CN106082234A - Intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour - Google Patents
Intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour Download PDFInfo
- Publication number
- CN106082234A CN106082234A CN201610429832.4A CN201610429832A CN106082234A CN 106082234 A CN106082234 A CN 106082234A CN 201610429832 A CN201610429832 A CN 201610429832A CN 106082234 A CN106082234 A CN 106082234A
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- Prior art keywords
- silica flour
- slag
- diamond wire
- intermediate frequency
- cutting silica
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of method reclaiming cutting silica flour, be specifically related to a kind of method that intermediate frequency (IF) smelting reclaims diamond wire cutting silica flour.The cutting silica flour produced in diamond wire monocrystal silicon or polysilicon slicing processes is as raw material, add slag agent melting after adding heat fusing, then repeat interpolation cutting silica flour and slag agent, until completely melted, silicon liquid and slag liquid are poured in cooling bag in the lump and cools down, thus obtain the silico briquette after recovery.The present invention adds slag agent in pyroprocess and avoids the oxidation of silica flour, solves a large amount of irretrievable difficult problems of silicon mud produced in monocrystal silicon/polysilicon slicing processes, it is to avoid a large amount of " silicon mud " pollution on the environments；The present invention reclaims yield and is up to more than 90%, low cost, it is simple to industrial applications.
Description
Technical field
The present invention relates to a kind of method reclaiming cutting silica flour, be specifically related to a kind of intermediate frequency (IF) smelting and reclaim diamond wire cutting silicon
The method of powder.
Background technology
At present, the diamond wire cutting technique that the most especially solar energy enterprise of Japan tries out in sapphire cutting use draws
Enter in silicon chip line cutting field.Diamond wire cutting technique is to utilize plating or resin bonded method to be adhered to by diamond abrasive
On steel wire surface, diamond wire is directly acted on and produces grinding with silicon rod or silicon ingot surface, reach the purpose of cutting.Diamond wire cuts
Have that cutting speed is fast, precision is high, it is low to be lost, piece rate advantages of higher.At present, the technological break-through of line of cut is that silicon chip is processed into
The important channel of this decline, diamond wire cutting speed is the twice of common steel wire, therefore the depreciation of specific yield, manually becomes with energy consumption
This reduction half；Therefore, diamond wire cutting application in photovoltaic enterprise has broad prospects.
In monocrystal silicon enterprise, diamond wire section is widely used；And, in polysilicon is cut into slices, diamond wire
It is expected to replace steel wire and mortar section is tried to be the first exploitation by all multiple enterprises.Diamond wire cutting monocrystal silicon, polysilicon process in, meeting
Producing substantial amounts of cutting silica flour, the average-size of this silica flour is 5um；Additionally, containing substantial amounts of cutting liquid in cutting silica flour.This powder
End, by flocculating sedimentation, is then collected by pressure filter, is finally given " mud cake ", hereinafter simply referred to as " silicon mud ".Due to " silicon mud "
The size of middle silica flour is less, and containing moisture and the impurity of non-silicon；" silicon mud " is not reclaimed ability by most enterprises.Therefore,
In photovoltaic industry, substantial amounts of " silicon mud " become industry in an insurmountable difficult problem.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of intermediate frequency (IF) smelting and reclaim diamond wire cutting silica flour
Method, solves a large amount of irretrievable difficult problems of silicon mud produced in monocrystal silicon/polysilicon slicing processes, it is to avoid a large amount of silicon mud pair
The pollution that environment causes.
Intermediate frequency (IF) smelting of the present invention reclaims the method for diamond wire cutting silica flour, cuts with diamond wire monocrystal silicon or polysilicon
The cutting silica flour produced during sheet, as raw material, adds slag agent melting after adding heat fusing, then repeat interpolation cutting silica flour
With slag agent, until completely melted, silicon liquid and slag liquid are poured in cooling bag in the lump and cools down, thus obtain the silico briquette after recovery.
Wherein: described fusing all uses intermediate frequency coil sensing heating.Frequency used by intermediate frequency coil sensing heating is preferred
Being 400～1000HZ, the magnetic induction line produced in intermediate frequency coil sensing heating process has stirring action to silicon liquid, and efficiently saves
Energy.
As the preferred technical scheme of one, intermediate frequency (IF) smelting of the present invention reclaims the method for diamond wire cutting silica flour,
Comprise the following steps:
(1) select the cutting silica flour produced in diamond wire monocrystal silicon or polysilicon slicing processes as raw material, place it in
In the crucible of induction furnace；
(2) starting heating, after silica flour to be cut is completely melt, add slag agent, temperature is maintained at 1650 DEG C～1850 DEG C；
(3), after melting a period of time, repeat to add cutting silica flour and slag agent, until after being completely melt, by silicon liquid and slag liquid
Cool down in the lump, thus obtain the high-purity silico briquette after recovery.
