CN101559947B - Smelting method of silicon - Google Patents

Smelting method of silicon Download PDF

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Publication number
CN101559947B
CN101559947B CN2008100709243A CN200810070924A CN101559947B CN 101559947 B CN101559947 B CN 101559947B CN 2008100709243 A CN2008100709243 A CN 2008100709243A CN 200810070924 A CN200810070924 A CN 200810070924A CN 101559947 B CN101559947 B CN 101559947B
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China
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silicon
carbon
dioxide
powder
smelting process
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CN2008100709243A
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CN101559947A (en
Inventor
郑智雄
林霞
戴文伟
胡满根
闻震利
洪紫州
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Nanan Sanjing Sunshine and Power Company Limited
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NANAN SANJING SUNSHINE AND POWER Co Ltd
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Abstract

The invention discloses a smelting method of silicon. The method comprises the steps as follows: alkaline solution is added into a blending body of carbon powder and silica dioxide powder to corrode the surface of the silica dioxide powder body, the blending powder of the carbon powder and the silica dioxide powder added with the alkaline solution are squeezed to form a massive shape under the temperature of 800-100 DEG C to enable the surface of the carbon powder body and the surface of the silica dioxide powder body to be fully combined to increase a reaction contact surface, and moisture inthe alkaline solution is evaporated. The invention provides the smelting method of metal silicon with low production cost and simple operation steps.

