CN101181997A - Method for preparing metallic silicon material - Google Patents

Method for preparing metallic silicon material Download PDF

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Publication number
CN101181997A
CN101181997A CNA2007101965632A CN200710196563A CN101181997A CN 101181997 A CN101181997 A CN 101181997A CN A2007101965632 A CNA2007101965632 A CN A2007101965632A CN 200710196563 A CN200710196563 A CN 200710196563A CN 101181997 A CN101181997 A CN 101181997A
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silicon
dioxide
furnace
oxygen
sand form
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CNA2007101965632A
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Chinese (zh)
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罗应明
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JINGZHAN (NANCHANG) SCIENCE AND TECHNOLOGY Co Ltd
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JINGZHAN (NANCHANG) SCIENCE AND TECHNOLOGY Co Ltd
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Priority to CNA2007101965632A priority Critical patent/CN101181997A/en
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Abstract

The invention discloses a preparation method of a metallic silicon raw material and equipment used in the preparation method. The invention uses a method that quartz mineral sand silicon dioxide is firstly purified and then reverted into the metallic silicon by injecting oxygen instead of avoiding oxygen, and improves traditional melting furnaces processing equipment such as electric arc furnaces and argon arc furnaces, can reach large-scale production as well as greatly promote the pureness of the metallic silicon; the invention has few processing steps and convenient operation and provides highly productive and low energy-consuming raw materials for solar polysilicon/monocrystalline silicon.

Description

A kind of preparation method of metallic silicon material
Technical field
The invention belongs to metallic silicon material engineering field.The present invention relates to a kind of preparation method of metallic silicon material, special, the present invention relates to the quartzy ore in sand form silicon-dioxide of a kind of first purifying, and then reduction and prepare the method for metallic silicon material.The invention still further relates to a kind of used equipment of preparation method of described metallic silicon material.
Background technology
Pure Silicon Metal is the main raw material(s) that solar cell polysilicon is purified, and the purification precision of Pure Silicon Metal directly has influence on purification efficiency, cost and the effect of solar energy polycrystalline silicon.The mainstream technology of metallic silicon raw material preparation is to utilize electric arc furnace/argon arc stove/all kinds of radio-frequency furnaces to carry out high temperature reduction in the world, quartzy (SiO 2) reduce in reduction furnace with carbon and to generate industrial (metal) silicon, its chemical reaction is: SiO 2+ C → Si+CO 2↑.And the chemical reaction of siemens's chemical method is: Si (s)+3HCl (g)=SiHCl 3(g)+H 2(g) (heat release), the SiHCl of generation 3With PCl 3And BCl 3Have on relative volatility that (their boiling point is respectively 31.8 ℃, 74 ℃ and 13 ℃, can use rectification and purification effectively than big-difference.Use H at 1100 ℃ at last 2Reduction SiHCl 3, carry out the inverse process of chlorination reaction: SiHCl 3(g)+H 2(g) → Si (s)+3HCl (g).Solid-state silicon is separated out in reaction, just becomes chunk polysilicon after smashing.So just can obtain purity and be 99.9999999% polycrystalline silicon raw material, in other words, in just average 1,000,000,000 Siliciumatoms an impurity atoms be arranged.Simultaneously, countries in the world also have the improvement of use Siemens Method (being Russian method), silane thermal decomposition process, fluidized bed method, metallurgy method, wherein improve Siemens Method and account for more than 80% of global output.But no matter adopt any processing method without exception, on average purify the power consumption of per kilogram polycrystalline silicon raw material all about the 250--400 degree.Therefore, in the present existing metallic silicon raw material technology of preparing, high energy consumption, the low output of high investment is the major cause under the polycrystalline silicon raw material cost is in not, has seriously restricted the universal use of solar cell.
Summary of the invention
The preparation method and the equipment used thereof that the purpose of this invention is to provide a kind of metallic silicon raw material.
