CN106082231B - Crystal silicon wafer cutting edge material flotation removes carbon method - Google Patents

Crystal silicon wafer cutting edge material flotation removes carbon method Download PDF

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Publication number
CN106082231B
CN106082231B CN201610476937.5A CN201610476937A CN106082231B CN 106082231 B CN106082231 B CN 106082231B CN 201610476937 A CN201610476937 A CN 201610476937A CN 106082231 B CN106082231 B CN 106082231B
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cutting edge
crystal silicon
silicon wafer
wafer cutting
edge material
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CN106082231A (en
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杨梦洁
孙毅
申君来
王杰
杨正宏
辛玲
高敏杰
宋中学
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Henan Yicheng New Energy Co ltd
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Henan Yicheng New Energy Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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Abstract

The invention discloses a kind of crystal silicon wafer cutting edge material flotation to remove carbon method, it is intended to solves existing crystal silicon wafer cutting edge material except carbon method except carbon is not thorough, except the technical problem that carbon efficiencies are low, gained silicon carbide micro-powder purity is low after processing, can not directly use.This method comprises the following steps:Batch mixing, add flotation agent and be heated slurry;Compressed air is continuously introduced into floation tank and is stirred;Strike off the carbon dust impurity layer that liquid level air supporting goes out in time by material scraping plate;Slurry is pumped into siphon cylinder action of forced stirring and waterpower classification of sedimentation, inclined tube processor is then pumped into and scraper plate centrifuge carries out concentration and centrifugal dehydration separating treatment respectively, used after gained silicon carbide micro-powder drying and processing after dither batcher sieves pine processing.This method strong operability, except carbon is thorough, efficient, gained silicon carbide micro-powder purity is high, granularity concentration degree is good, can directly be used as crystal silicon wafer cutting edge material, application value is high.

