CN109161963A - A kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon - Google Patents
A kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon Download PDFInfo
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- CN109161963A CN109161963A CN201811268276.2A CN201811268276A CN109161963A CN 109161963 A CN109161963 A CN 109161963A CN 201811268276 A CN201811268276 A CN 201811268276A CN 109161963 A CN109161963 A CN 109161963A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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Abstract
The present invention relates to polysilicon recovery technologies, propose a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon.Firstly, being pre-processed to silicon powder waste material, then silicon powder waste material is granulated using the heating method of high-energy density, vacuum oriented solidification is carried out to the silico briquette after granulation later, electron-beam smelting finally is carried out to silicon ingot.The present invention uses laser or electric arc heated mode, due to having the characteristics that energy density is high, can make superfine silica powder in certain area under the premise of having not enough time to occur severe oxidation, instant melting and rapid condensation is at the silico briquette with certain volume.High-energy density granulation process, yield > 95% of silicon significantly improve the charging efficiency of subsequent fusion process, reduce cost.Meanwhile the present invention can more efficiently improve the removal rate of impurity, finally obtain solar-grade polysilicon further combined with effumabilities impurity such as the dephlegmation of vacuum oriented solidification impurity and electron-beam smelting removal P, O.
Description
Technical field
The present invention relates to polysilicon recovery technologies, and in particular to a kind of method of high efficiente callback Buddha's warrior attendant wire cutting silicon powder.
Background technique
With being constantly progressive for battery mounting technology and melting technique, the totle drilling cost of crystal silicon solar batteries preparation is continuous
It reduces, but the cost for cutting silicon wafer can not have always been high any more.In the premise of the existing multi-wire cutting technology being most widely used
Under, since there are joint-cutting loss, a large amount of HIGH-PURITY SILICON is wasted in this process.Buddha's warrior attendant wire cutting is nearly 2 years emerging one kind
Multi-wire cutting technology, if cut using pure water, cuts the height generated since it is a kind of fixed abrasive material cutting technique
Pure silicon powder can be directly recycled, and be equivalent to and reproduced a crystal silicon market, be most possibly to solve silicon powder from source
The cutting technique of scrap recovery considerations.Therefore, the recycling for studying Buddha's warrior attendant wire cutting silicon powder waste material is imperative.Currently, both at home and abroad
Great concern all is given to the recycling of the waste material, it is desirable to find the Suitable applications of the silicon powder waste material.According to statistics, only 2018
The annual consumption of domestic polysilicon is calculated i.e. up to 36~400,000 tons, by cut quality loss for 35%, produces silicon powder siccative per year
Up to 13.6~140,000 tons.Due to the quantity cumulative year after year, and purposes exploitation is less, and a large amount of waste from stacking causes very serious
Environmental pollution and the wasting of resources, be badly in need of exploitation be suitble to the material apply large scale processing technology.
Due to the substantial amounts of silicon powder waste material, general processing method is difficult the so more amount of consumption, therefore people are earliest
Want to carry out industrial silicon manufacture to the waste material using traditional smelting mode.According to investigations, it industrially attempted to silicon powder waste material diameter
Induction melting is carried out, but since Buddha's warrior attendant wire cutting silicon powder is thinner, generally less than 0.5 μm, induction melting temperature is lower in addition,
Irreversible chemical reaction easily occurs with carbon atmosphere etc. for superfine silica powder during melting, therefore general yield is no more than
70%.Wherein there are one very important the disadvantage is that the filling rate of silicon powder is very low, since silicon powder surface is attached with organic addition
Agent, the silicon powder after drying is more fluffy, and stacking density is generally 0.3 g/cm3, actual charging efficiency is no more than 10%.Consider
To the consumption of crucible, this mode economic feasibility is poor, therefore there is no expanded.Another way is slag making melting, is lacked
Point is still that yield is lower, and due to the problem of oxidation during filler, yield is general less than 60%, and can introduce a large amount of
Slag agent impurity.In recent years, the recycling research for being directed to Buddha's warrior attendant wire cutting silicon powder waste material is in the trend of cumulative year after year, from having sent out
It is seen on the document of table, specifically includes that hot plasma melting, induction melting, ball milling directly prepare solar energy at nano particle system
Battery, bromine hydrogenation and aerosol reaction etc..The necessary theoretical branch of application and the offer of silicon powder has been widened in these researchs of forefathers
Support, but be not dedicated to fundamentally solving the practical problem of current silicon powder waste recovery.
There are two types of the modes for solving the high yield of silicon powder melting, and one kind is to ensure that in fusion process in gas medium easily and silicon
The bias of the substance of reaction is less than absolute numerical value, and silicon is made to avoid that serious chemical reaction occurs in slow temperature-rise period.