One aspect of the present invention provides a kind of preparation method of metallic silicon raw material, comprises the quartzy ore in sand form silicon-dioxide of first purifying, and then is reduced into Pure Silicon Metal, wherein, does not use rare gas element to keep away oxygen, on the contrary oxygenation.The purity of silicon raw material obtained by the method for the present invention reaches 99.999% even higher by being commonly 98-99% at present in the industry, for next step solar energy polycrystalline silicon/silicon single crystal provides high yield, less energy-consumption, low cost raw material.
Design of the present invention is to utilize smelting furnace such as electric arc furnace/argon arc stove/heating mode melting silicon-dioxide (SiO such as all kinds of radio-frequency furnaces 2), restore into Pure Silicon Metal.Particularly utilize the smelting furnace heating mode to be silicon-dioxide (SiO 2) annotate oxygen in the consummate treating processes, make silicon-dioxide (SiO 2) in phosphorus, boron ion, the abundant oxidation of compound.Under hot conditions, make phosphorus, boron ion, compound gasification then, discharge, thereby reduce silicon-dioxide (SiO via vacuum extractor 2) in phosphorus, boron and all kinds of metal content.Experiment confirm silicon-dioxide (SiO 2) in phosphorus, boron content can reduce to below the 5ppma by the hundreds of ppma of former mineral content, metal content is also reduced to below tens of ppma by 0.2%-.Raw ore silicon-dioxide (SiO 2) purity is promoted to more than 99.99% from about 99%.Through reducing process with silicon-dioxide (SiO 2) be reduced into behind the Pure Silicon Metal as polysilicon silicon single crystal purification raw material.Significantly reduce production, cost of investment.Make solar energy polycrystalline silicon/silicon single crystal and even photovoltaic industry be able to fast development.
At the foregoing invention purpose, the invention provides following technical scheme:
On the one hand, the invention provides a kind of preparation method of metallic silicon material, described method is first purifying quartz sand silicon-dioxide (SiO 2), and then described silicon-dioxide is reduced into Pure Silicon Metal, the advantage that adopts this method is not need to use rare gas element (as nitrogen, argon) to keep away oxygen, oxygenation on the contrary.
Preferably, the quartzy ore in sand form silicon-dioxide of described purifying SiO 2Operation comprise: adopt the chemical pickling method, drying, high temperature is urged oxygen, and high melt.
Preferably, described chemical pickling method comprises: with chloroazotic acid flush away heavy metal, metal ion/compound, the composition proportioning of chloroazotic acid is 3HCl: HNO 3With HF solution flush away phosphorus boron compound.
Preferably, described HF solution ratio consists of, 50 parts of pure water: the HF of 1 part of 49% concentration.
Preferably, described method also comprises: at the quartzy ore in sand form silicon-dioxide of purifying SiO 2After, use centrifuge dewatering again, baking box baking desiccating method drying makes water content<1%.
Preferably, described method also comprises: at the quartzy ore in sand form silicon-dioxide of purifying SiO 2Before, crushed quartz ore in sand form silicon-dioxide SiO 2To micron order.
Preferably, described quartzy ore in sand form silicon-dioxide SiO 2For, get natural purity and reached quartzy ore in sand form silicon-dioxide SiO more than 99% 2, wherein impurity comprises: Al 2O 3And/or CaO and/or Fe 2O 3And/or TiO 2And/or P 2O 5
Preferably, described high temperature is urged oxygen, and high melt carries out in smelting furnace, described high temperature urges oxygen to be operating as, and promptly begins to annotate oxygen technology when temperature reaches 600 ℃, and the oxygen that is fed must be high oxygen concentration, furnace temperature rises to 1300 ℃ gradually, makes quartzy ore in sand form silicon-dioxide SiO 2Interior phosphorus boron complete oxidation type becomes phosphorus boron oxide compound-P 2O 5/ B 2O 3
Preferably, the concentration of described high oxygen concentration is higher than 98%.