Description

A kind of smelting process of silicon
Technical field
The present invention relates to the metallic silicon smelting method, particularly relate to the smelting process of a kind of purity greater than 99% Pure Silicon Metal.
Background technology
Silicon is a kind of important metallurgy, chemical industry, electronics, optical material, plays an important role in wide field such as information, communication, space flight and aviation, environmental protection, silicon solar cells, and the market requirement is also increasing.Pure Silicon Metal production all is that to adopt quartzite, the refinery coke of mining to obtain general quality at electric arc furnace smelting be 98.5%, is siliceous 99% through logical oxygen refining quality, and this mode consumes electric power is huge, and production cost is high.
In addition, a large amount of quartz crucibles that in semiconductor crystal making processes, use are often regarded the waste material abandoned after damage; In graphite, carbon element processing industry, a large amount of highly purified graphite, the tankage abandoned of carbon element corner are arranged, thereby caused the generation of a large amount of waste residues.
Summary of the invention
The object of the present invention is to provide a kind of smelting process of silicon, to solve the problem that exists in the prior art.The present invention is through adding the surface of basic soln corrode silicon dioxide powder in carbon dust and silicon dioxide powder mixing body; Then under 800 ℃~1000 ℃, the mixed powder of aforementioned adding silicon dioxde solution is squeezed into bulk, the surface of carbon, silicon-dioxide powdery is fully combined, increase the reaction contact surface; Make silicon-dioxide more be prone to carry out deoxygenation; Moisture content in the basic soln also is able to evaporate simultaneously, thereby provides a kind of production cost low, the simple metallic silicon smelting method of operation steps.
Technical scheme provided by the invention is following:
A kind of smelting process of silicon may further comprise the steps:
A, to get weight ratio be that 1: 3 carbon, silicon-dioxide is crushed to below 40 orders, mixes;
B, add that concentration is 20%~30%, 1/4~1/2 NaOH, KOH solution of mixed powder that volume is carbon and silicon-dioxide in the steps A, stirring and evenly mixing is after 1~3 hour, the mixture with mixing under 800 ℃~1000 ℃ is squeezed into bulk;
C, the block that obtains among the step B is cut into 1~3cm 3Rectangular parallelepiped or square piece material, drop into to smelt in the electric arc furnace and obtain purity greater than 99% Pure Silicon Metal.
Among the present invention, the carbon that adds in the steps A is the reductor that uses in the silicon Metal smelting process; It is 1: 3 carbon, the feed ratio of silicon-dioxide that the present invention selects weight ratio for use.Like this, can make deoxygenation carry out relatively fully, and reduce carbon residual in Pure Silicon Metal.
Among the step B, the basic soln NaOH that in carbon, silicon-dioxide mixed powder, adds, the surface of the corrodible silicon-dioxide powdery of KOH, thus make silicon-dioxide more be prone to carry out deoxygenation.The carbon, the silicon-dioxide mixed powder that are chosen among the step B under 800 ℃~1000 ℃ the basic soln that adds push; Said temperature can make carbon, silicon-dioxide mixed powder soften; The surface of carbon, silicon-dioxide mixed powder can fully be combined; Increase the reaction contact surface, thereby the deoxygenation of silicon-dioxide is taken place fully.800 ℃~1000 ℃ temperature also can make the moisture content in the basic soln all be able to evaporation.
Among the step C silicon-dioxide dropped in the electric arc furnace to smelt and be routine techniques, the present invention does not also further improve it, no longer specifies at this.
In the smelting process of aforementioned silicon, basic soln can be preferably NaOH for NaOH, KOH etc.
Said silicon-dioxide is preferably the inferior quartz crucible that semicon industry uses, and said carbon is preferably graphite or/and the remaining corner of carbon element processing industry tankage.The silica sand as traditional metal silicon raw materials for production is high for the purity of silicon-dioxide in the quartz crucible, and simultaneously, carbon content is also than higher in the corner tankage of graphite, carbon element processing industry.Because the impurity source is mainly by bringing into as original impurity in raw-material quartzite, the carbon in the Pure Silicon Metal, therefore, above-mentioned choices of raw materials can further improve from the purity of the silicon of electric arc furnace acquisition.Simultaneously, inferior quartz crucible that the present invention also will handle as waste residue and graphite or/and the remaining corner of carbon element processing industry tankage reuse again, thereby reduced the discharging of " three wastes ".
At the bottom of the metallic silicon smelting method production cost among the present invention; Operation steps is simple; The present invention then is squeezed into bulk with carbon dust, silicon dioxide powder through add the surface of basic soln corrode silicon dioxide powder at the carbon of pulverizing, silicon-dioxide, and the surface of carbon dust, silicon-dioxide powdery is fully combined; Increase the reaction contact surface, thereby make silicon-dioxide more be prone to carry out deoxygenation.Inferior quartz crucible that the present invention uses when also using preparation monocrystalline or polycrystal and graphite are or/and the remaining corner of carbon element processing industry tankage are produced starting material as Pure Silicon Metal; Above-mentioned choices of raw materials can further improve from the purity of the silicon of electric arc furnace acquisition, also can make the industrial waste that produces in the above-mentioned industry obtain recycling.
Embodiment
Below in conjunction with embodiment the present invention is done further description, but do not constitute any restriction of the present invention.
Embodiment 1
Carbon, the silicon-dioxide getting weight ratio and be 1: 3 are crushed to below 40 orders, mix.Wherein, the inferior quartz crucible that silicon-dioxide uses when being preparation monocrystalline or polycrystal, carbon is that graphite is or/and the remaining corner of carbon element processing industry tankage.
The NaOH solution stirring mixing that add concentration and be 20%, volume is aforementioned mixed powder 1/4 was squeezed into bulk with aforementioned powder after 1 hour under 800 ℃, the surface of carbon dust, silicon dioxide powder is fully combined, and the whole moisture content in the evaporation NaOH solution.
The block that obtains in the abovementioned steps is cut into 3cm 3Rectangular parallelepiped or square piece material, drop in the electric arc furnace and smelt with ordinary method, the purity of gained Pure Silicon Metal is 99.5%.
Embodiment 2
Carbon, the silicon-dioxide getting weight ratio and be 1: 3 are crushed to below 40 orders, mix.Wherein, the inferior quartz crucible that silicon-dioxide uses when being preparation monocrystalline or polycrystal, carbon is that graphite is or/and the remaining corner of carbon element processing industry tankage.
The NaOH solution stirring mixing that add concentration and be 25%, volume is aforementioned mixed powder 1/2 was squeezed into bulk with aforementioned powder after 3 hours under 900 ℃, the surface of carbon dust, silicon dioxide powder is fully combined, and the whole moisture content in the evaporation NaOH solution.
The block that obtains in the abovementioned steps is cut into 2cm 3Rectangular parallelepiped or square piece material, drop in the electric arc furnace and smelt with ordinary method, the purity of gained Pure Silicon Metal is 99.9%.
Embodiment 3
Carbon, the silicon-dioxide getting weight ratio and be 1: 3 are crushed to below 40 orders, wherein, the inferior quartz crucible that silicon-dioxide uses during for preparation monocrystalline or polycrystal, carbon is that graphite is or/and the remaining corner of carbon element processing industry tankage.
After silicon-dioxide, the carbon dust of gained in the abovementioned steps mixed; The NaOH solution stirring mixing that add concentration and be 30%, volume is aforementioned mixed powder 2/5 is after 3 hours; At 1000 ℃ aforementioned powder is squeezed into bulk; The surface of carbon dust, silicon dioxide powder is fully combined, and the whole moisture content in the evaporation NaOH solution.
The block that obtains in the abovementioned steps is cut into 1cm 3Rectangular parallelepiped or square piece material, drop in the electric arc furnace and smelt with ordinary method, the purity of gained Pure Silicon Metal is 99.8%.
Above-mentionedly be merely three specific embodiments of the present invention, but design concept of the present invention is not limited thereto, allly utilizes this design that the present invention is carried out the change of unsubstantiality, all should belong to the behavior of invading protection domain of the present invention.