Second is the energy density and heating rate for trying every possible means to improve heating method, so that silicon powder is realized thawing in a short time, makes silicon
Powder is melted into rapidly silico briquette under the premise of not having enough time occurring severe reaction.Wherein first way is relatively difficult to achieve, such as
Realize that lower vacuum degree generally requires to vacuumize equipment, a large amount of superfine powder is handled in a vacuum, is held very much
It easily splashes, and is unfavorable for realizing Continuous maching processing.Melt-through process is also unfavorable for the timely discharge of impurity.Second
Mode has absolute advantage in processing superfine silica powder, instantaneous melt characteristic, melting process as brought by high-energy density
In to oxygen content require and it is insensitive.Therefore, whole operation can carry out in air, have to realization continuous production very big
Help.There are mainly three types of the heating methods that high-energy density can be provided at present, electron beam, laser and high-temperature plasma.
Wherein, electron beam needs are run under stringent vacuum condition, be used primarily in high pure metal removal effumability impurity into one
In step purification, the powder high for melting superfine powder and impurity content is substantially impossible.In contrast laser and
Electric arc has absolute advantage for melting powder in an atmosphere, and after laser and electric arc are granulated, the yield of silicon is greater than
95%, and since the silico briquette of formation has certain macroscopical volume, it is highly beneficial for subsequent traditional melting purification process,
Smelting efficiency can be significantly improved and reduce cost.
Summary of the invention
To solve problems of the prior art, it is main that the invention proposes a set of with high-energy density prilling process
The recycling of feature Buddha's warrior attendant wire cutting silicon powder waste material and the method for preparing solar-grade polysilicon.Using laser or electric arc laser and electricity
Arc is granulated silicon powder, and the yield of silicon is greater than 95%, and since the silico briquette of formation has certain macroscopical volume, for subsequent
Traditional melting purification process it is highly beneficial, smelting efficiency can be significantly improved and reduce cost.The present invention is further combined with biography
The dephlegmation of vacuum oriented solidification impurity of uniting and electron-beam smelting remove the effumabilities impurity such as P, O, can be more efficiently
The removal rate for improving impurity, finally obtains solar-grade polysilicon.
To achieve the above object, the technical solution adopted by the present invention are as follows: propose a kind of high efficiente callback Buddha's warrior attendant wire cutting silicon
The method that powder prepares solar-grade polysilicon, follows the steps below:
(1) powder pre-processes: first by blocky scrap silicon grinds shape silicon powder, and drying to constant weight, then carries out at Low Temperature Thermal
Reason, the argon gas that flowing is passed through in low temperature heat treatment are protected；
(2) heating is granulated: passing through step (1), treated, and silicon powder tiles into melting kettle, and carries out flowing argon to powder
Gas shielded carries out continuously linear scanning along silicon powder surface using the high temperature heat source that laser or high-temperature electric arc generate, to silicon powder into
Row, which melts, to be granulated, and the flue dust generated in fusion process is absorbed by dust exhaust apparatus, after granulation process, to obtained
After silico briquette is cooled to room temperature, flowing argon gas is closed, and the obtained silico briquette with certain volume is taken out, carry out ultrasonic cleaning baking
It is dry；
(3) vacuum oriented solidification: the silico briquette that step (2) is obtained is put into the graphite crucible for being coated with anticracking coating, is taken out to equipment
Induction heating is carried out after vacuum, melts silico briquette sufficiently, is then oriented solidification and is drawn ingot processing, obtains silicon ingot；
(4) electron-beam smelting: the silicon ingot that step (3) is obtained is put into water jacketed copper crucible, after vacuumizing to equipment, is first adopted
First silicon ingot is sufficiently melted with electron beam, behind stable molten bath to be formed, then promotes electron beam line and power, and make electron beam
Circular scanning is carried out in weld pool surface, electron-beam smelting is carried out to silicon ingot, after fusion process, reduces electron beam using slow
The mode of line carrys out induced coagulation process, and silicon molten bath is preferentially solidified close to water jacketed copper crucible bottom, and the surface in silicon molten bath is last
Resolidified region, impurity be eventually enriched in electron beam receive arc region in.
Further, the granularity of powdery silicon powder is between 0.5-1 μm in the step (1), and by its item at 100 DEG C
Drying to constant weight under part.
Further, in the step (1) Low Temperature Heat Treatment technological parameter are as follows: argon flow be 2-5 L/min, heating
Rate is 5-10 DEG C/min, and temperature keeps the temperature 4-6 h after reaching 450 DEG C.
Further, the tail gas generated in step (1) low temperature heat treatment is taken out of by the argon gas flowed, into tail
Flash Gas Compression Skid System processing is discharged into atmosphere after detection is qualified.
Further, in the step (2) power control of laser in 2000-4000 W, the output power of high-temperature electric arc
Control is in 1-40 kW.
Further, the high-temperature electric arc in the step (2) uses non-diverting electric arc or transferred arc.
