CN110217797A - A kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online - Google Patents
A kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online Download PDFInfo
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- CN110217797A CN110217797A CN201910576738.5A CN201910576738A CN110217797A CN 110217797 A CN110217797 A CN 110217797A CN 201910576738 A CN201910576738 A CN 201910576738A CN 110217797 A CN110217797 A CN 110217797A
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Abstract
A kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online disclosed by the invention, first, generation silica fine powder is collected into accumulator tank during diamond wire saw is prepared silicon wafer, flows into filter press after the silica fine powder sawdust material in accumulator tank is added water cooling dilution；Secondly, being sent into pelletizer after the siliceous solution in filter press is carried out de-watering extrusion and being granulated, dryer distributing device is sent into after being granulated, after drying, obtaining outer diameter is 5mm~10mm, and length is 10mm~25mm silicon grain；Finally, the silicon grain that step 2 is obtained, which is placed in progress melting in vacuum medium frequency induction furnace, obtains high-purity industrial silicon.Method disclosed by the invention, realizes side cutting monocrystalline silicon, and scrap silicon is collected on side, side purifies scrap silicon, realizes waste utilization, shortens process flow, so that the solid waste of slicing single crystal silicon enterprise is not dispatched from the factory and can be recycled, reach circulation company standard, and produces high added value.
Description
Technical field
The invention belongs to the technical fields that the secondary resource of silicon materials recycles, and in particular to a kind of Buddha's warrior attendant wire cutting list
The method that crystal silicon waste material manufactures high-purity industrial silicon online.
Background technique
Industrial silicon (also known as silicon metal, metallic silicon) is one of important materials in modern industrial production, the purposes ten of industrial silicon
Divide extensively, is applied to the fields such as electronics, steel-making, optics, machinery, automobile manufacture, chemical industry, metallurgy, medicine, national defence, is known as " work
Industry monosodium glutamate ".Additive of the industrial silicon as non-ferrous alloy, also serves as the alloying constituent for requiring stringent silicon steel, is steel-making, non-ferric
Based alloy smelts essential deoxidier.High Purity classes and grades in school industrial silicon is more needed for integrated circuit and solar energy power generating
It can be used for solar-energy photo-voltaic cell after the raw material of crystal silicon, monocrystalline silicon, monocrystalline silicon or the cutting of polysilicon silicon wafer.Diamond wire saw silicon
For piece because speed is fast, consumptive material is low, and cutting piece rate is high, and silicon wafer is thin flexible, and cell conversion rate is high, has dragged down the cost of silicon wafer, gold
Hard rock wire cutting silicon wafer is completely instead of traditional abrasive wire sawing technique.Saw is inevitably generated in silicon wafer cutting process
End, sawdust silicon content 90% or so, how more efficient recycling these industrial wastes, reduce entreprise cost, alleviate environmental protection pressure
Power, the added value for promoting industrial waste are most important.
Monocrystalline silicon slice station-service slicer carries out silicon rod with diamond wire to be cut into silicon wafer at present, what cutting process generated
Recovery pond is flowed into after the dilution of silica fine powder sawdust material and carries out collection neutralization natural sedimentation, and flocculant is added in recovery pond and is oriented solidification
Afterwards, silicon clay coating state is deposited in recycling bottom of pond portion, after top moisture is taken away, paste state silicon mud is carried out filters pressing, is fallen after silicon mud filters pressing
Enter in recycling basket, jumbo bag is spread on the inside of recycling basket, temporary storehouse is transported to fork truck after pack and carries out sunning cooling, by 24-48
It is transported to sale warehouse after hour Temperature fall, post sales, other clients use silicon mud as raw material intermediate frequency furnace or other heating
Mode produces industrial silicon.The recovery method of the silicon cutting waste material put forward at present is mostly half pyrogenic process of half wet process or Whote-wet method work
Skill.If having that production capacity is low, reaction speed is slow, long flow path, corrodes to equipment in production practices using Whote-wet method technique
Greatly, the problems such as silicon purity is not also high, half thermal process of half wet process, can also have the problems such as technique is cumbersome.
Summary of the invention
The object of the present invention is to provide a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online, solutions
Existing method of purification of the having determined problem that process is tedious and the silicon purity of purification is not high.
