CN108584961A - A kind of method of purification with silicon ore metal smelting silicon - Google Patents
A kind of method of purification with silicon ore metal smelting silicon Download PDFInfo
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- CN108584961A CN108584961A CN201810773021.5A CN201810773021A CN108584961A CN 108584961 A CN108584961 A CN 108584961A CN 201810773021 A CN201810773021 A CN 201810773021A CN 108584961 A CN108584961 A CN 108584961A
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- silicon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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Abstract
The present invention provides a kind of method of purification with silicon ore metal smelting silicon, and step is：Silicon ore raw material is cleaned and dried after crushed；Silicon ore after drying is subjected to magnetic separation processing；The silicon ore that magnetic separation is completed is ground and screens out silica flour；The silica flour filtered out is subjected to electron-beam smelting, realizes that silica flour is molten into silicon liquid；Silicon liquid carries out cooling obtained silicon melt；The resistivity of silicon melt surface is detected, the silicon melt for meeting detected value preset value is cut, and is fitted into after cutting in silica crucible and is placed in progress ingot casting in ingot furnace.Purifying technique advantages of simple of the present invention, by being silica flour by silicon ore magnetic separation post-processing, using electron-beam process, in conjunction with directional solidification method, metallic silicon is purified, improves refining effect, the resistivity of cooperation detection silicon melt surface, the requirement of solar cell grade high-purity silicon is met, and then improves the quality of metallic silicon product, is conducive to the development of solar photovoltaic industry.
Description
Technical field
The present invention relates to metallic silicon smelting purification technique field more particularly to a kind of purifications with silicon ore metal smelting silicon
Method.
Background technology
With the pay attention to day by day of the traditional fossil energies such as coal, oil, natural gas petered out with people to environmental protection,
More and more countries strengthen the development and utilization to regenerative resource.Solar energy is as a kind of inexhaustible, nexhaustible
Clean energy resource, it be widely used to alleviate energy shortage and mitigate environmental pollution be of great significance, wherein solar-electricity
Pond, which generates electricity, receives the great attention of countries in the world as reproducible clear energy sources.Metallic silicon is the master for making solar cell
Material, the purity of silicon is wanted to will have a direct impact on the transfer efficiency and battery life of solar cell, therefore, the metallic silicon of high-purity
It is of great significance to efficient, the stabilization of solar cell.
Generally use silicon ore metal smelting silicon, there are purifying technique complexity, purification effects in the production process of metallic silicon
The undesirable problem of fruit, cannot be satisfied the requirement of solar cell grade high-purity silicon, limit the development of solar photovoltaic industry.
Invention content
Present invention seek to address that the deficiencies in the prior art, and a kind of method of purification with silicon ore metal smelting silicon is provided.
The present invention to achieve the above object, using following technical scheme：
A kind of method of purification with silicon ore metal smelting silicon, which is characterized in that its step is：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, is put into double conic rotary vacuum dryer
In processing is dried, and control moisture content within 0.7%；
B, by after drying silicon ore carry out magnetic separation processing, remove silicon ore in be mingled with machinery iron, containing ferromagnetic mineral,
Weak magnetic mineral and contain iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve；
D, the silica flour filtered out being added in electron beam calciner and carries out electron-beam smelting, vacuum degree is 0.4Pa~2Pa,
Accelerate electronics by voltage drop, assembles electron beam with electric field and magnetic field, it is made to bombard metal, electronics loses when with metal bump
It removes kinetic energy and becomes heat to realize that silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, at this
In the process, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity for detecting silicon melt surface, the silicon melt that preset value is not met to detected value repeat step b~step
E, the silicon melt for meeting detected value preset value are cut, and are fitted into be placed in ingot furnace in silica crucible after cutting and be cast
Ingot.
Preferably, in the step a double conic rotary vacuum dryer operating pressure be -0.09MPa~-
0.096MPa, charging volume are 500L~800L.
Use processing capacity for the dry-type deferrization machine of 10t/h~20t/h when preferably, magnetic separation being handled in the step b.
Preferably, the specification of sieve is the mesh of 200 mesh~300 in the step c.
Preferably, the running parameter difference of electron beam calciner is as follows in the step d：Fusing power be 10kW~
20kW, burn-off rate are 150kg/h~180kg/h.
Preferably, using the resistivity of glow discharge spectrometry detection silicon melt surface in the step f.
The beneficial effects of the invention are as follows：The present invention provides a kind of method of purification with silicon ore metal smelting silicon, purifies work
Skill advantages of simple, by being silica flour by silicon ore magnetic separation post-processing, using electron-beam process, in conjunction with directional solidification method, to gold
Belong to silicon to be purified, improve refining effect, it is high-purity to meet solar battery grade for the resistivity of cooperation detection silicon melt surface
The requirement of silicon, and then the quality of metallic silicon product is improved, it is conducive to the development of solar photovoltaic industry.