Further, the vacuum degree of equipment is 2.5 × 10^-2 Pa in the step (3), the liter during induction heating
Warm rate is 5-10 DEG C/min, 1550 DEG C of maximum temperature, keeps the temperature 30-50 min.
Further, in the step (3) in directional solidification process, draw ingot speed control in 0.8-1.8 mm/min.
Further, in the step (4) equipment be evacuated to vacuum degree be 2.5 × 10^-2 Pa, first use line for
300 mA and power are that 2.4 kW electron beams sufficiently melt silicon ingot, behind stable molten bath to be formed, then promote electron beam line
For 400 mA and power is 4.8 kW, and it is made to carry out circular scanning in weld pool surface, carries out electron-beam smelting to silicon ingot.
The beneficial effects of the present invention are embodied in:
(1) can be made ultra-fine in certain area using laser or electric arc heated mode due to having the characteristics that energy density is high
For silicon powder under the premise of having not enough time to occur severe oxidation, instant melting and rapid condensation are at the silico briquette with certain volume.It is high
Energy density granulation process, yield > 95% of silicon, and the charging efficiency of subsequent fusion process can be significantly improved, reduce at
This.
(2) laser or electric arc heated granulation process can remove 75% or more carbon impurity in a short time, and to other
Metal impurities have certain removal effect, dephlegmation and electricity of the present invention further combined with vacuum oriented solidification impurity
Beamlet melting removes the effumabilities impurity such as P, O, can more efficiently improve the removal rate of impurity, finally obtain solar level
Polysilicon.
(3) it can be realized the impurity content in silicon is purified to 6N or more from 2N using method of the present invention, through the
After two-step heating is granulated, the yield of silicon is up to 95% or more, and purity is up to 99.8%, and after vacuum oriented solidification, silicon purity can
Up to 99.99%, most afterwards after electron-beam smelting, silicon purity is up to 99.9999%, finally obtained solar-grade polysilicon relative to
Yield > 90% of dry cutting silicon powder waste material.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
The invention proposes a kind of using high-energy density comminution granulation as the recycling Buddha's warrior attendant wire cutting silicon powder waste material of main feature
And the method for preparing solar-grade polysilicon.The specific steps of which are as follows:
Step 1, the pretreatment of silicon powder waste material: by block-like silicon powder waste material grinds, granularity is between 0.5-1 μm, then 100
Drying to constant weight under conditions of DEG C.Low Temperature Heat Treatment is then carried out, is protected in the process using flowing argon gas, argon flow exists
2-5 L/min, heating rate are 5-10 DEG C/min, keep the temperature 4-6 h after reaching 450 DEG C.The low temperature of this process generation organic matter
It decomposes, decomposing to generate, there is the tail gas of penetrating odor to be taken out of by flowing argon gas, finally enter exhaust gas processing device, and detection is closed
Atmosphere is discharged into after lattice.
Step 2, high-energy density heating are granulated: will the tiling of treated silicon powder into melting kettle, and to powder into
Row flowing argon gas protection, carries out continuously linear scanning along silicon powder surface using the high temperature heat source that laser or high-temperature electric arc generate,
The power control of laser is in 2000-4000 W, and the output power of electric arc is in 1-40 kW.The flue dust generated in fusion process
It is absorbed by dust exhaust apparatus.After granulation process, after obtained silico briquette is cooled to room temperature, flowing argon gas is closed,
And the obtained silico briquette with certain volume is taken out, finally ultrasonic cleaning drying.
Step 3, vacuum oriented solidification: silico briquette obtained above is put into the graphite crucible for being coated with anticracking coating, right
Equipment is evacuated to 2.5 × 10^-2 Pa or so, then carries out induction heating, and heating rate is 5-10 DEG C/min, the highest temperature
1550 DEG C of degree keeps the temperature 30-50 min to ensure that silicon ball sufficiently melts, is then oriented process of setting, ingot speed control is drawn to exist
0.8 -1.8 mm/min。
Electron-beam smelting: step 4 silicon ingot obtained above is put into water jacketed copper crucible, is evacuated to equipment
Then 2.5 × 10^-2 Pa or so is 300 mA in electron beam line, power is first sufficiently molten by silico briquette under conditions of being 2.4 kW
Change.Electron-beam smelting is carried out after stabilised bath to be formed again, promoting electron beam line at this time is 400 mA, and power is 4.8 kW,
And circular scanning is carried out in weld pool surface, smelting time is 20-40 min.After fusion process, using the side of slow drop beam
Formula carrys out induced coagulation process, and silicon molten bath is preferentially solidified close to water-cooled copper bottom, and the surface in silicon molten bath is last resolidified region,
Impurity is eventually enriched in electron beam and receives in arc region.