The technical scheme adopted by the invention is that a kind of Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online
Method, specific operation process include the following steps:
Step 1, vacuum intermediate-frequency induction melting furnace is passed through into piping connection in the downstream of Buddha's warrior attendant linear cutting equipment, starts Buddha's warrior attendant
Linear cutting equipment, generation silica fine powder is collected into accumulator tank during Buddha's warrior attendant wire cutting is prepared silicon wafer, by the silicon in accumulator tank
Fine powder sawdust material flows into filter press after adding water cooling dilution；
Step 2, the siliceous solution in filter press being subjected to de-watering extrusion, is dewatered to 40%~50%, temperature is 30 DEG C~
At 50 DEG C, be sent into pelletizer be granulated, after being granulated be sent into dryer distributing device, by drying after, obtain outer diameter 5mm~
10mm, length are 10mm~25mm silicon grain；
Step 3, silicon grain step 2 obtained, which is transported to be placed in vacuum medium frequency induction furnace, carries out melting, after melting
Silicon liquid, which is poured into, to be seated in the intracorporal silicon ingot mold of vacuum chamber, vacuum cavity is pulled out after standing cooling 20min, after natural air cooled
Using silicon ingot is hung out from carrying jig to obtain high-purity industrial silicon.
Other features of the invention also reside in,
Preferably, accumulator tank, filter press, pelletizer, the inlet port and outlet port pipeline between dryer distributing device and
Exhaust fume collecting hood connection, entire material transport carry out under closed environment.
Preferably, the melting condition in step 3 in vacuum medium frequency induction furnace is as follows: vacuum pressure≤5Pa, smelting temperature
1500 DEG C~1600 DEG C, monitor system 800kW~1000kW, melting frequency 400Hz~500Hz, speed of melting 400kG/h~
600kG/h。
Preferably, the pouring condition in step 3 is as follows: casting in every 2 hours is primary, daily casting 10 times~12 times, every time
About 600kg~900kg.
Preferably, Si > 99.5%, Fe≤0.2%, Al≤0.2%, Ca≤0.2% in the high-purity industrial silicon being prepared.
The invention has the advantages that a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online,
According to the process and characteristic of the silicon powder sawdust material that diamond wire saw monocrystalline silicon piece generates, by vacuum medium frequency induction furnace and diamond wire
The device on-line joining process for cutting silicon wafer together, realizes the silicon powder sawdust material online recycling of Buddha's warrior attendant wire cutting generation and is transported to
Melting reaction is carried out in vacuum medium frequency induction furnace, is produced high-purity industrial silicon of high added value, is realized waste utilization, shorten work
Skill process makes the solid waste of slicing single crystal silicon enterprise not dispatch from the factory and can recycle, and realizes change cutting silicon wafer side recycling monocrystalline
The process of scrap silicon makes the solid waste of slicing single crystal silicon enterprise not dispatch from the factory and can recycle, and reaches circulation company standard, and
Produce high added value.
Specific embodiment
The present invention is described in detail With reference to embodiment.
A kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online of the invention, specific operation process
Include the following steps:
Step 1, vacuum intermediate-frequency induction melting furnace is passed through into piping connection in the downstream of Buddha's warrior attendant linear cutting equipment, starts Buddha's warrior attendant
Linear cutting equipment, generation silica fine powder is collected into accumulator tank during Buddha's warrior attendant wire cutting is prepared silicon wafer, by the silicon in accumulator tank
Fine powder sawdust material flows into filter press after adding water cooling dilution；
Step 2, the siliceous solution in filter press being subjected to de-watering extrusion, is dewatered to 40%~50%, temperature is 30 DEG C~
At 50 DEG C, be sent into pelletizer be granulated, after being granulated be sent into dryer distributing device, by drying after, obtain outer diameter be 5mm~
10mm, length are 10mm~25mm silicon grain；
Accumulator tank, filter press, pelletizer, the inlet port and outlet port pipeline between dryer distributing device and exhaust fume collecting hood connect
It connects, entire material transport carries out under closed environment；
Step 3, silicon grain step 2 obtained, which is transported to be placed in vacuum medium frequency induction furnace, carries out melting, after melting
Silicon liquid, which is poured into, to be seated in the intracorporal silicon ingot mold of vacuum chamber, vacuum cavity is pulled out after standing cooling 20min, after natural air cooled
Using silicon ingot is hung out from carrying jig to obtain high-purity industrial silicon.
Melting condition in step 3 in vacuum medium frequency induction furnace is as follows: vacuum pressure≤5Pa, and 1500 DEG C of smelting temperature~
1600 DEG C, monitor system 800kW~1000kW, melting frequency 400Hz~500Hz, speed of melting 400kG/h~600kg/h；
Pouring condition in step 3 is as follows: casting in every 2 hours is primary, daily casting 10 times~12 times, every time about 600kg
~900kg；
Si > 99.5%, Fe≤0.2%, Al≤0.2%, Ca≤0.2% in the high-purity industrial silicon being prepared.
A kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online of the invention, passes through vacuum intermediate-frequency
Induction furnace is connected directly between the downstream of Buddha's warrior attendant linear cutting equipment, when realizing Buddha's warrior attendant wire cutting monocrystalline silicon, is collected simultaneously scrap silicon simultaneously
Processing carries out vacuum melting and obtains HIGH-PURITY SILICON, realizes and purifies when cutting edge is collected, at present in relevant research not yet；This
The main advantage of invention is to melt silicon mud under vacuum conditions, and due to having completely cut off atmosphere, material is not oxidized, will not be generated
New compound, so that final products purity is very high, the rate of recovery reaches 90% or more.There is presently no use scrap silicon to mention for the country
The technique of pure silicon is all to carry out secondary purification with industrial silicon finished product.The technology mode of the domestic monocrystal silicon waste materials of recycling at present is to use
Intermediate frequency furnace melts scrap silicon, and material heats under atmosphere, and the 30% of material is directly just burned off, and is also created except material waste
Dust, these dust a part are spilt into atmosphere, and a part enters directly into silicon solution, cause final products purity low,
The rate of recovery is low, also causes atmosphere pollution.
Embodiment 1
The silicon sawdust material 210t that same day online recycling monocrystalline silicon diamond wire slice generates is obtained after dilution cools down filters pressing
Aqueous 41% silicon mud obtains aqueous 2.5% after granulation drying, and outer diameter 8mm, length is that the silicon grain of 25mm is placed in vacuum intermediate-frequency
In induction furnace, vacuum pressure 5Pa, 1500 DEG C of smelting temperature, melting rated power is 800kW, melting frequency 400Hz, melting
Speed 400kg/h, the same day be poured 10 times, industrial silicon casting yield be followed successively by 590kg, 625kg, 630kg, 646kg, 720kg,
715kg, 650kg, 623kg, 610kg, 450kg, same day industrial silicon add up to yield for 6259kg, and product index chemical examination Si >
99.5%, Fe≤0.2%, Al≤0.2%, Ca≤0.2%.
Embodiment 2
The silicon sawdust material 230t that same day online recycling monocrystalline silicon diamond wire slice generates is obtained after dilution cools down filters pressing
Aqueous 45% silicon mud obtains aqueous 1.5% after granulation drying, and outer diameter 5mm, length is that the silicon grain of 25mm is placed in vacuum intermediate-frequency
In induction furnace, vacuum pressure 4Pa, 1600 DEG C of smelting temperature, melting rated power is 900kW, melting frequency 500Hz, melting
Speed 600kg/h, the same day be poured 12 times, industrial silicon casting yield be followed successively by 640kg, 731kg, 730kg, 678kg, 725kg,
785kg, 746kg, 722kg, 710kg, 750kg, 770kg, 780kg, the same day add up to yield to be 8774kg, and product index chemically examines Si
> 99.5 (%), Fe≤0.2%, Al≤0.2%, Ca≤0.2.
Embodiment 3
The silicon sawdust material 260t that same day online recycling monocrystalline silicon diamond wire slice generates is obtained after dilution cools down filters pressing
Aqueous 50% silicon mud obtains aqueous 1.2% after granulation drying, and outer diameter 8mm, length is that the silicon grain of 18mm is placed in vacuum intermediate-frequency
In induction furnace, vacuum presses 3Pa, and 1550 DEG C of smelting temperature, melting rated power is 1000kW, melting frequency 450Hz, melting speed
Spend 500kg/h, the same day be poured 11 times, industrial silicon casting yield be followed successively by 690kg, 721kg, 740kg, 677kg, 780kg,
800kg, 850kg, 760kg, 710kg, 780kg, 860kg, the same day add up to yield to be 8368kg, and product index chemically examines Si > 99.5
(%), Fe≤0.2%, Al≤0.2%, Ca≤0.2.
Embodiment 4
The silicon sawdust material 220t that same day online recycling monocrystalline silicon diamond wire slice generates is obtained after dilution cools down filters pressing
Aqueous 40% silicon mud obtains aqueous 1% after granulation drying, and outer diameter 6mm, length is the silicon grain of 12mm, smelting temperature 1550
DEG C, melting rated power is 800kW, melting frequency 460Hz, speed of melting 600kg/h, and the same day is poured 10 times, and industrial silicon pours
The yield of note is followed successively by 865kG, 859kG, 788kG, 783kG, 847kG, 862kG, 774kG, 798kG, 750kG, the 754kG same day
Industrial silicon adds up to yield to be 8050kG, and product index chemically examines Si > 99.5 (%), Fe≤0.2%, Al≤0.2%, Ca≤0.2.