Preferably, described high temperature is urged oxygen, and high melt carries out in smelting furnace, and described high melt is operating as, and stops logical oxygen and be warming up to 1600 ℃-1700 ℃ again after finishing phosphorus boron complete oxidation, makes phosphorus boron oxide compound-P 2O 5/ B 2O 3Gasification, the P of gasification 2O 5/ B 2O 3Discharge by gas barrier.
Preferably, described high melt operation also comprises, furnace temperature is risen to above silicon-dioxide SiO again 2Melting point is more than 1700 ℃, and the high more eliminating phosphorus of temperature boron oxide compound effect is good more, utilizes physics heat impurities removal (matter) method that becomes simultaneously, carries out the segmentation cooling and gets rid of white residue impurity, despumation purifying silicon-dioxide.
Preferably, to rise to 1300 ℃ of heat-up rates of 1600 ℃-1700 ℃ of heating up and/or rise to gradually be 10 ℃ of per minutes to furnace temperature.
Preferably, the described carbon reduction that is operating as that is reduced into Pure Silicon Metal.
To sum up, the method for described purified metal silicon specifically can be divided into following three steps:
The quartzy ore in sand form purity of step 1, the Nature has reached more than 99%, and wherein impurity is Al 2O 3, CaO, Fe 2O 3, TiO 2, P 2O 5Deng.
Select the quartzy ore in sand form silicon-dioxide of high purity (as 99.5%) (SiO for use 2) carrying out pickling earlier, quartz sand is thinner, and wash result is better.
With chloroazotic acid (3 parts of hydrochloric acid HCl: 1 part of nitric acid HNO 3) the flush away heavy metal, metal ion/compound etc.
With HF[50 part pure water: 1 part of HF (concentration 49%)] flush away metal, phosphorus, boron compound.
Matting is to remove impurity effectively to reach low cost method, the silicon-dioxide (SiO after chemical examination is cleaned 2), be promoted to more than 99.9% by original 99.5%.
Use centrifuge dewatering then, baking box baking desiccating method dried silica (SiO 2), degree of being dried to reaches water content<1%.
Step 2, quartz sand silicon-dioxide (SiO that cleaned drying is intact 2) carry out High Temperature Furnaces Heating Apparatus and urge oxygen:
The smelting furnace of reincarnate is heated to 600 ℃ opens to make and add high purity oxygen gas (98%), furnace temperature rises to 1300 ℃ (rising 10 ℃ as per minute) gradually, makes the phosphorus boron complete oxidation in the quartzy ore in sand form.Stop logical oxygen then and be warming up to SiO again 21700 ℃ of fusing points, temperature rise speed such as preceding makes phosphorus, boron oxide compound-P 2O 5/ B 2O 3Gasification is discharged by gas barrier.
Step 3, continuity step 2-carry out melting:
Furnace temperature is risen to above more than the quartz sand melting point (1700 ℃), and the high more eliminating phosphorus of temperature boron oxide compound effect is good more, utilizes physics heat impurities removal (matter) method/metal smelting method that becomes simultaneously, despumation purifying silicon-dioxide.
Be described further with regard to the operation and the effect thereof of above-mentioned three steps respectively below:
At first, about the matting step, the concrete grammar of described matting is as follows:
Take from natural quartzy ore in sand form silicon-dioxide (SiO 2), this quartz ore in sand form silicon-dioxide purity has reached more than 99%, and wherein contained impurity is Al 2O 3, CaO, Fe 2O 3, TiO 2, P 2O 5Deng.
With the proportioning component is 3HCl: HNO 3Chloroazotic acid, flush away heavy metal, metal ion and/or metallic compound etc.
With HF solution [50 parts of pure water: 1 part of HF (49%)] flush away phosphorus boron compound.