Description

Crystal silicon wafer cutting edge material flotation removes carbon method
Technical field
The present invention relates to crystal silicon wafer cutting edge material flotation technology field, and in particular to a kind of crystal silicon wafer cutting edge material flotation removes Carbon method.
Background technology
Crystal silicon wafer cutting edge material is granularity generally between 5 μm~15 μm of relatively fine carborundum solid micro-powder particle, matter Ground is hard and has sharp corner angle, and the sword material as cutting solar energy crystal silicon chip cell piece, monocrystalline silicon and polysilicon are cut In flakes.Crystal silicon wafer cutting edge material usually can be mixed with impurity carbon dust, it is necessary to take certain measure to be removed during preparation, And finally obtain the silicon carbide micro-powder in the range of designated size.At present except carbon drags for the mode of carbon frequently with cyclonic separation or overflow, And add additive and adjust pH value, and then the carbon dust being mixed with carborundum is removed.Or air is blasted into silicon carbide slurry, Carbon impurity is brought to upper strata liquid level using the micro-bubble that gas produces in slurry and forms impurity froth bed, then passes through scraper plate Carbon impurity is struck off.Aforesaid way exist except carbon is not thorough, except carbon efficiencies it is low the problem of, and the silicon carbide micro-powder after processing is pure Spend that low, granularity concentration degree is poor, can not directly use, it is difficult to meet the needs of crystal silicon wafer cutting edge material.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of carbon dust to remove thoroughly, except carbon efficiencies are high, silicon carbide micro-powder is pure Degree is high, granularity concentration degree is good, can remove carbon method directly as the crystal silicon wafer cutting edge material flotation that crystal silicon wafer cutting edge material uses.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
Design a kind of crystal silicon wafer cutting edge material flotation and remove carbon method, comprise the following steps:
(1)The crystal silicon wafer cutting edge material of carbon dust impurity will be mixed with water by 1:0.5~5 mass ratio mixes in floation tank Close;Flotation agent is added into floation tank and is heated to 40~80 DEG C;
(2)Start the high speed rotor of the flotation column bottom in floation tank, make its Stirring in floation tank, mix slurry Close uniformly, and extraneous compressed air is constantly introduced by floation tank by the bleed hole of flotation column, and in floation tank upper strata liquid level Form carbon dust impurity layer;
(3)By step(2)The carbon dust impurity layer that middle floation tank liquid level is formed constantly is struck off in time by material scraping plate, until Untill carbon dust impurity no longer occurs in floation tank upper strata liquid level, obtain removing the crystal silicon wafer cutting edge material slurry after carbon in floation tank;
(4)By step(3)The slurry of gained is pumped into siphon cylinder by mortar pump, is carried out under the booster action of action of forced stirring Waterpower classification of sedimentation;
(5)By step(4)Slurries after waterpower classification of sedimentation are pumped into inclined tube processor by mortar pump and carry out concentration, Make solid content >=70% of carborundum in slurries;
(6)By step(5)Slurries after concentration are pumped to scraper plate centrifuge by mortar pump carries out centrifugal dehydration separating treatment, Obtain silicon carbide micro-powder particle and make its biodiversity degree≤10%;
(7)By step(6)The silicon carbide micro-powder of gained carries out drying and processing under the conditions of 100~110 DEG C, makes its mass distributary Amount degree is down to less than 0.05%, then is stored after dither batcher sieves pine processing.
Preferably, step(1)In used water be deionized water, the μ s/cm of its electrical conductivity≤1.
Preferably, step(1)Described in mode of heating for steam heat or heat-conducting oil heating.
Preferably, step(2)Described in flotation column high speed rotor rotating speed be 3000~5000 revs/min;Flotation column introduces Compressed air pressure be 5~10MPa.
Preferably, step(4)Described in the action of forced stirring time be 10~30 minutes, the sedimentation time be 60~90 points Clock.
Preferably, step(5)High-frequency vibration feed unit frequency used in middle sieve pine is 5000~6000 revs/min.
Preferably, step(1)Described in flotation agent for neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl Cellulose, kerosene or terpenic oil, its additive amount are the 0.01%~0.1% of crystal silicon wafer cutting edge material quality.
Preferably, step(1)Described in flotation agent for neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl Mixture of one of the cellulose with kerosene or with terpenic oil, its additive amount for crystal silicon wafer cutting edge material quality 0.01%~ 0.1%;In mixture, neopelex or ammonium hydrogen carbonate or diethanol amine or the quality of carboxymethyl cellulose and kerosene Than for 0.5~5:1;Neopelex or ammonium hydrogen carbonate or diethanol amine or the quality of carboxymethyl cellulose and terpenic oil Than for 0.5~5:1.
The advantageous effects of the present invention are:
1. step(1)The flotation agent of addition causes the carbon dust that crystal silicon wafer cutting edge material is wherein mixed with when high speed rotor stirs Between silicon carbide micro-powder produce electrostatic repulsion effect and it is discrete open, easy to the separation and removal of carbon dust;Particulate is exacerbated to exist Random motion in liquid phase, can improve the activity of flotation agent, make the dispersiveness enhancing of carbon dust contaminant particles in the liquid phase, improve Flotation removes the efficiency of carbon.Step(2)By the constant introduction of gas of flotation column in high speed rotor Stirring, by crystal silicon chip The carbon dust being mixed with cutting blade material is brought to floation tank upper strata liquid level by air supporting and forms carbon dust impurity layer, and passes through step(3) Carbon dust impurity is struck off in time.Step(4)Waterpower classification of sedimentation can meet requirement of the crystal silicon wafer cutting edge material to size distribution, step Suddenly(5)Inclined tube concentration is taken, the partial moisture in silicon carbide slurry is removed, improves the solid content of silicon carbide slurry, can subtract Light subsequent step(6)The pressure of centrifugal dehydration, improves centrifugal dehydration work efficiency, then through step(7)After drying and sieve pine processing, Gained silicon carbide micro-powder particle is in loose condition (of surface), reaches crystal silicon wafer cutting edge material requirement, can be cut directly as crystal silicon chip Sword material uses.
2. crystal silicon wafer cutting edge material flotation of the present invention removes carbon method and technique, led suitable for crystal silicon wafer cutting edge material flotation Domain, the crystal silicon wafer cutting edge material carbon dust handled by this method remove thorough, the silicon carbide micro-powder purity height of preparation, granularity concentration Spend, and method strong operability, except carbon efficiencies are high, gained crystal silicon wafer cutting edge material can be used directly, be highly suitable for industrializing Promote and apply.
Embodiment