Embodiment 5
The silicon sawdust material 240t that same day online recycling monocrystalline silicon diamond wire slice generates is obtained after dilution cools down filters pressing
Aqueous 42% silicon mud obtains aqueous 1.5% after granulation drying, and outer diameter 6mm, length is the silicon grain of 20mm, smelting temperature
1500 DEG C, melting rated power is 1000kW, melting frequency 450Hz, speed of melting 480kg/h, and the same day is poured 12 times, industry
Silicon casting yield be followed successively by 800kg, 820kg, 781kg, 760kg, 697kg, 823kg, 800kg, 850kg, 760kg,
750kg, 780kg, 860kg, the same day add up to yield to be 9481kg, and product index chemically examines Si > 99.5 (%), and Fe≤0.2%, Al≤
0.2%, Ca≤0.2.
Claims (5)
1. a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online, which is characterized in that concrete operations
Journey includes the following steps:
Step 1, vacuum intermediate-frequency induction melting furnace is passed through into piping connection in the downstream of Buddha's warrior attendant linear cutting equipment, starts diamond wire and cuts
Equipment is cut, generation silica fine powder is collected into accumulator tank during Buddha's warrior attendant wire cutting is prepared silicon wafer, by the silica fine powder in accumulator tank
Sawdust material flows into filter press after adding water cooling dilution；
Step 2, the siliceous solution in filter press is subjected to de-watering extrusion, is dewatered to 40%~50%, temperature is 30 DEG C~50 DEG C
When, be sent into pelletizer be granulated, after being granulated be sent into dryer distributing device, by drying after, obtain outer diameter be 5mm~
10mm, length are 10mm~25mm silicon grain；
Step 3, silicon grain step 2 obtained, which is transported to be placed in vacuum medium frequency induction furnace, carries out melting, by the silicon liquid after melting
It is poured into and is seated in the intracorporal silicon ingot mold of vacuum chamber, pull out vacuum cavity after standing cooling 20min, used after natural air cooled
Silicon ingot is hung out from carrying jig to obtain high-purity industrial silicon.
2. a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online as described in claim 1, special
Sign is, the accumulator tank, filter press, pelletizer, the inlet port and outlet port pipeline sum aggregate cigarette between dryer distributing device
Cover connection, entire material transport carry out under closed environment.
3. a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online as described in claim 1, special
Sign is that the melting condition in the step 3 in vacuum medium frequency induction furnace is as follows: vacuum pressure≤5Pa, 1500 DEG C of smelting temperature
~1600 DEG C, monitor system 800kW~1000kW, melting frequency 400Hz~500Hz, speed of melting 400kG/h~600kG/h.
4. a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online as described in claim 1, special
Sign is that the pouring condition in the step 3 is as follows: casting in every 2 hours is primary, daily casting 10 times~12 times, every time about
600kg~900kg.
5. a kind of method that Buddha's warrior attendant wire cutting monocrystal silicon waste materials manufacture high-purity industrial silicon online as described in claim 1, special
Sign is, Si > 99.5%, Fe≤0.2%, Al≤0.2%, Ca≤0.2% in the high-purity industrial silicon being prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807372A (en) * | 2020-07-21 | 2020-10-23 | 昆明理工大学 | Method for top-blown refining of silicon wafer cutting waste |
| CN113023732A (en) * | 2021-03-05 | 2021-06-25 | 昆明理工大学 | Method for preparing high-purity silicon by recovering silicon wafer cutting waste |
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| CN104310405A (en) * | 2014-10-10 | 2015-01-28 | 东莞市长安东阳光铝业研发有限公司 | Microwave-plasma-assisted polysilicon purification method |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
| 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 |
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Patent Citations (5)
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| JP2002293528A (en) * | 2001-03-30 | 2002-10-09 | Sharp Corp | Production method of silicon for solar cell |
| CN104276574A (en) * | 2013-07-05 | 2015-01-14 | 河南省超贝工程设备有限公司 | Method for extraction of high-purity silicon from crystal silicon cutting waste liquid |
| CN104310405A (en) * | 2014-10-10 | 2015-01-28 | 东莞市长安东阳光铝业研发有限公司 | Microwave-plasma-assisted polysilicon purification method |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807372A (en) * | 2020-07-21 | 2020-10-23 | 昆明理工大学 | Method for top-blown refining of silicon wafer cutting waste |
| CN113023732A (en) * | 2021-03-05 | 2021-06-25 | 昆明理工大学 | Method for preparing high-purity silicon by recovering silicon wafer cutting waste |
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