Matting is to remove impurity effectively to reach low cost method, the silicon-dioxide (SiO after chemical examination is cleaned 2), be promoted to more than 99.9% by original 99.5%.
Use the lyophilization drying again, make water content<1%.
To be broken to micron (μ m) level through the quartzy ore in sand form silicon dioxide powder of aforesaid operations, cleaning performance is better.
Metallic silicon raw material purification preparation method of the present invention, the quartzy ore in sand form silicon-dioxide of first purifying (SiO 2) as the raw material of purifying, wherein cleaning step is most crucial.
Secondly, urge oxygen step and melting step about High Temperature Furnaces Heating Apparatus:
As follows to described scrap build: as to install smelting furnace such as electric smelter, argon arc stove, all kinds of radio-frequency furnace additional oxygenate apparatus and CO 2The discharging collection device specifically can be referring to accompanying drawing 1.
Reach 600 ℃ at smelting furnace and promptly begin to annotate oxygen technology, the oxygen that is fed must be that high purity oxygen is (as 98%O 2), furnace temperature rises to 1300 ℃ (as 10 ℃ of per minutes) gradually, makes quartzy ore in sand form silicon-dioxide (SiO 2) interior phosphorus boron complete oxidation formation phosphorus boron oxide compound-P 2O 5/ B 2O 3
Behind phosphorus boron complete oxidation, stop logical oxygen and be warming up to SiO again 21700 ℃ of fusing points, temperature rise speed such as preceding makes phosphorus boron oxide compound-P 2O 5/ B 2O 3Gasification, the P of gasification 2O 5/ B 2O is discharged by gas barrier.Thus, silicon-dioxide (SiO 2) in existing effect of phosphorus boron of difficult removal by existing effect of row arranged.
Again furnace temperature is risen to above silicon-dioxide (SiO 2) more than the melting point (1700 ℃), the high more eliminating phosphorus of temperature boron oxide compound effect is good more, utilizes physics heat to become impurities removal (matter) method to silicon-dioxide (SiO simultaneously 2) implementation segmentation cooling eliminating white residue impurity, despumation purifying silicon-dioxide.
On the other hand, the invention provides a kind of equipment that is used for described purified metal silicon method, this equipment comprises smelting furnace and/or resistance furnace, and conventional silicon-dioxide reduction furnace, wherein installs oxygenate apparatus and exhaust gas emission collection device on smelting furnace and/or resistance furnace additional.
Preferably, described smelting furnace and/or resistance furnace comprise bell jar and place container bell jar, that be used for fused quartz ore in sand form silicon-dioxide.
Preferably, described oxygenate apparatus and exhaust gas emission collection device are installed on the bell jar of smelting furnace and/or resistance furnace.
Preferably, described equipment comprises a kind of smelting furnace, wherein installs oxygenate apparatus and exhaust gas emission collection device additional at common smelting furnace such as electric smelter, argon arc stove, all kinds of radio-frequency furnace, specifically can be referring to accompanying drawing 1.
Preferably, described smelting furnace is electric arc furnace, argon arc stove or radio-frequency furnace.
Preferably, described oxygenate apparatus is an oxygenation pipeline, and is preferred, has an air intake valve on the described pipeline.
Preferably, described exhaust gas emission collection device is a gas exhaust duct, and is preferred, has a drain tap on the described pipeline.
In equipment of the present invention, described container is crucible preferably.Described crucible is preferably made by silicon carbide or graphite.
Technique effect of the present invention is:
Utilization present method can purify to quartz more than 99.999% for several times.
In the method for purified metal silicon of the present invention, utilize traditional silicon-dioxide (SiO 2) reduction furnace is reduced into Pure Silicon Metal with silicon-dioxide, the carbon that is used must be high pure carbon certainly.Pure Silicon Metal has just been obtained so cheaply.And purity is up to more than 99.999%.
Preparation method of the present invention is applicable to any pattern smelting furnace such as electric arc furnace, argon arc stove, all kinds of radio-frequency furnaces etc., also is suitable for the resistance furnace of any pattern simultaneously.