Claims (9)
1. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon, which is characterized in that according to following
Step carries out:
(1) powder pre-processes: first by blocky scrap silicon grinds shape silicon powder, and drying to constant weight, then carries out at Low Temperature Thermal
Reason, the argon gas that flowing is passed through in low temperature heat treatment are protected；
(2) heating is granulated: passing through step (1), treated, and silicon powder tiles into melting kettle, and carries out flowing argon to powder
Gas shielded carries out continuously linear scanning along silicon powder surface using the high temperature heat source that laser or high-temperature electric arc generate, to silicon powder into
Row, which melts, to be granulated, and the flue dust generated in fusion process is absorbed by dust exhaust apparatus, after granulation process, to obtained
After silico briquette is cooled to room temperature, flowing argon gas is closed, and the obtained silico briquette with certain volume is taken out, carry out ultrasonic cleaning baking
It is dry；
(3) vacuum oriented solidification: the silico briquette that step (2) is obtained is put into the graphite crucible for being coated with anticracking coating, is taken out to equipment
Induction heating is carried out after vacuum, melts silico briquette sufficiently, is then oriented solidification and is drawn ingot processing, obtains silicon ingot；
(4) electron-beam smelting: the silicon ingot that step (3) is obtained is put into water jacketed copper crucible, after vacuumizing to equipment, is first adopted
First silicon ingot is sufficiently melted with electron beam, behind stable molten bath to be formed, then promotes electron beam line and power, and make electron beam
Circular scanning is carried out in weld pool surface, electron-beam smelting is carried out to silicon ingot, after fusion process, reduces electron beam using slow
The mode of line carrys out induced coagulation process, and silicon molten bath is preferentially solidified close to water jacketed copper crucible bottom, and the surface in silicon molten bath is last
Resolidified region, impurity be eventually enriched in electron beam receive arc region in.
2. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, the granularity of powdery silicon powder is dried under conditions of 100 DEG C between 0.5-1 μm, and by it in the step (1)
It does to constant weight.
3. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, in the step (1) Low Temperature Heat Treatment technological parameter are as follows: argon flow is 2-5 L/min, and heating rate is
5-10 DEG C/min, temperature keeps the temperature 4-6 h after reaching 450 DEG C.
4. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, the tail gas generated in step (1) low temperature heat treatment is taken out of by the argon gas flowed, into vent gas treatment
Device processing is discharged into atmosphere after detection is qualified.
5. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, in 2000-4000 W, the output power of high-temperature electric arc exists the power control of laser in the step (2)
1-40 kW。
6. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, the high-temperature electric arc in the step (2) uses non-diverting electric arc or transferred arc.
7. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, the vacuum degree of equipment is 2.5 × 10^-2 Pa in the step (3), the heating rate during induction heating
For 5-10 DEG C/min, 1550 DEG C of maximum temperature, 30-50 min is kept the temperature.
8. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, drawing ingot speed control in 0.8-1.8 mm/min in the step (3) in directional solidification process.
9. a kind of method that high efficiente callback Buddha's warrior attendant wire cutting silicon powder prepares solar-grade polysilicon according to claim 1,
It is characterized in that, it is 2.5 × 10^-2 Pa that equipment, which is evacuated to vacuum degree, in the step (4), first use line for 300 mA
And power is that 2.4 kW electron beams sufficiently melt silicon ingot, behind stable molten bath to be formed, then promoting electron beam line is 400
MA and power are 4.8 kW, and it is made to carry out circular scanning in weld pool surface, carry out electron-beam smelting to silicon ingot.
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Cited By (3)
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| CN109399637A (en) * | 2018-11-02 | 2019-03-01 | 大连理工大学 | A kind of non-diverting electric arc Granulation Equipments of the high temperature of Buddha's warrior attendant wire cutting silicon powder and method |
| CN111302345A (en) * | 2020-04-23 | 2020-06-19 | 四川宏图普新微波科技有限公司 | Method for preparing polycrystalline silicon particles from silicon waste |
| CN114875484A (en) * | 2022-04-15 | 2022-08-09 | 大连理工大学 | Method for preparing high-purity silicon by recovering diamond wire cutting silicon powder through electric field coupling directional solidification technology |
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| CN109399637A (en) * | 2018-11-02 | 2019-03-01 | 大连理工大学 | A kind of non-diverting electric arc Granulation Equipments of the high temperature of Buddha's warrior attendant wire cutting silicon powder and method |
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| CN111302345B (en) * | 2020-04-23 | 2023-03-10 | 四川宏图普新微波科技有限公司 | Method for preparing polycrystalline silicon particles from silicon waste |
| CN114875484A (en) * | 2022-04-15 | 2022-08-09 | 大连理工大学 | Method for preparing high-purity silicon by recovering diamond wire cutting silicon powder through electric field coupling directional solidification technology |
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Application publication date: 20190108 |