PURITY SILICON is formed after silicon melt condensation, contains Si 99~99.999% by mass percentage;When high scrap silicon be industrial silicon and/or When the high scrap silicon generated when silicon alloy is broken or cuts, when standing, silicon alloy melt and slag melt are layered, silicon alloy Silicon alloy is formed after melt condensation, contains Si >=50% by mass percentage.
7. a kind of high scrap silicon slag refining production HIGH-PURITY SILICON/silicon alloy method, feature according to claim 1 It is that the HIGH-PURITY SILICON using solidification is oriented in directional solidification furnace, comes out and cools down to room temperature after directional solidification and obtains Silicon ingot cuts off at the both ends end to end of silicon ingot respectively, and the resection length at both ends accounts for silicon ingot total length 20~30%, remainder end to end For the polysilicon of solar level, contain Si >=99.9999% by mass percentage.
CN201811219039.7A 2018-10-19 2018-10-19 A method of HIGH-PURITY SILICON/silicon alloy is produced with high scrap silicon slag refining Pending CN109292779A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110156023A (en) * 2019-06-14 2019-08-23 宝兴易达光伏刃料有限公司 A kind of environmentally protective smelting high-purity silicon method
CN112981101A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method for simultaneously recycling cut silicon waste and trapping rare and precious metals in spent catalyst
CN113860314A (en) * 2021-09-29 2021-12-31 新疆大全绿创环保科技有限公司 Method for producing industrial silicon by using silicon-containing solid waste

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070245854A1 (en) * 2006-04-25 2007-10-25 The Arizona Board Of Regents On Behalf Of The University Of Arizona Silicon refining process
CN101092741A (en) * 2007-07-17 2007-12-26 佳科太阳能硅(厦门)有限公司 Method for preparing big ingot of polysilicon in level of solar energy
CN101462723A (en) * 2009-01-05 2009-06-24 昆明理工大学 Method for preparing high purity silicon aluminum silicon alloy by vacuum carbon thermal reduction
CN102040219A (en) * 2009-10-14 2011-05-04 贵阳宝源阳光硅业有限公司 Method for preparing high-purity silicon by purifying industrial silicon
CN103011169A (en) * 2012-12-14 2013-04-03 厦门大学 Preparation method for sheet silicon
CN104058405A (en) * 2013-05-10 2014-09-24 福建兴朝阳硅材料股份有限公司 Method for removing impurities phosphorus and boron in silicon metal

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070245854A1 (en) * 2006-04-25 2007-10-25 The Arizona Board Of Regents On Behalf Of The University Of Arizona Silicon refining process
CN101092741A (en) * 2007-07-17 2007-12-26 佳科太阳能硅(厦门)有限公司 Method for preparing big ingot of polysilicon in level of solar energy
CN101462723A (en) * 2009-01-05 2009-06-24 昆明理工大学 Method for preparing high purity silicon aluminum silicon alloy by vacuum carbon thermal reduction
CN102040219A (en) * 2009-10-14 2011-05-04 贵阳宝源阳光硅业有限公司 Method for preparing high-purity silicon by purifying industrial silicon
CN103011169A (en) * 2012-12-14 2013-04-03 厦门大学 Preparation method for sheet silicon
CN104058405A (en) * 2013-05-10 2014-09-24 福建兴朝阳硅材料股份有限公司 Method for removing impurities phosphorus and boron in silicon metal

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JIAN KONG ET AL.: ""An Economical Approach for the Recycling of High-Purity Silicon rom Diamond-Wire Saw Kerf Slurry Waste"", 《SILICON》 *
韩至成等: "《太阳能级硅提纯技术与装备》", 31 October 2011, 冶金工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110156023A (en) * 2019-06-14 2019-08-23 宝兴易达光伏刃料有限公司 A kind of environmentally protective smelting high-purity silicon method
CN112981101A (en) * 2021-02-02 2021-06-18 昆明理工大学 Method for simultaneously recycling cut silicon waste and trapping rare and precious metals in spent catalyst
CN113860314A (en) * 2021-09-29 2021-12-31 新疆大全绿创环保科技有限公司 Method for producing industrial silicon by using silicon-containing solid waste

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