Advantage of the present invention is:
Utilize cheap matting to add that traditional technology melting equipment such as electric arc furnace, argon arc stove, all kinds of radio-frequency furnace carry out little transformation, just can reach, increase substantially silicon metal purity simultaneously in scale of mass production; Its processing step is few, and is simple to operate, is applicable to the melting equipment of any pattern.
Description of drawings
Fig. 1 shows the special-purpose smelting furnace that uses described purified metal silicon method.As seen from Figure 1, have an oxygenation pipeline on the described smelting furnace, have an air intake valve on the described pipeline, have a gas exhaust duct on the described smelting furnace, have a drain tap on the described pipeline.
Embodiment
Further specify detailed content of the present invention and relevant effect thereof below in conjunction with embodiment, but should be understood that following embodiment only is for illustrating the present invention, and not in office where face constitutes limitation of the scope of the invention.
Embodiment 1
Airtight tube stub that is used for oxygenation and the tube stub that is used for emission gases are installed on the bell jar of conventional electric arc furnace, be used for being installed into air valve and oxygenation pipeline on the tube stub of oxygenation, be used for that drain tap and gas exhaust duct are installed on the tube stub of emission gases, can obtain smelting furnace of the present invention, the concrete visible accompanying drawing 1 of its structure.
Embodiment 2
Selecting purity for use is that 99.5% quartzy ore in sand form silicon-dioxide carries out pickling earlier.Specifically: with the proportioning component is 3HCl: HNO 3Chloroazotic acid, flush away heavy metal, metal ion and/or metallic compound etc.Then, with HF solution [50 parts of pure water: 1 part of HF (49%)] flush away phosphorus boron compound.Through chemical examination, the silicon-dioxide (SiO after the cleaning 2), be promoted to 99.9% by original 99.5%.Use the lyophilization drying again, make water content<1%.
Will be through the quartzy ore in sand form silicon-dioxide of the aforesaid operations smelting furnace of the present invention of packing into.Reach 600 ℃ at smelting furnace and promptly begin to annotate oxygen, the oxygen that is fed is 98%O 2, furnace temperature rises to 1300 ℃ for 10 ℃ gradually with per minute, makes the phosphorus boron complete oxidation in the quartzy ore in sand form silicon-dioxide form phosphorus boron oxide compound-P 2O 5/ B 2O 3
Stop logical oxygen and be warming up to 1650 ℃ again behind phosphorus boron complete oxidation, temperature rise speed is 10 ℃ of per minutes, makes phosphorus boron oxide compound-P 2O 5/ B 2O 3Gasification, the P of gasification 2O 5/ B 2O is discharged by gas barrier.Thus, in the silicon-dioxide existing effect of the phosphorus boron of difficult removal by existing effect of row arranged.
Again furnace temperature is risen to 1750 ℃ (silica melting point is 1700 ℃), utilize the physics heat impurities removal matter method that becomes to get rid of white residue impurity simultaneously, silicon-dioxide is carried out the segmentation cooling get rid of white residue impurity, obtain the silicon-dioxide of purifying.After testing, quartz is purified to more than 99.999% after the process impurities removal for several times.
At last, utilize traditional silicon-dioxide reduction furnace that the silicon-dioxide of above-mentioned purifying is reduced into Pure Silicon Metal, the employed carbon that reduces is high pure carbon.Pure Silicon Metal has just been obtained so cheaply.And purity is up to more than 99.999%.
Embodiment 3
Selecting purity for use is quartzy ore in sand form silicon-dioxide more than 99%, and crushed quartz sand carries out pickling then to micron order.Specifically: with the proportioning component is 3HCl: HNO 3Chloroazotic acid, flush away heavy metal, metal ion and/or metallic compound etc.Then, with HF solution [50 parts of pure water: 1 part of HF (49%)] flush away phosphorus boron compound.Through chemical examination, the silicon-dioxide (SiO after the cleaning 2), be promoted to 99.9% by original 99.%.Use centrifuge dewatering desiccating method drying again, make water content<1%.