Wherein:
Cutting silica flour of the present invention is the cutting silica flour produced in diamond wire monocrystal silicon or polysilicon slicing processes.Cut
Cut in silica flour containing Organic substances such as a small amount of flocculant, coolants.The preferred silicon content of cutting silica flour used > 90%；Cutting silicon
The particle mean size of powder is≤20um.
Heating power described in step (2) is 50～80KW, and the time is 1～2h.
In step (2), the mass ratio of slag agent and cutting silica flour is 1:(50～200).
Slag agent is oxide, preferably CaO, MgO, Al2O3Or SiO2In one or more, slag agent purity > 99%.
The speed adding slag agent in step (3) is 5～20Kg/min.
In step (3), it is thus achieved that the purity of the high-purity silico briquette after recovery is: 99-99.98%.
The present invention, intermediate frequency (IF) smelting reclaims the response rate of diamond wire cutting silica flour and is up to more than 90%.
Putting case as the preferred technology of one, step (3) is: after melting 10～60min, is 100～200:1 in mass ratio
Repeating to add cutting silica flour and slag agent, when adding slag, power is 40～55KW, then carries out slag, and during slag, power is 45～60KW,
The slag time is 10min, is then incubated, and during insulation, power is 50～80KW, and temperature retention time is 20min；Until completely melted, will
Silicon liquid and slag liquid are poured in the lump in cooling bag and are cooled down, thus obtain the silico briquette after recovery.Wherein cooling bag is that one has orientation
The mould of refrigerating function, is commercially available prod known in this field.
In sum, the invention have the advantages that
(1) a large amount of irretrievable difficult problems of silicon mud produced during the present invention solves monocrystal silicon/polysilicon slicing processes, keep away
Exempt from a large amount of " silicon mud " pollution on the environment.
(2) present invention adds slag agent in pyroprocess and avoids the oxidation of silica flour.
(3) intermediate frequency (IF) smelting of the present invention reclaims the response rate of diamond wire cutting silica flour and is up to more than 90%, low cost,
It is easy to industrial applications.
(4) the present invention is directed to the specific physical chemical property of " silicon mud ", disclose a kind of intermediate frequency efficient, low cost and melt
Refining reclaim diamond wire cutting silica flour method, it is thus achieved that silico briquette purity more than 99.8%.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
A kind of intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour, comprises the following steps:
(1) the cutting silica flour produced during selecting diamond wire monocrystal silicon is as raw material, containing a small amount of in cutting silica flour
The Organic substance such as flocculant, coolant, cutting silica flour silicon content used is 90.1%；The particle mean size of cutting silica flour is 10um,
Intermediate frequency coil sensing heating is used in placing it in the crucible of induction furnace；
(2) starting heating, heating power is 80KW, and the time is 1h, after silica flour to be cut is completely melt, adds slag agent, temperature
Degree is maintained at 1850 DEG C, and the mass ratio of slag agent and cutting silica flour is 1:100, and slag agent is CaO；
(3) after melting 30min, repeating to add cutting silica flour and slag agent for 100:1 in mass ratio, when adding slag, power is
40KW, then carry out slag, during slag, power is 55KW, and the slag time is 10min, is then incubated, and during insulation, power is 50KW, protects
The temperature time is 20min；Until completely melted, silicon liquid and slag liquid are poured in the lump in the mould with orientation refrigerating function and cool down,
Thus obtain high-purity silico briquette that purity is 99.8%.
This method, intermediate frequency (IF) smelting reclaims the response rate of diamond wire cutting silica flour and is up to 91.7%.
Embodiment 2
A kind of intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour, comprises the following steps:
(1) select the cutting silica flour produced in polysilicon slicing processes as raw material, cutting silica flour contains a small amount of wadding
The solidifying Organic substance such as agent, coolant, cutting silica flour silicon content used is 90.5%；The particle mean size of cutting silica flour is 5um, by it
Intermediate frequency coil sensing heating is used in being placed on the crucible of induction furnace；
(2) starting heating, heating power is 50KW, and the time is 2h, after silica flour to be cut is completely melt, adds slag agent, temperature
Degree is maintained at 1650 DEG C, and the mass ratio of slag agent and cutting silica flour is 1:50, and slag agent is MgO；
(3) after melting 60min, repeating to add cutting silica flour and slag agent for 100:1 in mass ratio, when adding slag, power is
45KW, then carry out slag, during slag, power is 45KW, and the slag time is 10min, is then incubated, and during insulation, power is 80KW, protects
The temperature time is 20min；Until completely melted, silicon liquid and slag liquid are poured in the lump in the mould with orientation refrigerating function and cool down,
Thus obtain high-purity silico briquette that purity is 99.9%.