Specific implementation mode
With reference to embodiment, the invention will be further described：
A kind of method of purification with silicon ore metal smelting silicon, which is characterized in that its step is：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, is put into double conic rotary vacuum dryer
In processing is dried, and control moisture content within 0.7%；
B, by after drying silicon ore carry out magnetic separation processing, remove silicon ore in be mingled with machinery iron, containing ferromagnetic mineral,
Weak magnetic mineral and contain iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve；
D, the silica flour filtered out being added in electron beam calciner and carries out electron-beam smelting, vacuum degree is 0.4Pa~2Pa,
Accelerate electronics by voltage drop, assembles electron beam with electric field and magnetic field, it is made to bombard metal, electronics loses when with metal bump
It removes kinetic energy and becomes heat to realize that silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, at this
In the process, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity for detecting silicon melt surface, the silicon melt that preset value is not met to detected value repeat step b~step
E, the silicon melt for meeting detected value preset value are cut, and are fitted into be placed in ingot furnace in silica crucible after cutting and be cast
Ingot.
Preferably, in the step a double conic rotary vacuum dryer operating pressure be -0.09MPa~-
0.096MPa, charging volume are 500L~800L.
Use processing capacity for the dry-type deferrization machine of 10t/h~20t/h when preferably, magnetic separation being handled in the step b.
Preferably, the specification of sieve is the mesh of 200 mesh~300 in the step c.
Preferably, the running parameter difference of electron beam calciner is as follows in the step d：Fusing power be 10kW~
20kW, burn-off rate are 150kg/h~180kg/h.
Preferably, using the resistivity of glow discharge spectrometry detection silicon melt surface in the step f.
Embodiment 1
A kind of method of purification with silicon ore metal smelting silicon, step are：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, is put into double conic rotary vacuum dryer
In be dried processing, the operating pressure of double conic rotary vacuum dryer is -0.09MPa, and charging volume is 500L, and control contains
Water rate is within 0.7%；
B, the silicon ore after drying is subjected to magnetic separation processing, magnetic separation uses processing capacity to be removed for the dry type of 10t/h when handling
Iron machine removes the machinery iron being mingled in silicon ore, contains ferromagnetic mineral, weak magnetic mineral and contains iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve,
The specification of sieve is 200 mesh；
D, the silica flour filtered out is added in electron beam calciner and carries out electron-beam smelting, the work ginseng of electron beam calciner
Number is as follows respectively：Fusing power is 10kW, and burn-off rate 150kg/h, vacuum degree 0.4Pa accelerate electricity by voltage drop
Son assembles electron beam with electric field and magnetic field, it is made to bombard metal, and electronics loses kinetic energy when with metal bump and becomes heat
Realize that silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, at this
In the process, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity that silicon melt surface is detected using glow discharge spectrometry, the silicon that preset value is not met to detected value are molten
Weight answers step b~step e, and the silicon melt for meeting detected value preset value is cut, and is fitted into silica crucible and is set after cutting
In carrying out ingot casting in ingot furnace.
Embodiment 2
A kind of method of purification with silicon ore metal smelting silicon, step are：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, is put into double conic rotary vacuum dryer
In be dried processing, the operating pressure of double conic rotary vacuum dryer is -0.093MPa, and charging volume is 600L, and is controlled
Moisture content is within 0.6%；
B, the silicon ore after drying is subjected to magnetic separation processing, magnetic separation uses processing capacity to be removed for the dry type of 15t/h when handling
Iron machine removes the machinery iron being mingled in silicon ore, contains ferromagnetic mineral, weak magnetic mineral and contains iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve,
The specification of sieve is 280 mesh；
D, the silica flour filtered out is added in electron beam calciner and carries out electron-beam smelting, the work ginseng of electron beam calciner
Number is as follows respectively：Fusing power is 15kW, and burn-off rate 160kg/h, vacuum degree 1Pa accelerate electronics by voltage drop,
Assemble electron beam with electric field and magnetic field, it is made to bombard metal, electronics loses kinetic energy when with metal bump and becomes heat in fact
Existing silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, at this
In the process, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity that silicon melt surface is detected using glow discharge spectrometry, the silicon that preset value is not met to detected value are molten
Weight answers step b~step e, and the silicon melt for meeting detected value preset value is cut, and is fitted into silica crucible and is set after cutting
In carrying out ingot casting in ingot furnace.