Will be through the quartzy ore in sand form silicon-dioxide of the aforesaid operations smelting furnace of the present invention of packing into.Reach 600 ℃ at smelting furnace and promptly begin to annotate oxygen, the oxygen that is fed is 98%O 2, furnace temperature rises to 1300 ℃ gradually, makes the phosphorus boron complete oxidation in the quartzy ore in sand form silicon-dioxide form phosphorus boron oxide compound-P 2O 5/ B 2O 3
Behind phosphorus boron complete oxidation, stop logical oxygen and be warming up to 1670 ℃ again, make phosphorus boron oxide compound-P 2O 5/ B 2O 3Gasification, the P of gasification 2O 5/ B 2O is discharged by gas barrier.Thus, in the silicon-dioxide existing effect of the phosphorus boron of difficult removal by existing effect of row arranged.
Again furnace temperature is risen to 1800 ℃ (silica melting point is 1700 ℃), utilize the physics heat impurities removal matter method that becomes to get rid of white residue impurity simultaneously, silicon-dioxide is carried out the segmentation cooling get rid of white residue impurity, obtain the silicon-dioxide of purifying.After testing, quartzy being purified to more than 99.999%.
At last, utilize traditional silicon-dioxide reduction furnace that the silicon-dioxide of above-mentioned purifying is reduced into Pure Silicon Metal, the employed carbon that reduces is high pure carbon.Pure Silicon Metal has just been obtained so cheaply.And purity is up to more than 99.999%.
Below in conjunction with the embodiments the present invention detailed explanation and explanation have been carried out, but those skilled in the art understand, do not breaking away under the spirit and scope of the invention, any change, improvement, variant, modification and/or the equivalent of the embodiment of the invention is all in the scope of the invention of claims definition.

Claims (22)

1. a method for preparing Pure Silicon Metal comprises the quartzy ore in sand form silicon-dioxide of first purifying, and then is reduced into Pure Silicon Metal, it is characterized in that, does not use rare gas element to keep away oxygen, on the contrary oxygenation.
2. method according to claim 1 is characterized in that, the operation of the quartzy ore in sand form silicon-dioxide of described purifying comprises: the chemical pickling purifying, and drying, high temperature is urged oxygen, and high melt.
3. method according to claim 2 is characterized in that, described chemical pickling purification step comprises:
With chloroazotic acid flush away heavy metal, metal ion/compound, the composition proportioning of chloroazotic acid is 3HCl: HNO 3With
With HF solution flush away phosphorus boron compound.
4. method according to claim 3 is characterized in that, described HF solution ratio consists of, 50 parts of pure water: the HF of 1 part of 49% concentration.
5. according to each described method among the claim 1-4, it is characterized in that described method also comprises: behind the quartzy ore in sand form silicon-dioxide of purifying, use centrifuge dewatering again, baking box desiccating method drying makes water content<1%.
6. according to each described method among the claim 1-5, it is characterized in that described method also comprises: before the quartzy ore in sand form silicon-dioxide of purifying, crushed quartz ore in sand form silicon-dioxide is to micron order.
7. according to each described method among the claim 1-6, it is characterized in that described quartzy ore in sand form silicon-dioxide is that natural purity has reached the quartzy ore in sand form silicon-dioxide more than 99%.
8. according to each described method among the claim 1-7, it is characterized in that, described high temperature is urged oxygen, high melt carries out in smelting furnace, described high temperature urges oxygen to be operating as, and promptly begins to annotate oxygen technology when temperature reaches 600 ℃, and the oxygen that is fed must be high oxygen concentration, furnace temperature rises to 1300 ℃ gradually, makes the phosphorus boron complete oxidation in the quartzy ore in sand form silicon-dioxide form the phosphorus boron oxide compound.