Illustrate the embodiment of the present invention with reference to embodiment, but following embodiments are used only to describe in detail The present invention, does not limit the scope of the invention in any way.
Embodiment 1:Flotation is carried out to crystal silicon wafer cutting edge material according to the following steps and removes carbon:
(1)The crystal silicon wafer cutting edge material of carbon dust impurity will be mixed with deionized water that electrical conductivity is 0.8 μ s/cm by 1:2 Mass ratio mixes in floation tank;Then flotation agent neopelex is added into floation tank, its additive amount is crystal silicon The 0.09% of wafer cutting edge material quality, and by slurry, it is heated to 40 DEG C using steam-heated mode.
(2)Start floation tank in flotation column bottom high speed rotor, make its rotating speed be 4000 revs/min under conditions of Stirring in floation tank, crystal silicon wafer cutting edge material, flotation agent, water are uniformly mixed, and will be outer by the bleed hole of flotation column The compressed air that boundary's pressure is 6MPa constantly introduces floation tank, and forms carbon dust impurity layer in floation tank upper strata liquid level.
(3)By step(2)The carbon dust impurity layer that middle floation tank liquid level is formed constantly is struck off in time by material scraping plate, until Untill carbon dust impurity no longer occurs in floation tank upper strata liquid level, obtain removing the crystal silicon wafer cutting edge material slurry after carbon in floation tank;
(4)By step(3)The slurry of gained is pumped into siphon cylinder by mortar pump, is carried out under the booster action of action of forced stirring Waterpower classification of sedimentation, the action of forced stirring time is 20 minutes, the sedimentation time is 70 minutes.
(5)By step(4)Slurries after waterpower classification of sedimentation are pumped into inclined tube processor by mortar pump and carry out concentration, Make solid content >=70% of carborundum in slurries.
(6)By step(5)Slurries after concentration are pumped to scraper plate centrifuge by mortar pump carries out centrifugal dehydration separating treatment, Obtain silicon carbide micro-powder particle and make its biodiversity degree≤10%.
(7)By step(6)The silicon carbide micro-powder of gained carries out drying and processing under the conditions of 100~110 DEG C, makes its mass distributary Amount degree is down to less than 0.05%, then is stored after dither batcher sieves pine processing, the shake of dither batcher Dynamic frequency is 5000 revs/min.
Embodiment 2:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 1 and removes carbon, difference exists In step(1)In 80 DEG C are heated to slurry;Its additive amount of flotation agent neopelex used cuts for crystal silicon chip The 0.075% of sword material quality.
Embodiment 3:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 1 and removes carbon, difference exists In step(1)Flotation agent used is ammonium hydrogen carbonate, its additive amount is the 0.01% of crystal silicon wafer cutting edge material quality, step(2)It is floating The high speed rotor rotating speed for selecting column is 3000 revs/min, and the compressed air pressure of introducing is 8MPa.
Embodiment 4:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 3 and removes carbon, difference exists In step(1)Flotation agent used is diethanol amine, its additive amount is the 0.03% of crystal silicon wafer cutting edge material quality.
Embodiment 5:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 1 and removes carbon, difference exists In step(1)Slurry is heated by the way of heat-conducting oil heating to 40 DEG C, flotation agent used is carboxymethyl cellulose, it is added Measure as the 0.05% of crystal silicon wafer cutting edge material quality.
Embodiment 6:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 5 and removes carbon, difference exists In step(1)Flotation agent used is kerosene, its additive amount is the 0.04% of crystal silicon wafer cutting edge material quality.
Embodiment 7:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 5 and removes carbon, difference exists In step(1)Flotation agent used is terpenic oil, its additive amount is the 0.025% of crystal silicon wafer cutting edge material quality.
Embodiment 8:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 1 and removes carbon, difference exists In step(2)Flotation agent used is one of neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl cellulose With the mixture of kerosene, its additive amount is the 0.01%~0.1% of crystal silicon wafer cutting edge material quality;Wherein, dodecyl benzene sulfonic acid The mass ratio of the two in the mixture of sodium and kerosene is 5:1;The mass ratio of the two in the mixture of ammonium hydrogen carbonate and kerosene is 1: 1;The mass ratio of the two in the mixture of diethanol amine and kerosene is 2:1;The two in the mixture of carboxymethyl cellulose and kerosene Mass ratio be 4:1.
Embodiment 9:Flotation is carried out to crystal silicon wafer cutting edge material according to the same manner as in Example 1 and removes carbon, difference exists In step(1)Flotation agent used is one of neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl cellulose With the mixture of terpenic oil, its additive amount is the 0.01%~0.1% of crystal silicon wafer cutting edge material quality;Wherein, detergent alkylate sulphur The mass ratio of the two is 4.5 in the mixture of sour sodium and terpenic oil:1;The matter of the two in the mixture of ammonium hydrogen carbonate and terpenic oil Amount is than being 0.8:1;The mass ratio of the two in the mixture of diethanol amine and terpenic oil is 1.5:1;Carboxymethyl cellulose and pine camphor The mass ratio of the two is 3.5 in the mixture of oil:1.
Involved instrument and equipment is routine instrument device unless otherwise instructed in the embodiment above;Involved The raw material of industry is commercially available regular industrial raw material unless otherwise instructed.
After 1~9 method of the embodiment of the present invention carries out flotation carbon removal treatment to crystal silicon wafer cutting edge material, gained crystal silicon chip The mass percentage of carbon is down to less than 0.01% in cutting blade material, and the mass percentage of carborundum is up to more than 99%, its grain Concentration degree is spent at 5.4 μm ~ 13.5 μm, contrasts the JIS correlation grains that its granularity concentration degree is significantly better than silicon carbide micro-powder industry universal 4.5 μm ~ 20 μ ms of scale alignment request, can use directly as crystal silicon wafer cutting edge material, meet industry requirement, and Strong operability of the present invention, except carbon efficiencies are high, gained silicon carbide micro-powder purity is high, is highly suitable for industrial application.
In addition, step(2)When heating-up temperature is higher, the random motion of particulate in the liquid phase is increased, improves flotation The activity of agent, makes the dispersiveness enhancing of carbon dust contaminant particles in the liquid phase, improves the efficiency that flotation removes carbon.Mutually exist together reaching 15%~20% conditioning agent dosage can be saved when managing effect, can further reduce production cost.
The present invention is described in detail above in conjunction with embodiment, still, person of ordinary skill in the field can Understand, can also be to each design parameter make a change in above-described embodiment, shape on the premise of present inventive concept is not departed from Into multiple specific embodiments, it is common excursion of the invention, is no longer described in detail one by one herein.