This method, intermediate frequency (IF) smelting reclaims the response rate of diamond wire cutting silica flour and is up to 93.5%.
Embodiment 3
A kind of intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour, comprises the following steps:
(1) select the cutting silica flour produced in polysilicon slicing processes as raw material, cutting silica flour contains a small amount of wadding
The solidifying Organic substance such as agent, coolant, cutting silica flour silicon content used is 91%；The particle mean size of cutting silica flour is≤20um, will
It uses intermediate frequency coil sensing heating in being placed on the crucible of induction furnace；
(2) starting heating, heating power is 65KW, and the time is 1.5h, after silica flour to be cut is completely melt, adds slag agent,
Temperature is maintained at 1750 DEG C, and the mass ratio of slag agent and cutting silica flour is 1:200, and slag agent is CaO and Al2O3Mix for 1:1 in mass ratio
Close；
(3) after melting 20min, repeating to add cutting silica flour and slag agent for 200:1 in mass ratio, when adding slag, power is
55KW, then carry out slag, during slag, power is 60KW, and the slag time is 10min, is then incubated, and during insulation, power is 60KW, protects
The temperature time is 20min；Until completely melted, silicon liquid and slag liquid are poured in the lump in the mould with orientation refrigerating function and cool down,
Thus obtain high-purity silico briquette that purity is 99.93%.
This method, intermediate frequency (IF) smelting reclaims the response rate of diamond wire cutting silica flour and is up to 94.3%.
Claims (10)
1. the method that an intermediate frequency (IF) smelting reclaims diamond wire cutting silica flour, it is characterised in that: with diamond wire monocrystal silicon or polysilicon
The cutting silica flour produced in slicing processes, as raw material, adds slag agent melting after adding heat fusing, then repeat interpolation cutting silicon
Powder and slag agent, until completely melted, pour into silicon liquid and slag liquid in the lump in cooling bag and cool down, thus obtain the silico briquette after recovery.
Intermediate frequency (IF) smelting the most according to claim 1 reclaims the method for diamond wire cutting silica flour, it is characterised in that: described is molten
Change and all use intermediate frequency coil sensing heating.
Intermediate frequency (IF) smelting the most according to claim 2 reclaims the method for diamond wire cutting silica flour, it is characterised in that: intermediate frequency coil
Frequency used by sensing heating is 400～1000HZ.
4. the method reclaiming diamond wire cutting silica flour according to the arbitrary described intermediate frequency (IF) smelting of claim 1-3, it is characterised in that: bag
Include following steps:
(1) select the cutting silica flour produced in diamond wire monocrystal silicon or polysilicon slicing processes as raw material, place it in sensing
In the crucible of stove；
(2) starting heating, after silica flour to be cut is completely melt, add slag agent, temperature is maintained at 1650 DEG C～1850 DEG C；
(3) after melting a period of time, repeat to add cutting silica flour and slag agent, until after being completely melt, by silicon liquid and slag liquid in the lump
Cooling, thus obtain the silico briquette after recovery.
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: cutting silica flour
Middle silicon content > 90%；The particle mean size of cutting silica flour is≤20um.
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: step (2)
Described in heating power be 50～80KW, the time is 1～2h.
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: step (2)
The mass ratio of middle slag agent and cutting silica flour is 1:(50～200).
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: slag agent is
CaO、MgO、Al2O3Or SiO2In one or more, slag agent purity > 99%.
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: step (3)
The speed adding slag agent is 5～20Kg/min.