Claims (3)

1. the smelting process of a silicon may further comprise the steps:
A, to get weight ratio be that 1: 3 carbon, silicon-dioxide is crushed to below 40 orders, mixes;
B, add that concentration is 20%~30%, 1/4~1/2 NaOH, KOH solution of mixed powder that volume is carbon and silicon-dioxide in the steps A, stirring and evenly mixing is after 1~3 hour, the mixture with mixing under 800 ℃~1000 ℃ is squeezed into bulk;
C, the block that obtains among the step B is cut into 1~3cm 3Rectangular parallelepiped or square piece material, drop into to smelt in the electric arc furnace and obtain purity greater than 99% Pure Silicon Metal.
2. according to the smelting process of the silicon described in the claim 1, it is characterized in that: said silicon-dioxide is preferably the inferior quartz crucible that semicon industry uses, and said carbon is preferably graphite or/and the remaining corner of carbon element processing industry tankage.
3. according to the smelting process of the silicon described in the claim 1, it is characterized in that: the solution that step B adopts is preferably NaOH solution.
CN2008100709243A 2008-04-15 2008-04-15 Smelting method of silicon Expired - Fee Related CN101559947B (en)

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CN101559947B true CN101559947B (en) 2012-07-11

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1237537A (en) * 1998-06-01 1999-12-08 永川市科学技术委员会 Production process for smelting commercial silicon by using quartz sand
CN1281819A (en) * 2000-08-31 2001-01-31 齐国庆 New method for smelting industrial silium and ferro-silicon and its equipment
CN101112986A (en) * 2007-06-29 2008-01-30 商南中剑实业有限责任公司 Method for producing industrial silicon by using petroleum coke as reducing agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1237537A (en) * 1998-06-01 1999-12-08 永川市科学技术委员会 Production process for smelting commercial silicon by using quartz sand
CN1281819A (en) * 2000-08-31 2001-01-31 齐国庆 New method for smelting industrial silium and ferro-silicon and its equipment
CN101112986A (en) * 2007-06-29 2008-01-30 商南中剑实业有限责任公司 Method for producing industrial silicon by using petroleum coke as reducing agent

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