Claims (8)

1. a kind of crystal silicon wafer cutting edge material flotation removes carbon method, it is characterised in that comprises the following steps:
(1)The crystal silicon wafer cutting edge material of carbon dust impurity will be mixed with water by 1:0.5~5 mass ratio mixes in floation tank;To Flotation agent is added in floation tank and is heated to 40~80 DEG C;
(2)Start the high speed rotor of the flotation column bottom in floation tank, make its Stirring in floation tank, make slurry mixing equal It is even, and extraneous compressed air is constantly introduced by floation tank by the bleed hole of flotation column, and formed in floation tank upper strata liquid level Carbon dust impurity layer;
(3)By step(2)The carbon dust impurity layer that middle floation tank liquid level is formed constantly is struck off in time by material scraping plate, until flotation Untill carbon dust impurity no longer occurs in pond upper strata liquid level, obtain removing the crystal silicon wafer cutting edge material slurry after carbon in floation tank;
(4)By step(3)The slurry of gained is pumped into siphon cylinder by mortar pump, and waterpower is carried out under the booster action of action of forced stirring Classification of sedimentation;
(5)By step(4)Slurries after waterpower classification of sedimentation are pumped into inclined tube processor by mortar pump and carry out concentration, make slurry Solid content >=70% of carborundum in liquid;
(6)By step(5)Slurries after concentration are pumped to scraper plate centrifuge by mortar pump carries out centrifugal dehydration separating treatment, obtains Silicon carbide micro-powder particle simultaneously makes its biodiversity degree≤10%;
(7)By step(6)The silicon carbide micro-powder of gained carries out drying and processing under the conditions of 100~110 DEG C, makes its biodiversity hundred Divide and be down to less than 0.05% than content, then stored after dither batcher sieves pine processing.
2. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(1) In, water used is deionized water, the μ s/cm of its electrical conductivity≤1.
3. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(1) In, the mode of heating is heated for steam or heat-conducting oil heating.
4. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(2) In, the high speed rotor rotating speed of the flotation column is 3000~5000 revs/min;The compressed air pressure that flotation column introduces for 5~ 10MPa。
5. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(4) In, the action of forced stirring time is 10~30 minutes, and the sedimentation time is 60~90 minutes.
6. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(5) In, the high-frequency vibration feed unit frequency sieved used in pine is 5000~6000 revs/min.
7. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(1) In, the flotation agent is neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl cellulose, kerosene or terpenic oil, Its additive amount is the 0.01%~0.1% of crystal silicon wafer cutting edge material quality.
8. crystal silicon wafer cutting edge material flotation according to claim 1 removes carbon method, it is characterised in that in the step(1) In, the flotation agent is one of neopelex, ammonium hydrogen carbonate, diethanol amine, carboxymethyl cellulose and kerosene Or the mixture with terpenic oil, its additive amount are the 0.01%~0.1% of crystal silicon wafer cutting edge material quality;In mixture, dodecane Base benzene sulfonic acid sodium salt or ammonium hydrogen carbonate or diethanol amine or the mass ratio of carboxymethyl cellulose and kerosene are 0.5~5:1;Dodecyl Benzene sulfonic acid sodium salt or ammonium hydrogen carbonate or diethanol amine or the mass ratio of carboxymethyl cellulose and terpenic oil are 0.5~5:1.
CN201610476937.5A 2016-06-27 2016-06-27 Crystal silicon wafer cutting edge material flotation removes carbon method Expired - Fee Related CN106082231B (en)

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CN101033066B (en) * 2006-03-06 2011-06-22 张捷平 Method of recovering silicon carbide micro-powder
CN105127009B (en) * 2015-08-26 2018-04-06 连云港龙塔研磨材料有限公司 The flotation unit and method of free carbon in a kind of removal carborundum powder

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