Embodiment 3
A kind of method of purification with silicon ore metal smelting silicon, step are：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, is put into double conic rotary vacuum dryer
In be dried processing, the operating pressure of double conic rotary vacuum dryer is -0.096MPa, and charging volume is 800L, and is controlled
Moisture content is within 0.5%；
B, the silicon ore after drying is subjected to magnetic separation processing, magnetic separation uses processing capacity to be removed for the dry type of 20t/h when handling
Iron machine removes the machinery iron being mingled in silicon ore, contains ferromagnetic mineral, weak magnetic mineral and contains iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve,
The specification of sieve is 300 mesh；
D, the silica flour filtered out is added in electron beam calciner and carries out electron-beam smelting, the work ginseng of electron beam calciner
Number is as follows respectively：Fusing power is 20kW, and burn-off rate 180kg/h, vacuum degree 2Pa accelerate electronics by voltage drop,
Assemble electron beam with electric field and magnetic field, it is made to bombard metal, electronics loses kinetic energy when with metal bump and becomes heat in fact
Existing silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, at this
In the process, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity that silicon melt surface is detected using glow discharge spectrometry, the silicon that preset value is not met to detected value are molten
Weight answers step b~step e, and the silicon melt for meeting detected value preset value is cut, and is fitted into silica crucible and is set after cutting
In carrying out ingot casting in ingot furnace.
The present invention is exemplarily described above, it is clear that present invention specific implementation is not subject to the restrictions described above,
As long as using the various improvement of inventive concept and technical scheme of the present invention progress, or not improved directly apply to other fields
It closes, within protection scope of the present invention.
Claims (6)
1. a kind of method of purification with silicon ore metal smelting silicon, which is characterized in that its step is：
A, silicon ore raw material is subjected to cleaning process after crushed, after the completion of cleaning, be put into double conic rotary vacuum dryer into
Row is dried, and controls moisture content within 0.7%；
B, the silicon ore after drying is subjected to magnetic separation processing, removes the machinery iron being mingled in silicon ore, containing ferromagnetic mineral, weak magnetic
Property mineral and contain iron mineral inclusion enclave；
C, the silicon ore that magnetic separation is completed is ground, is sieved after grinding, silica flour is filtered out through sieve；
D, the silica flour filtered out is added in electron beam calciner and carries out electron-beam smelting, vacuum degree is 0.4Pa~2Pa, is passed through
Voltage drop accelerates electronics, assembles electron beam with electric field and magnetic field, so that its is bombarded metal, electronics loses dynamic when with metal bump
Can and become heat to realize that silica flour is molten into silicon liquid；
E, silicon liquid is flowed out from the outlet of electron beam calciner, coagulation forming in the container for be oriented solidification is poured into, in the process
In, cooling obtained silicon melt is carried out by water cooling；
F, the resistivity for detecting silicon melt surface, the silicon melt that preset value is not met to detected value repeats step b~step e, right
The silicon melt that detected value meets preset value is cut, and is fitted into after cutting in silica crucible and is placed in progress ingot casting in ingot furnace.
2. a kind of method of purification with silicon ore metal smelting silicon according to claim 1, which is characterized in that the step
The operating pressure of double conic rotary vacuum dryer is -0.09MPa~-0.096MPa in a, and charging volume is 500L~800L.
3. a kind of method of purification with silicon ore metal smelting silicon according to claim 1, which is characterized in that the step
Use processing capacity for the dry-type deferrization machine of 10t/h~20t/h when magnetic separation is handled in b.
4. a kind of method of purification with silicon ore metal smelting silicon according to claim 1, which is characterized in that the step
The specification of sieve is the mesh of 200 mesh~300 in c.
5. a kind of method of purification with silicon ore metal smelting silicon according to claim 1, which is characterized in that the step
The running parameter difference of electron beam calciner is as follows in d：Fusing power be 10kW~20kW, burn-off rate be 150kg/h~
180kg/h。
6. a kind of method of purification with silicon ore metal smelting silicon according to claim 1, which is characterized in that the step
Using the resistivity of glow discharge spectrometry detection silicon melt surface in f.
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| CN201810773021.5A CN108584961A (en) | 2018-07-14 | 2018-07-14 | A kind of method of purification with silicon ore metal smelting silicon |
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| CN201810773021.5A CN108584961A (en) | 2018-07-14 | 2018-07-14 | A kind of method of purification with silicon ore metal smelting silicon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396720A (en) * | 2019-08-19 | 2019-11-01 | 大同新成新材料股份有限公司 | A kind of thermal field crucible application method that more product silicon growth speed are adjusted |
| CN112978744A (en) * | 2021-02-24 | 2021-06-18 | 赤峰市奇运蒙脱石精细化工有限公司 | Rotary mixing method for bentonite raw material |
-
2018
- 2018-07-14 CN CN201810773021.5A patent/CN108584961A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110396720A (en) * | 2019-08-19 | 2019-11-01 | 大同新成新材料股份有限公司 | A kind of thermal field crucible application method that more product silicon growth speed are adjusted |
| CN112978744A (en) * | 2021-02-24 | 2021-06-18 | 赤峰市奇运蒙脱石精细化工有限公司 | Rotary mixing method for bentonite raw material |
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Application publication date: 20180928 |
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