Intermediate frequency (IF) smelting the most according to claim 4 reclaims the method for diamond wire cutting silica flour, it is characterised in that: step (3)
For: after melting 10～60min, being 100～200:1 to repeat to add cutting silica flour and slag agent in mass ratio, when adding slag, power is 40
～55KW, then carrying out slag, during slag, power is 45～60KW, and the slag time is 10min, is then incubated, and during insulation, power is
50～80KW, temperature retention time is 20min；Until completely melted, silicon liquid and slag liquid are poured in cooling bag in the lump and cools down, thus obtain
Silico briquette after must reclaiming.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610429832.4A CN106082234A (en) | 2016-06-15 | 2016-06-15 | Intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour |
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|---|---|---|---|
| CN201610429832.4A CN106082234A (en) | 2016-06-15 | 2016-06-15 | Intermediate frequency (IF) smelting reclaims the method for diamond wire cutting silica flour |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445170A (en) * | 2017-09-04 | 2017-12-08 | 大连理工大学 | A kind of method of laser pre-treated directional solidification purification Buddha's warrior attendant wire cutting silica flour waste material |
| CN108059167A (en) * | 2017-12-26 | 2018-05-22 | 中国科学院过程工程研究所 | Cut the method and device that silica flour slag prepares HIGH-PURITY SILICON |
| WO2018103713A1 (en) * | 2016-12-09 | 2018-06-14 | 成都斯力康科技股份有限公司 | Control system and method for regenerative smelting using crushed silicon from silicon factory |
| CN108163860A (en) * | 2018-03-02 | 2018-06-15 | 邱清余 | A kind of industrial silicon rectification systems and refinery practice |
| CN108383122A (en) * | 2018-05-04 | 2018-08-10 | 河南润祥新材料科技有限公司 | A kind of ultra-fine pSi powder recycling method |
| CN108793169A (en) * | 2017-03-27 | 2018-11-13 | 储晞 | A kind of square law device and system recycling Buddha's warrior attendant wire cutting silicon material by-product silicon mud |
| CN110078077A (en) * | 2019-05-14 | 2019-08-02 | 刘亮 | A method of the clay standby metallic silicon of Buddha's warrior attendant wire cutting silicon is recycled based on intermediate frequency (IF) smelting |
| CN110194456A (en) * | 2019-06-14 | 2019-09-03 | 宝兴易达光伏刃料有限公司 | A method of utilizing discarded silicon mud metal smelting silicon |
| CN114212795A (en) * | 2021-12-21 | 2022-03-22 | 湖南立新硅材料科技有限公司 | Device and method for refining silicon sludge |
| CN114772602A (en) * | 2022-04-27 | 2022-07-22 | 中国科学院赣江创新研究院 | Method for improving yield of silicon metal prepared by smelting silicon mud obtained by diamond wire cutting |
| CN115676835A (en) * | 2022-11-30 | 2023-02-03 | 云南铝业股份有限公司 | Slag former for silicon mud smelting and preparation method thereof |
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| 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 |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103713A1 (en) * | 2016-12-09 | 2018-06-14 | 成都斯力康科技股份有限公司 | Control system and method for regenerative smelting using crushed silicon from silicon factory |
| US11261095B2 (en) | 2016-12-09 | 2022-03-01 | Chengdu Silicon Technology Co., Ltd. | Control system and control method for recycling and smelting crushed silica from silicon plants |
| CN108793169A (en) * | 2017-03-27 | 2018-11-13 | 储晞 | A kind of square law device and system recycling Buddha's warrior attendant wire cutting silicon material by-product silicon mud |
| CN107445170A (en) * | 2017-09-04 | 2017-12-08 | 大连理工大学 | A kind of method of laser pre-treated directional solidification purification Buddha's warrior attendant wire cutting silica flour waste material |
| CN108059167A (en) * | 2017-12-26 | 2018-05-22 | 中国科学院过程工程研究所 | Cut the method and device that silica flour slag prepares HIGH-PURITY SILICON |
| CN108163860A (en) * | 2018-03-02 | 2018-06-15 | 邱清余 | A kind of industrial silicon rectification systems and refinery practice |
| CN108383122A (en) * | 2018-05-04 | 2018-08-10 | 河南润祥新材料科技有限公司 | A kind of ultra-fine pSi powder recycling method |
| CN110078077A (en) * | 2019-05-14 | 2019-08-02 | 刘亮 | A method of the clay standby metallic silicon of Buddha's warrior attendant wire cutting silicon is recycled based on intermediate frequency (IF) smelting |
| CN110078077B (en) * | 2019-05-14 | 2021-10-22 | 刘亮 | Method for preparing metal silicon based on intermediate frequency smelting recovered diamond wire cutting silicon mud |
| CN110194456A (en) * | 2019-06-14 | 2019-09-03 | 宝兴易达光伏刃料有限公司 | A method of utilizing discarded silicon mud metal smelting silicon |
| CN110194456B (en) * | 2019-06-14 | 2022-10-21 | 宝兴易达光伏刃料有限公司 | Method for smelting metal silicon by using waste silicon sludge |
| CN114212795A (en) * | 2021-12-21 | 2022-03-22 | 湖南立新硅材料科技有限公司 | Device and method for refining silicon sludge |
| CN114772602A (en) * | 2022-04-27 | 2022-07-22 | 中国科学院赣江创新研究院 | Method for improving yield of silicon metal prepared by smelting silicon mud obtained by diamond wire cutting |
| CN114772602B (en) * | 2022-04-27 | 2023-08-15 | 中国科学院赣江创新研究院 | Method for improving yield of metal silicon prepared by smelting diamond wire cutting silicon mud |
| CN115676835A (en) * | 2022-11-30 | 2023-02-03 | 云南铝业股份有限公司 | Slag former for silicon mud smelting and preparation method thereof |
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