9. method according to claim 8 is characterized in that the concentration of described high oxygen concentration is higher than 98%.
10. according to the described method of claim 1-7, it is characterized in that described high temperature is urged oxygen, high melt carries out in smelting furnace, and described high melt is operating as, and stops logical oxygen and be warming up to 1600 ℃-1700 ℃ again behind phosphorus boron complete oxidation, make the gasification of phosphorus boron oxide compound, the P of gasification 2O 5/ B 2O 3Discharge by gas barrier.
11. method according to claim 10 is characterized in that, the operation of described high melt also comprises, furnace temperature is risen to more than the silica melting point again, utilizes the physics heat impurities removal method that becomes simultaneously, despumation purifying silicon-dioxide.
12. each described method is characterized in that according to Claim 8-11, it is 10 ℃ of per minutes that furnace temperature rises to 1300 ℃ of heat-up rates of 1600 ℃-1700 ℃ of heating up and/or rise to gradually.
13., it is characterized in that the described carbon reduction that is operating as that is reduced into Pure Silicon Metal according to each described method among the claim 1-12.
14. any described used equipment of method for preparing Pure Silicon Metal of claim 1-13, this equipment comprises smelting furnace and/or resistance furnace, and conventional silicon-dioxide reduction furnace, it is characterized in that, on smelting furnace and/or resistance furnace, install oxygenate apparatus and exhaust gas emission collection device additional.
15. equipment according to claim 14 is characterized in that, described smelting furnace is electric arc furnace, argon arc stove or radio-frequency furnace.
16., it is characterized in that described oxygenate apparatus is an oxygenation pipeline according to claim 14 or 15 described equipment.
17., it is characterized in that described exhaust gas emission collection device is a gas exhaust duct according to claim 14 or 15 described equipment.
18. according to claim 16 or 17 described equipment, it is characterized in that, have valve on described oxygenation pipeline and/or the gas exhaust duct.
19., it is characterized in that described smelting furnace and/or resistance furnace comprise bell jar and place container bell jar, that be used for fused quartz ore in sand form silicon-dioxide according to each described equipment among the claim 14-18,
20. equipment according to claim 19 is characterized in that, described container is a crucible.
21. equipment according to claim 20 is characterized in that, described crucible is made by silicon carbide or graphite.
22., it is characterized in that described oxygenate apparatus and exhaust gas emission collection device are installed on the bell jar of smelting furnace and/or resistance furnace according to each described equipment among the claim 19-21.
CNA2007101965632A 2007-11-29 2007-11-29 Method for preparing metallic silicon material Pending CN101181997A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102211771A (en) * 2010-04-06 2011-10-12 富田孝司 Method and system for manufacturing silicon and silicon carbide
CN101837978B (en) * 2009-03-19 2012-02-01 金亦石 Continuous purification reaction treating device and method for producing monocrystalline silicon or polycrystalline silicon by using silica ore
CN108689409A (en) * 2017-04-06 2018-10-23 镇江荣德新能源科技有限公司 A method of preparing metallic silicon using silica crucible fragment
CN110899219A (en) * 2018-09-18 2020-03-24 3S韩国株式会社 Device and method for washing impurities of silicon-based powder

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101837978B (en) * 2009-03-19 2012-02-01 金亦石 Continuous purification reaction treating device and method for producing monocrystalline silicon or polycrystalline silicon by using silica ore
CN102211771A (en) * 2010-04-06 2011-10-12 富田孝司 Method and system for manufacturing silicon and silicon carbide
CN108689409A (en) * 2017-04-06 2018-10-23 镇江荣德新能源科技有限公司 A method of preparing metallic silicon using silica crucible fragment
CN110899219A (en) * 2018-09-18 2020-03-24 3S韩国株式会社 Device and method for washing impurities of silicon-based powder

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